Is laboratory SAXS a proven technique?

Over the last two decades small angle X-ray scattering (SAXS) has seen a rise in popularity driven by the improved brightness and collimation of 3rd generation synchrotron beams as well as upgrades in detection systems. However, recent technical advances in laboratory X-ray sources, hybrid pixel detection systems and improved analysis tools (corroborated with the progress in computer science that lead to an increase in calculation power necessary for easy and accurate data analysis of the large data sets generated) have made laboratory SAXS a powerful and versatile technique for the structural characterization of various samples.

Small angle X-ray scattering is an established technique in the experimental toolbox of many research labs. Numerous scientific research fields including materials, food, cosmetics, polymer science, among others, are using a large panel of characterization techniques such as electron microscopy, surface force measurement, nuclear magnetic resonance, light scattering and others. SAXS, by virtue of the X-ray nature of the light used to characterize samples, provides complementary information which can be essential in painting a complete picture of the sample. Its numerous advantages, such as limited requirements for sample preparation, speedy and non-destructive measurements, and the ability to offer both surface and bulk information, make it a standard characterization tool for morphology analysis at the nanometric scale. Recent interlaboratory studies [1] and the emergence of dedicated ISO standards [2,3] have proven the accuracy and traceability of the technique.

Furthermore, the high quality and statistically relevant results together with the possibility to perform experiments in-situ, operando, or under changing conditions (such as temperature, humidity or external fields (tensile, electrical etc.)) have enabled researchers to answer numerous scientific questions and share the newly acquired knowledge with the community through publications in peer-reviewed journals.

The number of publications with laboratory SAXS has doubled over the last decade

One of the key performance indicators of an experimental technique is the number and quality of publications accepted in peer-reviewed journals. In the last decade, the popularity of laboratory SAXS has seen tremendous growth, as it can be deduced from Fig. 1. The number of publications resulting from data collected either wholly or partially on laboratory small angle X-ray scattering instruments has shown a steady increase, doubling over the past decade. This ascending trend is also mimicked by the number of citations these papers have received, suggesting that the results obtained with laboratory SAXS have a considerable impact on the research fields to which they belong.

Fig. 1 In green, the monthly average number of papers published each year resulting from data collected either wholly or partially on laboratory small angle X-ray scattering instruments. In red, the monthly average number of citations received each year for all previously published articles. Data extracted from dimensions.ai in March 2024 and cumulated over all commercially available SAXS instruments.

A growth in the number of publications is however to be expected as this is the trend, with different rates, for most scientific fields. What is probably more telling of the technique’s popularity is the evolution, within the field of small angle X-ray scattering, of publications employing laboratory instruments. As showcased in Fig. 2, the percentage of publications performed on laboratory sources has consistently risen and accounts today for more than 50% of all publications that include SAXS data.

Fig. 2 Percentage of papers showcasing data collected either wholly or partially on laboratory small angle X-ray scattering instruments from the total number of articles presenting SAXS data. Data extracted from dimensions.ai in March 2024 and cumulated over all commercially available SAXS instruments and synchrotron SAXS beamlines. Data in good agreement with ref. [4].
 

Laboratory SAXS reveals a multitude of information on a variety of materials

The versatility of the technique is proven on one hand by the variety of materials studied and on the other by the multitude of information extracted from SAXS measurements. These are enabled by the capability of the technique to adapt the geometry of the measurement to the different requirements imposed by the samples. A wide range of length scales is available by detecting X-rays scattered into small angles (SAXS) revealing the structure between 1 and a few hundred nanometers or wide angles (WAXS) revealing structural information at the atomic scale. Even though most experiments are performed in transmission mode, as can be deduced from Fig. 3, grazing incidence (GI) geometry can be adopted in order to obtain surface and subsurface structural information or to study the structure of thin films.

Fig. 3 Distribution of measuring techniques used in recent publications. The data has been extracted from approximately 700 publications resulting from data obtained on Xenocs instruments in the period 2016 – 2020.

Fig. 4 shows a selection of samples presented in recently published articles. Not only do these exhibit very different structural characteristics (from biological materials to polymers, nanoparticles, and fibers) but they also cover multiple applications (such as drug formulation and delivery, renewable energy and storage, food, cosmetics, or materials science). This proves that laboratory SAXS plays an important role in the development of multiple research fields.

Fig. 4 Treemap showing the various materials studied with laboratory SAXS. The data has been extracted from approximately 700 publications resulting from data obtained on Xenocs instruments in the period 2016 – 2020.

For each of these samples, SAXS is able to provide a variety of information generally extracted from a single measurement. Fig. 5 displays a selection of information presented in recently published papers. Detailed structural analysis over different length scales plays a crucial role in understanding the interplay between nanostructures and their respective functions which in turn are essential for modern materials development.

Fig. 5 Word cloud showing the various types of information obtained with laboratory SAXS. The data has been extracted from approximately 700 publications resulting from data obtained on Xenocs instruments in the period 2016 – 2020.

Over the past years, laboratory small angle X-ray scattering has seen a steady increase in popularity, a trend which suggests that the technique will continue also in the future to strengthen its position as a standard method for nanostructural analysis touching a myriad of research domains. Given its important research influence on the characterization of materials, SAXS is very likely to play an increasingly impactful role in providing structural information on an ever-increasing array of systems.

Article written by: Xenocs

(www.xenocs.com)

References:

X-Ray Fluorescence (XRF)

What is X-ray Fluorescence?

X-ray fluorescence is an analytical technique that can be used to determine the chemical composition of a wide variety of sample types including solids, liquids, slurries and loose powders. XRF is also used to determine the thickness and composition of layers and coatings. It can analyze elements from beryllium (Be) to uranium (U) in concentration ranges from 100 wt% to sub-ppm levels.

Principles of X-Ray Fluorescence

XRF is an atomic emission method, similar in this respect to optical emission spectroscopy (OES), ICP and neutron activation analysis (gamma spectroscopy). Such methods measure the wavelength and intensity of ‘light’ (X-rays in this case) emitted by energized atoms in the sample. 

In XRF, irradiation by a primary X-ray beam from an X-ray tube causes the emission of fluorescent X-rays with discrete energies characteristic of the elements present in the sample.

Figure, right: Example of the X-Ray fluorescence (XRF) process: 1) Incoming photon 2) Characteristic photon.

Applications of X-Ray Fluorescence

XRF is a versatile analytical technique that finds application across an extensive spectrum of industries and scientific fields. Its adaptability and precision have made it an indispensable tool for understanding and manipulating the elemental composition of materials. From aiding in material identification and quality control in industries to preserving cultural heritage and advancing scientific research, XRF continues to play a pivotal role in enhancing our understanding of the elemental world.

Quality Control and Elemental Analysis

XRF is widely used in quality and process control. Users can quickly get accurate and precise results with limited effort on sample preparation, and it can be readily automated for use in high-throughput industrial environments. XRF’s precision and non-destructive nature make it an invaluable tool for quality control in various manufacturing sectors, such as: 

  • Metallurgy: In metallurgical processes, XRF ensures the integrity of alloys by confirming their composition. It’s a critical step in manufacturing products such as aircraft components, car parts, and structural materials.
  • Electronics: Electronics manufacturers employ XRF to inspect circuit boards, ensuring components’ adherence to strict elemental standards.
  • Cement: XRF is employed in the cement industry for analyzing raw materials and alternative fuels, as well as controlling the quality of the final product.

Research and Development

XRF plays a pivotal role in materials research and development:

  • Material Science: Researchers study the properties of materials and create new compounds (I.e., catalysts or coating materials) by precisely and accurately analyzing elemental composition.
  • Semiconductor Industry: XRF contributes to the development of cutting-edge semiconductors by ensuring the purity and composition of materials used in chip manufacturing.
  • Art and Archaeology: XRF helps conservators and archaeologists analyze pigments, ceramics, and artifacts, shedding light on their origins and authenticity.

Pharmaceuticals and Medicine

In the pharmaceutical and medical fields, XRF also has diverse applications:

  • Drug Analysis: It verifies the quality and safety of drugs and ensures they meet stringent quality standards according to ICH-Q3D. XRF is also used as a quick screening tool before the samples are analyzed by the more labour intensive ICP and AAS methods. 
  • Biomedical Research: XRF aids in studying trace elements in biological samples, offering insights into diseases and treatment.

Instruments with thoughtful innovations

Malvern Panalytical instruments’ have driven XRF innovation in several areas. Elemental analysis instruments can be energy-intensive and generate significant waste, but eco-efficient innovation from Malvern Panalytical has the potential to change this.

We also believe that an instrument should not be complicated to use just because it is powerful, so we have invested in user-friendly features that make method development and data quality management a breeze. With our XRF instruments, you benefit from the optimum combination of technological advancement, thoughtful flexibility, and sustainable performance.

No compromise on quality, speed, or accuracy

Speed or accuracy? There is often a dilemma with XRF spectrometers between quality data that is still usable and rapid results that are detailed enough. With our premium instruments, the trade-off between performance and speed disappears, thanks to innovative features and thoughtful design across our range.

We also offer innovative form factors for a variety of space requirements. Some of our portable and benchtop instruments have accuracy similar to floor-standing XRF instruments.

XRF instruments that can keep up with you

The XRF spectrometers of the past often struggled to keep up with the demands of an ambitious laboratory. Each sample method required extensive training, and the instruments often lacked the sample changer capacity for efficient measurement.

With our instruments, you can count on accurate results and high sample throughput, saving your lab valuable time. Fast feedback loops and a variety of monitoring features across our range further enhance your XRF efficiency by streamlining your workload and simplifying maintenance.

Advantages of XRF analysis

There are many ways to analyze elemental composition in quality control – ICP, AAS, and XRF, for example – and each technique has its advantages. But XRF has a particularly high number of advantages compared with other techniques.

Where alternative techniques often require destructive sampling for the analysis to work, XRF is fast and non-destructive. In addition, analysis can be done in air at the production site, and it’s typically more cost-effective than other techniques.

Blog Written by : Malvern Panalytical Ltd. 
(www.malvernpanalytical.com)

DRI: the ‘direct’ route to greener steel

Today, directness is more than a virtue – it’s a strategy for success. And even the steel industry is following suit! Solutions such as direct reduced iron (DRI) are helping the industry to confront environmental challenges head-on by providing an alternative method to reduce iron ore, a notoriously energy-intensive process. With steel producers striving to reduce carbon emissions, evolving technologies and efficient methods are at the forefront of this revolutionary shift.

Taking the first step

Maximizing energy efficiency in steel production not only saves energy (and costs!) but significantly reduces emissions that damage the environment. Accurate process monitoring, using versatile technologies like X-ray diffraction (XRD) and pulsed fast and thermal neutron activation (PFTNA) on-line, can play a crucial role in optimizing both energy use and process efficiency. This is a great ‘first step’ for many production operations. These on-line tools can be used to create immediate impact within existing setups as drop-in solutions, speeding up analysis that was previously done manually, or improving blast furnace efficiency through more stable feeds. Later, the same solutions can form part of a new or updated process that is designed for greater sustainability in future and incorporates new methods.

The direct route

But how to get from this first step to a more futureproof setup? The industry’s pivot toward carbon neutrality is leading to the development of new technologies and carbon-free steel production methods – and DRI is quickly becoming a key player in this green revolution. By requiring both lower operating temperatures and much less (or no) coke during the iron reduction process, DRI represents a significant improvement in both energy consumption and emissions. It also represents a great ‘direct’ route to more sustainable operations due to its versatility.

In DRI processes, coke or another carbon reductant is replaced by a reducing gas, such as H2. Iron ore pellets are reduced in a shaft furnace where the temperature can be relatively low – in the region of 800° C. Depending on the production setup, the DRI can then be fed either into a blast furnace as hot briquetted iron (HBI), in which case the blast furnace runs much more efficiently and uses less coke, or into an electric arc furnace (EAF).

Even while still relying on the blast furnace, DRI helps to significantly mitigate the environmental impact of this famously resource-hungry process – offering a way for producers to begin making progress quickly toward sustainability goals. When the EAF is used, this offers the opportunity to make the entire primary steelmaking production chain carbon neutral by powering the furnace with green electricity.

How efficiency unlocks the future

And process efficiency is no less relevant during this process than in the ‘old fashioned’ approach. Running both blast furnaces and EAFs at maximum efficiency will make a big difference to energy consumption – and this relies on smart monitoring.

XRD gives insight into critical parameters such as metallic iron content (Femet), metallization (Metn), total carbon content (Ctot), and mineralogical phase content. One case study demonstrated that these parameters could be derived from a single five-minute measurement taken on an Aeris Metals edition XRD. By providing quick and precise control of these parameters, XRD removes the ‘brakes’ that could slow down the uptake and future potential of greener methods like DRI – and unlocks many other efficiencies throughout the steelmaking process.

Taking the direct approach together

The future of steelmaking is here – it’s efficient and green. With DRI processes as a great example and advanced technologies providing critical support, we’re witnessing a paradigm shift in the industry. The path to sustainable steelmaking is ‘direct,’ and it’s a journey we’re committed to navigating together.

Throughout the entire steel value chain, from raw material to steel and coating, cutting-edge technologies and efficient process monitoring are shaping the journey towards sustainability. Malvern Panalytical is leading this transformation by providing a blend of expertise and innovation for a greener future in the iron and steel industry – so, get in touch today to discover how we could bring the green transformation to your processes!

Blog Written by : Uwe König, Tuesday,15 August 2023
(www.materials-talks.com)

Enhancing Manufacturing Processes through XRPD Analysis: A Comprehensive Review

The 1980s is an iconic decade for many reasons – but it wasn’t all big hair and neon fashion statements. This vibrant decade also gave us the earliest form of additive manufacturing (AM), the innovation that would become what many know today as ‘3D printing’. It might seem like a slow start – but technology is quickly catching up to AM’s potential.

Process control is vital in Additive Manufacturing

Increasingly, AM is being used to create spare parts and fixtures for manufacturing machines, revolutionizing custom tooling. AM also has great potential to create critical parts for aerospace and medical applications. But any flaws in these parts could have catastrophic consequences, especially in safety critical applications. Process control couldn’t be more crucial – especially materials analysis when working with metals.

The solution here might seem obvious to anyone with a background in metallurgy: X-ray diffraction, the industry standard, is a tried-and-true method for characterizing materials. Unfortunately, there’s a catch.

The particle statistics problem

X-ray diffraction (XRD) analysis relies on measuring the angle of diffraction as X-rays pass through a sample, characterizing its crystalline structures. But the ideal sample for XRD has a grain or crystallite size of less than 1 µm, while AM often produces parts with grain sizes of 100 µm and larger.

At this size, XRD can struggle to give useful data. This is illustrated below in Figure 1 below, which shows (left) that the standard error increase with crystallite size, and (right) that larger crystallite sizes tend to give a spotty diffraction pattern instead of a continuous arc of intensity. Note a grain and crystallite are not necessarily the same (a grain can contain several crystallites) but larger grains generally have larger crystallites.

The problem, often known as ‘particle statistics’, is that XRD only measures a small number of crystallites in a sample – they aren’t all oriented correctly to ‘catch’ the radiation. The bigger the grains and crystallites, the fewer there are overall; so in a sample with large crystallites sizes, fewer will contribute to the measurement. This makes both peak intensity and peak position measurements much less accurate, producing errors in lattice parameter and residual stress calculations.

Traditional solutions to this issue often assume you’re working with a powder, which could be ground more finely or sieved. But when analyzing AM parts, techniques suitable for powders aren’t an option. Spinning or oscillating the sample can help, but this is difficult when the specimen is large or has a complex shape – which is often the case, as AM specializes in complex shapes!

Better data from the same resources

So, the question is how to improve the results with common resources. Our new white paper ‘…..’ shows that that the quality of data produced can be significantly improved through a couple of techniques available to standard instruments. By using a wider divergence slit to increase the irradiated area and the rocking angle of crystallites, and using a linear or area detector in scanning mode, unusable data can be improved to become useful.

One of the most noticeable improvements is when a larger X-ray beam is used, as it directly improves the crystallite (particle) statistics. However, when this is not a viable option, using a scanning detector mode increases the effective crystallite rocking angle and improves the crystallite statistics. In effect, the result is the same as oscillating the sample. Both solutions reduce peak errors, giving a clearer picture overall.

In times of change, versatility is key

These solutions may need some creativity, but they don’t call for entirely new resources. The study was carried out on one of our Empyrean X-ray diffractometers and made use of its in-built functionality to test each solution. The Empyrean range is known for its versatility – its modular design and multipurpose features have made it popular in both research and process control – and is created to last much longer than a single project or industry trend.

As AM and wider industry practices continue to evolve as part of Industry 4.0, these adaptable solutions will be the key to making the transition smoother. At Malvern Panalytical, we specialize in analytical instruments that prepare you for the future – while improving your current processes too. We can’t wait to see the full potential of AM as it develops, and we’ll be there to support the industry every step of the way!

Blog Written by : John Duffy , Friday 23 June 2023
(www.materials-talks.com)

The gold plant of the future

Kenneth deGraaf paints a picture of highly sophisticated gold plants that can provide improved sampling and ESG outcomes, thereby helping to meet the ongoing demand for gold that is processed safely, efficiently and sustainably.

Why is now the right time to be talking about harnessing technology to get the most out of gold processing plants?
Kenneth deGraaf (KD): Gold processing plants are operating in an increasingly challenging environment with regards to energy, labour and environmental, social and governance (ESG) considerations. We are also seeing average grades of new deposits continuing to decline.

Optimising operations over a range of sometimes competing objectives requires the best available technology and trained personnel to operate and maintain plants. None of this has a simple answer, and the challenges are often site-specific. But harnessing the most advanced yet acceptable technology should always be a component of getting the most out of any mineral processing plant.

In your presentation at Gold Plant, you talked about the importance of correct sampling practice – can you please explain why this is critical for plant operators to get right? What sort of value can proper sampling provide?
KD: In a gold processing plant, if you don’t have accurate information on how much gold is entering and leaving the plant through various process streams then you will not know whether your plant is operating efficiently or if it is optimised.

What’s more, it is not enough to know how efficiently the plant is recovering the gold product – it is often important to know what deleterious elements the plant may also be processing and releasing into the tailings. It can also be very important for the tailings management team to know if desliming of tailings is meeting particle size specifications for the tailings storage facility. All of these require accurate sample collection and analyses.

How can laboratory automation improve plant optimisation and productivity?
KD: It is often overlooked that the largest errors in analysing any process stream containing solids (dry or slurry) occur in the initial collection of a sample and the subsequent sample preparation steps (crushing/splitting/pulverizing), not the actual analysis of the sample (fire assay or ICP analysis).

Properly selected and installed automated sampling systems that adhere to the Theory of Sampling are imperatives for unbiased accurate sample collection; it is physically impossible for a human to consistently collect unbiased samples from the usually large process flow streams in modern gold processing plants.

Once the samples are collected, consistent proper sample preparation is essential for maintaining the representativeness of any sample collected from a process stream. Automated sample collection and automated sample preparation laboratories deliver consistently more reliable samples and dependable sample preparation, which in turn provides reliable data for assessing plant performance and optimisation strategies.

Can you provide a real world example/case study of such a laboratory?

KD: FLSmidth has been involved in more than 90 per cent of the global robotic mining laboratories representing over 250 installations, so there are multiple examples/case studies to show the benefits of automated sampling and laboratories. Automated laboratories have been shown to reduce operational costs, enhance quality of analyses, deliver quicker turnaround of analytical results, and also deliver benefits regarding ergonomics, health and safety for plant personnel.

How do resource professionals fit into automated plants – what skills do they need and how will they continue to help deliver business improvements?
KD: For metallurgists and plant engineers, an automated plant would allow for more sophisticated and prompt analyses of operational parameters and the optimisation of process parameters and production. These would likely lead to improved recoveries, reduced reagent consumption/wastage, and lower energy and water consumption.

How might the resource plant of the future improve overall ESG outcomes?
KD: The resource plant of the future should improve overall ESG outcomes by reducing water wastage, reducing energy consumption and reducing emissions – both from fossil fuel usage and from reduced reagent usage. FLSmidth has its ‘Mission Zero’ initiative with the goal to deliver solutions in mining processes to manage zero-emissions by 2030. It’s an ambitious goal that we have proudly committed to that requires a paradigm shift in collaboration, innovation and adoption of new technologies in the mining industry.

Written by: Kenneth deGraaf, FLSmidth’s Global Product Line Manager. Originally published by: AusIMM Bulletin. Posted in: FLSmidth (www.flsmidth.com)

Cementing a great relationship: How X-ray fluorescence and X-ray diffraction go hand-in-hand in cement production

If you’ve ever baked a cake (or watched a baking show), you’ll know how important it is to use the right ingredients in the right quantities. Otherwise, your cake won’t taste very good – and it might not even look like a cake at all! (We’ve all been there.) But imagine if you were describing a list of baking ingredients to a robot, and said ‘sugar’. The robot might choose raw sugar cane, sugar syrup, or sugar lumps. They’re all sugar, after all – just in different forms!

So, the form or state of the ingredients is equally important information to know as what they’re made of. This is quite obvious when you’re working with delicious cake, but it becomes much trickier when you’re working at the microscopic level with individual elements.

Balancing the elements with XRF

In cement manufacturing, the final properties of the cement are affected by its chemical composition. The raw materials are limestone (the calcareous raw component containing CaO – typically around 85%), shale or clay (the argileous component containing SiO2, Al2O3 and Fe2O3 – around 13%), and additives (SiO2, Al2O3 and Fe2O3 at <1% each), which are crushed into powder and mixed to form raw mix. At this point, it’s vital to monitor exactly how much of each material is in the raw mix to keep the correct balance – and this careful monitoring continues throughout the production process using X-ray fluorescence, or XRF.

In fact, there is a whole array of oxides and elements to keep track of. For example, MgO should not exceed 4-5% to avoid cement expansion, alkalis (K, Na) can affect both kiln operation (build-ups) and product quality, and sulphurs can create setting issues and build-ups when present in excess (limited gypsum additions). The typical ratio of alkali to sulphur needs to be kept between 0.8-1.2 (molar). Finally, chloride content must be less than 0.02% to avoid serious build-up problems. XRF analysis is the best way to monitor all these various components, and has been used for process control in cement manufacturing for many years.

This mixture is fired in a furnace, where the heat causes the calcium carbonate of the limestone to decompose into calcium oxide. This part of the process releases carbon dioxide (CO2) along with other by-products – another good reason to ensure all the ratios are precise, as minimizing CO2 emissions is important both to reduce environmental impact and to comply with regulations. It’s also important to control the potentially hazardous elements in alternative fuels, which are increasingly being used to heat the kiln using recycled waste materials. These can cause other emissions that also have a negative impact on the environment.

Completing the picture with XRD

But while all this elemental composition data is invaluable, more information is needed. In our cake analogy, we know we need sugar, but we don’t yet know which form it should be in. That’s where X-ray diffraction (XRD) comes in.

XRD has been traditionally used to catch any instances of early hydration in the final cement product, but it can also be used for process control. Today, XRD is being used more and more often to control the mineralogy of cement clinker, as it identifies the crystalline phase of each component at key stages such as CaCO3, CaSO4, CaSO4.1/2H2O, CaSO4.2H2O, quartz, free lime, free magnesia (periclase), clinker phases and other mineral phases in conventional and alternative raw materials. The Rietveld method allows a complete quantitative picture of the crystal phases in cement, including polymorphs of alite and belite, along with free lime, calcite and calcium sulphates.

This is the key information that was missing before, giving deeper insight into the product as a whole and allowing a more holistic monitoring and control process. Increasingly, data from XRF and XRD are combined into a single report throughout the production process of cement and concrete, providing a well-rounded overview of both elemental composition, crystalline phase, and quality.

By combining XRF and XRD, it’s much easier for manufacturers to control the quality and final properties of their cement and concrete from an earlier stage in the process. This reduces waste, as any anomalies are picked up earlier, as well as making kilns more efficient and saving energy and CO2 emissions.

Smart systems for future-proof processes

A highly accurate XRF spectrometer like Malvern Panalytical’s Zetium pairs well with a compact and robust XRD instrument, such as the Aeris. The benefit of using these together is that they both support automation using the Universal Automation Interface, and Malvern Panalytical offers support and guidance from initial setup to advice on sample preparation and technical assistance. Our instruments are suitable for use from a busy production environment to a laboratory, and can also be integrated into laboratory information management systems (LIMS).

Written by: Murielle Goubard, Posted by: Malvern Panalytical (www.materails-talks.com)

Digging into rare earth elements: Mineralogical analysis with XRD

Contrary to what their name suggests, the 17 rare earth elements (REE) are not all that rare. In fact, they can be found in many minerals, and are often helpfully gathered together – but they occur in such small concentrations that they’re hard to isolate. So why go to the effort of trying to extract them?

To answer that, we need to understand why worldwide demand for REE has boomed in recent years (according to the US Geological Survey, REE mine production more than doubled between 2017 and 2021, to around 280,000 metric tons). Quite simply, it’s because REE are essential for the technologies that underpin today’s (and tomorrow’s) society. The elements that make up this group are used in everything from the everyday to the futuristic, in industries as diverse as electric mobility, wind power, consumer electronics, and defense technologies.

Facing up to the challenge

With demand for REE in applications like catalysts, screens, and magnets on the rise – and recycling rates remaining very low – getting hold of these valuable elements efficiently is becoming increasingly critical. Locating deposits for the most in-demand minerals can be a challenge all of its own, but even after sourcing, rare earth exploration and deposit mining need more frequent, more accurate monitoring solutions to ensure optimal characterization and processing. In turn, this can reduce the costs of reagents and improve the yield from the raw ore feed.

Twice as nice: Combine our XRD and XRF solutions

Malvern Panalytical’s Aeris Minerals edition provides the mineralogical insights mine operators are looking for. Using the power of X-ray diffraction (XRD), it enables operators to understand the qualitative and qualitative composition of complex REE-bearing minerals, including bastnäsite, synchesite, monazite, xenotime, florencite, eudialyte, catapleiite, aeschynite, and samarskite. With this intuitive compact machine, users can rely on high sample throughput with rapid analysis and maximum uptime. 

Better still, the Aeris is perfectly complemented by the Minerals edition of our Zetium X-ray fluorescence (XRF) spectrometer, the ideal solution for elemental analysis of geological materials. The Zetium Minerals edition has been designed to deliver superior analytical performance and stability, even in demanding mining environments. 

Together, the Aeris and Zetium Minerals editions support speedy, informed decision-making – giving your REE operations the edge and helping you mine those rarest of elements: time and cost efficiencies!

Written by: Uwe Konig, Posted by: Malvern Panalytical (www.materials-talks.com)

Why iron ore pellets are good news for sustainable steel

What does your kitchen sink have in common with the Burj Khalifa skyscraper in Dubai? They might be on a slightly different scale, but they’re both made of steel – the metal that supports our society. Without the steel industry, our world would look very different. But as economies around the world turn toward sustainability with increasing urgency, the steel industry is faced with the challenge of keeping pace. 

Supporting society in a new way

Achieving carbon neutrality by 2050 – the ambitious target set by many governments – won’t be easy for any of us, but the steel industry is facing one of the biggest challenges of all. Partly, this is due to its size: during 2020, about 1,864 million metric tons of crude steel were produced. At this scale, serious environmental impact is guaranteed using traditional production methods. The sintering phase is particularly well-known as the most energy-intensive and polluting step in the entire process. Society needs the industry’s support in a new way today: through rapid change. 

However, the huge scale of the steel industry could prove to be its biggest asset in the race to sustainability. Working at scale means that small changes have big effects – it’s the reason that process efficiency is so important. Each improvement has a big impact, which makes each step very meaningful. 

The sinter solution

Manufacturers have already begun to focus on sinter as the focus to start cutting emissions, and pelletized iron ore offers an innovative solution. Pellets reduce the amount of coking coal required and improve furnace productivity, reducing CO2 emissions in the process. By replacing sinter with high-grade pellets, traditional sintering can be skipped entirely – with electric arc furnaces (EAF) taking the place of the blast furnace, and direct-reduced iron (DRI) as an alternative feed material to steel scrap. This method is known as DRI-fed EAF, and it’s widely considered one of the best ways for the industry to reduce emissions. 

DRI-fed EAF offers a practical and hopeful solution to manufacturers at a time of pressure, which is why many have already made the switch. But process control is just as important in this more sustainable method as in the past, as manufacturers need to keep quality high and their furnaces running as efficiently as possible.  

Preparing for Industry 4.0

Process control in metal production relies heavily on analysis, and precision is key. To reduce waste, keep costs low and ensure quality, manufacturers need to understand every property of their materials, from their mineralogical phase and crystalline structure to particle size. This has always been the case when working with sinter, and it applies to iron ore pellets too. Any efficiencies gained can be lost again if materials are ‘off-spec’.

Tools such as X-ray diffraction (XRD), X-ray fluorescence (XRF) and laser diffraction analysis are already widely used and will only become more important in the transition to carbon-neutrality. But the days of laboratory testing and unrepresentative sampling are over – at least, in optimized production environments. Often called ‘industry 4.0’, automated solutions and high-throughput analysis are presenting manufacturers with another valuable way to maximize their efficiency and reduce their environmental impact.  

Futureproof tools

Instruments like the AerisAxios FAST and Insitec ranges from Malvern Panalytical are helping metals companies keep up in the sustainability race and future-proof their processes. With automation options and high-throughput capacity, they offer expert analysis at the speed the modern industry demands – saving time, resources, and costs. In a rapidly evolving steel landscape, better analysis is a trustworthy guide. 

We’re proud to be helping make the transition to automation and sustainable practices smoother and easier.  

Written by: Uwe Konig, Posted by: Malvern Panalytical (www.materials-talks.com)

Discover how an X-ray diffractometer can automate thin film metrology processes – Q&A

If you would like cleaner, quicker, and more efficient wafer analysis with your X’Pert³ MRD XL X-ray diffractometer for thin film metrology, our recently launched MRD XL Automation tool might just the answer you are looking for. By communicating closely with the host computer with the widely used SECS/GEM protocols, this MRD XL can be automatically controlled, adapted, and efficiently managed throughout the research or production process – from initial wafer selection to results distribution – to meet all your needs.

To engage with our partners and provide insights into how to effectively automate your thin film metrology processes, we recently hosted a live webinar. If you missed it – no worries. You can find the recording here. We’d also like to share some of the most relevant questions we received, as well as our answers…

In the analysis automation can limits be set where any values outside a certain range are flagged with the area on wafer highlighted but do not stop the process?

There are several routes imaginable to achieve this. Firstly, in the host. Secondly, in an analysis script on the local PC. To provide a precise answer, we would need more case-specific information, but there are definitely opportunities for outputting the requested information.

Can I treat reciprocal space mappings in an automated fashion and process the results?

Yes, AMASS (our analysis package) enables complex peak finding and labeling processes and has extensive options regarding its automation via its language-agnostic interface.

Where do you keep measurement data?

By default, the data is stored on a local PC but storage on a file server is also possible. As scripting is part of the solution the opportunities to do this is virtually unlimited.

What’s the maximum and minimum scan areas? And what are the max number of spots on wafer that you can set for automation?

A 200mm wafer can be fully mapped. A 300mm wafer can be handled by automation, but only partially mapped. We have experience with 3-digit numbers of spots for measurements and see no reason for a limit that will be reached in practice.

Written by: Tom Gorter, Posted by: Malvern Panalytical (www.materials-talk.com)

How lower energy use is becoming more accessible in mining

How did you get to work today? Whether it was in an electric car or on a train powered by renewable electricity, the energy transition is already happening all around us. But reshaping the infrastructure of our homes, workplaces, and industries to become more sustainable will take a lot of work – and a lot of metal.

Powering the energy transition…

It’s projected that up to three billion tons of metal will be needed to support the net-zero targets adopted by many countries and industries. Good news for metals prices – but also a dilemma, as the industry takes on sustainability challenges of its own and seeks to reduce its environmental impact.

Accounting for around 3.5-4% of the world’s energy use, the mining industry is a significant player in worldwide consumption. Many mining processes are inherently energy-intensive, and more sustainable alternatives are not yet available. With many companies having made sustainability commitments ahead of 2030, time is short.

…while decreasing our energy consumption

Accurate elemental analysis provides a flexible, immediate solution to this challenge. Better elemental analysis can be applied from the stockpile to the blast furnace to unlock significant process efficiencies. As the demand for metals continues to spike – those three billion tons will be needed soon! – inefficiencies that might have gone unnoticed before will make themselves felt, but the ability to sort ores easily and in real time can transform the entire metals value chain.

Sorting ores allows the direct detection of any variations or anomalies in ore composition, which makes stockpile management much more efficient. Controlling washing and preventing the processing of waste material saves significant time and energy, and ensures higher consistent quality.

Having ores sorted from the beginning of the process also makes later stages run more smoothly, compounding the benefits downstream. A more consistent output means that fewer additives or corrections will be needed, and eventually can enable more efficient running of the blast furnace – the most visible point of energy consumption.

What do we mean by ‘better’ analysis?

The most immediate way to make analysis more efficient is to get results in real time. Cross-belt analyzers eliminate the need for sampling, saving both time and costs. Analyzing all the material on the belt – from large rocks to fines – means that results will always be representative, and any adjustments needed can be made instantly rather than after testing is carried out elsewhere. The CNA cross-belt analyzers from Malvern Panalytical are designed to accommodate a wide range of belt sizes, making them suitable for many different applications.

At the smaller scale, the CNA instruments make use of pulsed fast thermal neutron activation (PFTNA) technology, using a pulsed flow of neutrons to interact with the nuclei of the atoms in the passing material. The atoms emit gamma rays, and the instrument measures the characteristic energy levels of these rays to identify and quantify the elemental composition of the material.

CNA instrument in the Nickel mining plant

Highly accurate, this method is also very safe for operators. The neutron-emitting module can be switched off during downtime or for maintenance, minimizing their exposure to radiation, and saving precious time on administration and compliance procedures to comply with safety regulations. There’s also no hazardous waste, making PFTNA significantly more sustainable in the long term.

 

Can this be applied across the industry?

PFTNA technology can be applied across a wide range of mining and metals applications, including in the processing of iron ore, bauxite, coal, copper, nickel, and limestone. The CNA analyzers from Malvern Panalytical come in a variety of industry-specific formats, with designs tailored to the specific ore to ensure the greatest efficiency gains possible. They’re flexible in calibration and particle size, depending on the application, and their robust design keeps the cost of ownership and maintenance low.

So, the dilemma of supporting the energy transition while lowering energy use doesn’t have to be a dilemma at all – it can be an opportunity! Thanks to technological innovations like PFTNA, mining and metals can find a way forward that swaps challenges for benefits.

 

Written by: Uwe Konig, Posted by: Malvern Panalytical (www.materils-talks.com)