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Introduction
As so many 3-D products are created from powder particles, the shape and size of these particulates can have a great impact on the physical and chemical properties of the final product. Analysis of the size distribution and shape of the particles can also give useful information concerning the processes they go through in manufacturing, and can help make these processes more efficient as well as, of course, helping to solve problems. This is of particular importance in the field of medical materials and devices, as processing control for materials that enter the body is vital. This white paper will discuss laser diffraction, a well-known method for measuring particle size distribution (PSD). As well as describing the theory behind it, the paper will focus on how important laser diffraction can be to the field of medical materials.
modal particle size, and the d10, d50 and d90 values. These values represent the sizes (in microns) at which 10%, 50% and 90% of the total particles has a smaller size, and are often used as standards in QC work. The second green line is the cumulative volume, which shows the amount of particles in total that are under any given size. It is important to appreciate that these curves can also take the form of volume or number distributions, and care needs to be taken when selecting which to use. If particle size is small, e.g. sub-micron level, then a number distribution will provide more accurate information as each particles contribution to the overall volume is small. Conversely for larger particles, a volume distribution would give more accurate results4.
Incident Light
Incident Light
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Once the measurements have been taken, a mathematical process based on the Mie theory takes these values and predicts the scattering of light at all possible angles. According to ISO13320-1, this is the best method for particle sizes less than 50m (below sieve measuring limits). Another theory that was widely used, the Fraunhofer approximation, only accounts for classical diffraction around the particles and assumes that they are opaque, whereas the Mie theory takes the refractive index of the particle into account. The Mie theory requires knowledge of the particle and dispersant refractive indices, as well as the imaginary particle refractive index, all of which can be obtained from the apparatuss database. If a materials RI values are not listed, the values can be estimated and then edited later on depending on their fit with the data. There needs to be good agreement between the so-called residual values, the difference between the actual measurement and the predicted data. However, it must be noted that a good data fit does not necessarily give a correct result4.
in conjunction with previous ones - The Role of Zeta Potential in the Manufacture of Healthcare Materials and The Applications of Zeta Potential in Process Control on the Ceram website. An example of the link between zeta potential and PSD is shown in some testing work carried out for a client on titania powders. The initial experiments showed that the titania particles were flocculating and giving a misleading merged bi-modal distribution. After conducting zeta potential vs pH measurements and then mixing in a small amount of a suitable anionic surfactant, PSD measurements gave a distribution with one, much sharper peak at the lower particle size rather than two. The surfactant had the effect of increasing the surface charge of the particles, and subsequently their zeta potential. This meant that the particles possessed enhanced electrostatic repulsions (versus Van Der Waals forces) leading to no flocculation6.
Conclusion
While it may seem initially like a relatively simple routine characterisation test, measuring the particle size distribution of a solid powder can be challenging. When performed correctly however, it can give a lot of information that informs powder processing and so end-product performance. This is vital for a wide range of industries, and Ceram can help ensure that clients materials are of the right specification for their needs.
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References
1. Work done at Ceram in 2013 for a client, investigating the particle size distribution of a range of different biomaterials. 2. Good Practice Guide for Improving the Consistency of Particle Size Measurement, K Mingard, R Morrell, P Jackson, S Lawson, S Patel and R Buxton, National Physical Laboratory Publications (2009) 3. Malvern Instruments MS3000 Customer Training Course, Part 1 Basic Principles and Data Quality (2012) 4. Malvern Instruments MS3000 Customer Training Course, Part 2 Obtaining and Understanding the Size Distribution (2012) 5. Malvern Instruments MS3000 Customer Training Course, Part 3 Method Screening, Wet Measurements (2012) 6. Work done at Ceram in 2012 for a client, investigating the particle size distribution of titania suspensions. 7. P. Chean and K.A. Khor, Biomaterials 17 (1996) 537-544 8. M. Monsalve, H. Ageorges, E. Lopez, F. Vargas, F. Bolivar, Surface and Coatings Technology 220 (2013) 6066
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About Ceram
Ceram is an independent expert in innovation, sustainability and quality assurance of materials. With a long history in the ceramics industry, Ceram has diversified into other materials and other markets including aerospace and defence, medical and healthcare, minerals, electronics and energy and environment. Partnership is central to how we do business; we work with our clients to understand their needs so that we can help them overcome materials challenges, develop new products, processes and technologies and gain real, tangible results. Headquartered in Staffordshire, UK, Ceram has approved laboratories around the world.
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