There's no doubt that 3D printing technologies are leading to the next major industrial revolution and that Additive Manufacturing plays a key-role in the Industry 4.0, saving time and costs, being decisive for process efficiency and reducing its complexity, allowing for rapid prototyping and highly decentralized production processes. Currently, more and more industrial segments are adopting Additive manufacturing (AM) : AM allows 3D objects to be manufactured in a completely revolutionary way, adding layer upon layer instead of removing material from a master piece of material. Three main categories of materials can be used in Additive manufacturing: polymers, ceramics and metals. These materials are often produced in powder form, and the physical properties of these powders significantly influence their ability to be processed in AM machines and strongly condition the final product quality. Poor quality of the powder can produce defects in the final component such as pores, inclusions, residual tensions, cracks and surface roughness. Furthermore, a low quality of powder affects the process by compromising the uniformity and flowability of the powder bed. There is a direct correlation between the physical properties of the powder and the performance of process and final components.
The characterization of the powders physical properties therefore allows to optimize the process and improve the final product. It is crucial in different steps of the Additive manufacturing process:
powder production: characterization and quality control of powders produced with different technologies
choice of the best performing powders for processing: definition of the ideal physical characteristics of the powders according to the application field.
input raw material: control of specifications declared by the manufacturer and monitoring of supplies constancy
recycling of waste powder: evaluation of the number of process cycles on the physical characteristics of the powder, in order to reuse powders as much as possible,to lower manufacturing costs.
Which physical characteristics of the powder determine its performance? Both batch and individual particles properties! The ability to flow and to compact at best is crucial to allow consistent dosages and stratifications during process. These properties are directly, although not exclusively, influenced by the particles size and shape, as well as by their surface roughness, bulk density and electrostatic charge. Flowability, compaction density, particle size distribution and particle shape can be assessed quickly and effectively by means of powder rheology, density, laser diffraction and image analysis tests. Alfatestlab provides a complete analytical service to characterize the wide range of bulk powders and particle properties that can have a critical impact on AM processes, thanks to a latest generation technological platform. Contact us to answer your analytical needs
 International Journal of Engineering and Technical Research 8(8):3-8, 2018
The instrumentation in ALFATESTlaballows a complete physical/chemical characterization of pharmaceutical products (active ingredients, excipients, etc.), dry powders (micronized and not only) or wet suspensions/emulsions.
The ability to accurately measure particle size, morphology, BET surface area, density, porosity and water absorption allows to obtain a complete range of information on the pharmaceutical ingredients such as dissolution time, bioavailability, content uniformity, hygroscopicity and to improve the knowledge and efficiency of production processes. Furthermore, the detailed shape parameters, area, porosity and particle size allow to reduce the development time of a new drug and to better protect the intellectual property. Many of these measurements are required by chapters like USP1059 Excipient Performance Chapter.
Suspensions / emulsions
The possibility to measure the particle size, the morphology, the rheological properties, the zeta potential of suspensions and emulsions and verify quickly and objectively the stability / instability (flocculation, coalescence, sedimentation and creaming) allows to optimize the formulations and improve quality, performance and shelf-life. The USP729Globule Size Distribution in Lipid Injectable Emulsionsindicates Dynamic Light Scattering (also called PCS Photon Correlation Spectroscopy) or laser diffraction (also called "classical light scattering") as the techniques for measuring the average diameter of droplets in emulsion. The measurement of foreign particles and contaminants present in injectables (USP788, EP 2.9.19, JP 6.07) is achievable, even on the filter, with great accuracy and reproducibility thanks to automated image analysis instruments present in ALFATESTlab. In addition to the product characterization, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction in emulsions or suspensions to produce stable nanodispersions, perform nano-encapsulation or cell lysis.
In ALFATESTlab, our instrumentation is regularly validated with IQ/OQ procedures and is compliant with most of the industry regulations (US Pharmacopeia, Pharmacopeia EP, JP Pharmacopeia), such as:
Laser diffraction particle size: USP 429, EP 2.9.31, JP 10, ISO 13320.
Automated image analysis: USP 776, EP 2.9.37, JP 3.04, ISO 13322. The measureent with an image analysis system is suggested by USP and EP as the comparison method for sample analysis of non-spherical particle in laser diffraction.
Scanning Electron Microscopy SEM: USP 1181.
BET Specific Surface Area: USP 846.
Mercury intrusion porosimetry: USP 267.
Dynamic Vapor Sorption DVS: USP 1241, the amount of water adsorbed and absorbed by a pharmaceutical product influences the crystallinity of active ingredients (in some cases may induce the conversion into an amorphous material or in a hydrate crystal ), the storage module, the permeability, the melting point and density.
Real density of solids and powders - gas pycnometry: USP 699.
Rotational Rheology: USP 912.
Detailed characterization of the physico-chemical properties of a new formulation, rapid and objective stability assessment allow to accelerate time-to-market of a new product and ensure its quality.
Suspensions and Emulsions
For this type of dispersions, it is fundamental to control interconnected parameters, all able to influence the stability and the final properties of the products, such as: particle size distribution, rheological properties (viscosity and visco-elasticity) and the Zeta potential. In addition to the product characterization, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction and stability improvement of emulsions or suspensions, ideal on a wide range of products including creams, mascara, lipsticks, sunscreens for quality and stability improvement.
The ability to accurately measure particle size, morphology, BET surface area, density, porosity and water absorption allows to improve the knowledge and efficiency of production processes (flowability, uniformity) and the quality characteristics of the products in development.
Inks, paints and coatings
Properties such as coverage power, leveling, adhesion properties, viscosity can perfectly be characterized by rheological measurements, particle size and zeta potential analysis. In addition, the objective stability measurement in short time using light scattering techniques allows to accelerate the product time-to-market. The control of these parameters is crucial also for digital printing inks to optimize the formulations and prevent flocculation phenomena that would affect the print quality. For the latter, in addition to the product characterization, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction, aggregate removal and stability improvement of emulsions or suspensions, to obtain stable high quality inks.
It's well known to all powder coating manufacturers the importance of a careful particle size parameters control for the final product quality. The development of these products, which has also widened significantly the range of applications, has led to the introduction of ever more complex formulations (for example the metallic powder coatings) for which the particle size alone cannot be a sufficient control parameter to ensure quality. Analysis such as morphology and surface area can provide important further information to improve the performance of a powder coating.
The products in the packaging industry include plastics or other materials, that often involve a polymer coating. The properties to be assessed may vary depending on the final use of the products. For example, in the case of food packaging is critical that they don't release smells in foods and beverages. For this purpose electronic noses are of fundamental support. High-resolution images with scanning electron microscopes SEM allow to investigate the quality and defects of the coating.
Properties such as porosity (micro, meso and macro pores), high surface area and particle size (for example in the case where the porous structure uses nanoparticles as precursors) are closely linked to the catalyst activity and efficiency.
Adhesives and Sealants
Rheological properties (viscosity and viscoelasticity) and particle size control along with high-resolution images (such as SEM images) are used to understand the influence of formulation parameters on the product behavior such as the coverage property and / or stability.
Detergents and Surfactants
Particle size and surface area parameters are useful to characterize the powder detergent; zeta potential and rheology analysis allow to determine the CMC (critical micellar concentration) of surfactants, to understand the influence pH and concentration on the micellar size. High resolution images such as SEM images allow to check precisely the detergent ability to remove dirt and preserve the tissues. In addition to the product characterization, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction and stability improvement of emulsions or suspensions.
Some lubricants are made from emulsions that are "sprayed" on metal parts to prevent overheating during operation. The size of the emulsion droplets and their stability (avoiding coalescence and creaming) are fundamental aspects for the efficiency of these products.
In the ceramic industry the porosity of the so-called green body depends strictly on the particle size. If the particles are too large, the structure after sintering will show too large pores resulting in structural fragility of the final product. It is recommended to use polydisperse particle sizes so that the smaller particles fill the gaps left by larger ones. Controlling the presence of agglomerates can avoid defects in the final product.
Properties such as particle size, morphology, porosity, water absorption and rheology have a crucial impact on the performance of products such as cements or mortars and on the evaluation of degradation phenomena from natural stones (marble, stone, granite ...) and artificial materials (mortars, plasters).
Particle size distribution, particle morphology and surface area are parameters that for several reasons influence the cement resistance. Rheological properties characterization can instead help in the understanding of the polymerization phenomena (curing). Finally moisture absorption by buildings may affect their lifetime and should therefore be controlled.
In the metal powders, particle size distribution, morphology, surface area and density may be cause of shoddy compaction and sintering processes. SEM images in high resolution, however, allow an accurate assessment of any imperfections on the final product.
The polymer and plastics field is large and heterogeneous, depending on the applications material characterizations and control may require the measurement of molecular weight and branching of polymers, the measurement of particle size and morphology of raw materials, the use of rotational or capillary rheology for process simulation such as extrusion and molding of plastic materials. In addition, the use of catalysts in many industrial processes of synthesis requires the characterization of their activity and efficiency using surface area, particle size and porosimetry measurements.
In the field of food and drinks product success is often closely linked to quality and safety. Research & development and production are influenced by the interactions between the various raw materials and intermediates. The aspects related to sensory quality, stability, shelf-life or just quality control are very important.
Whether it's solid, liquid, emulsion or gel, ALFATESTLabcan assist customers in assessing the consistency of raw materials, in predicting shelf-life, to optimize grinding and granulation operations, or to accelerate the new formulation testing and new product development.
In addition, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction and stability improvement of emulsions, nano-emulsions or suspensions.
The automotive and aerospace industries are strongly concerned by the quality, energy efficiency and safety of the final products. The development and production of these products are influenced by raw and intermediate materials quality and performances. Controlling rheological properties, particle size, morphology, surface area, porosity, potential zeta, etc.becomes thus fundamental to check the consistency of materials incoming.
There are several applications in the electronics industry where characterization of parameters such as particle size, morphology, zeta potential, rheology and stability of the dispersions is relevant. In the case of Chemical Mechanical Planarization Slurries (CMPs), used for polishing of silicon wafers and more, the chemical-physical properties listed above are critical to obtain a good dispersion and prevent destabilization phenomena (flocculation and sedimentation). The control of these properties (particle size, etc.) remains fundamental as well in the case of nanoparticle dispersions used as a coloring material in liquid crystal displays.
In many countries nowadays the use of heavy metals such as lead, copper, cadmium and mercury is prohibited, and this has had a big impact in semiconductor industry, creating big problems of production: for example, the lead removal from solder can result in a rapid increase in the formation of pond "whiskers" that are a potential cause of electrocution and arc effect in the chip. Collecting high-definition images using SEM allows an accurate control of any imperfection frequently due to failures in electronic devices.
ALFATESTLabcan then be the ideal partner for various characterizations in electronics and semiconductor industries, beyond the examples briefly described.
Petrochemicals are derived from the crude oil refining and are used to produce common and important materials such as organic chemicals, fuels, waxes, polymers, detergents etc. ALFATESTlaboffers a range of analytical techniques to solve many issues related to this wide area.
Asphalt and Bitumen
Asphalts and bitumens are viscoelastic materials consisting of a mixture of aromatic hydrocarbons used as a binder in the roads building, and result in complex colloidal systems with different additives (polymers, oils, pH regulators) which scope is to improve the mechanical properties. ALFATESTlabis able to perform the measurement of rheological properties (Dynamic Shear Rheometer DSR) and apply standard classification methods of asphalts to evaluate their durability and load parameters, in different climatic conditions. In the case of bitumen emulsions, also used as a waterproof coating for different materials, the stability and particle size measurements in addition to the viscosity profile are critical to evaluate the quality of the emulsion.
In addition to the product characterization, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction and stability improvement of emulsions.
They are oil or water-based suspensions with minerals, salts and polymers, used to protect wells and drills during the production of oil and gas. The control of rheological properties (viscosity and viscoelasticity) and stability helps to ensure the ability of the sludge to lubricate at best. Particle size and particle shape are indicators of the agglomerates presence that could cause damage, gas leaks and pore block. In order to prevent the aggregate formation, the zeta potential measurement can help you find the right salt concentration.
Lubricants and greases
The tribological and lubricant properties of industrial greases can be measured at different temperatures and shear rate with a rotational rheometer, allowing the characterization of sedimentation resistance, pumping characteristics, thixotropy index, etc. For emulsions-based or colloidal suspensions-based lubricants, stability measurement is vital in the formulation process and quality control. ALFATESTlaballows a good evaluation of particle size, zeta potential and rheological properties and an objective and rapid measurement of destabilization phenomena (flocculation, cremaggio, sedimentation, coalescence). In addition to the product characterization, ALFATESTlaboffers its customers the innovative laboratory scale process fromMicrofluidicsfor uniform particle size reduction in emulsions or suspensions, to obtain stable nanodispersions.
Measurements on soils and sediments allow a classification based of their physical properties. ALFATESTLabis able to provide:
Rapid determination of sand fractions, silt and clay for the classification of weaving using laser diffraction particle size
Quantitative confirmation of fractions by means of size and morphology measurements using automated image analysis
Evaluation of permeability, porosity and water adsorption by means of mercury porosimetry techniques, helium pycnometry and DVS (Dynamic Vapor Sorption)
Assessment of morphology using high-resolution SEM images
Fuel Cells / Solar Cells
The control of electrode porosity in fuel cells, optimization of rheological properties for screen-printing processes, water absorption isotherms in polymeric membranes used as electrolytes ... are all characterizations that find answer in ALFATESTLab.
Drinking waters are generally treated for both mineral and organic contaminant removal. Typically the objective is to improve the coagulation ability in water treatment plants, using cationic additives as flocculants. The zeta potential measurements provide a valid tool to quantify the optimal concentration of additives necessary for the flocculation and removal of contamination.
The high-resolution images obtained with a scanning electron microscope (SEM) are ideal to verify the presence of micro defects in various industries such as microelectronics, precision mechanics, automotive / aerospace, chemical, metallurgy etc.
The desktop SEM Phenom ProX present in ALFATESTLablaboratory allows to quickly obtain high resolution images for microstructural analysis and quality evaluation of products such as ceramic materials, cement, plastics, dairy, textiles, clothing accessories, etc.
The performance evaluation of a filter or a membrane often requires the characterization of fiber thickness and through-pores size. ALFATESTLabis equipped for these measurements thanks to a scanning electron microscope SEM coupled to a unique software called Fibermetric for automatic measurement of fiber thickness, and to various techniques for pore size distribution measurements.
In many industries, fibers are used according to their applications properties: for instance, fibers with high mechanical properties are used to reinforce materials, unlike those used in textile or medical fields. The choice of fibers material can then be guided by a rheological characterization, GPC and Light Scattering measurements, and subsequent evaluation of fibers can be performed with automated image sistem (Morphologi G3 from Malvern Instruments also uses a shape parameter dedicated to the fibers characterization).
With 'Advanced materials and Composites' we indicate a general category that includes nanostructured materials, eco-materials (ecoplastics, biopolymers etc.), technical textiles, metals and alloys bearing various properties (memory, luminescence, breathable ...), nanofluids, technical ceramics, metal foams and polymers , stickers etc.
For all these products ALFATESTLabmay be a reliable interface for measurements of viscoelastic properties, molecular weights and branching of polymers, particle size and morphology, porosity, and for high resolution SEM images with microanalysis.
A colloidal system is defined as a system in which a material is finely dispersed in another, with dimensions typically below the micron. Nanoparticles are often present in colloidal dispersions and their size directly impacts on the ability of the dispersion to maintain the chemical, thermal, electronic and optical properties. In the study of a colloidal system the surface chemistry plays an extremely important role, and in many industries (pharmaceuticals, cosmetics, ceramics, food, inks and paints, etc.) the long term colloidal stability is of great importance. ALFATESTLab provides a comprehensive framework for the measurement of colloids and nanoparticles size (and formation of aggregates), the characterization of diluted and concentrated colloidal suspensions stability, as well as the measurement of zeta potential and rheological properties (in order to understand the microstructures). In addition to the product characterization, ALFATESTlab offers its customers the innovative laboratory scale process from Microfluidics for uniform particle size reduction and production of stable colloidal systems and nano-dispersions.