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New applications of ceramic multilayers, for example, in biotechnology, sensor technology, and chemical micro-reaction technique, call for cavities with complex geometries. Hot embossing offers a promising, cost-effective way to generate these structures on the surfaces of green tapes or laminates. Cavities inside low-temperature co-fired ceramic multilayer were manufactured by a combination of hot embossing, lamination by a special adhesive technique, and zero shrinkage sintering. The edge and surface quality in the green state as well as the sintered multilayers with surface structures and cavities were extensively characterized by laser surface scanning, optical and ultrasound microscopy. Sintering shrinkage of hot-embossed laminates could be reduced in the x and y directions to less than 0.5%.
Presented are results of an inter-laboratory study (ILS) for measurements of the particle size distribution of fine powders in wet dispersion by laser diffraction. In this proficiency test 32 participants from four countries took part. They utilized 13 different devices from 7 manufacturers.
Three commercial powders (glass spheres and two silicon carbide powders) showing a median diameter of about 30, 10 and 1 µm (volume distribution), respectively, were chosen for the procedure. A homogeneity study was carried out after the units had been separated and bottled.
All participants received their test samples including a description of the standard operating procedures based on ISO 13320:2009 – to ensure that experiments were performed in a consistent manner. Results were calculated using the Mie Theory. The general means and the precision of the results were estimated in accordance with ISO 5725-2:2002.
The evaluation showed excellent values of repeatability standard deviation. Values of 4 to 21?% of the reproducibility standard deviation of the results were found in the particle size range above 1 µm. Much larger deviation between the labs was detected in the case of smaller particles. Differences in the design of the analyzers were unambiguously identified as the main reason for the large deviations.
This is the final report on the proficiency test (PT) „Measurement of the particle size distribution of ceramic powders by laser diffraction”. The PT was organized by the Federal Institute for Materials Research and Testing (BAM), division 5.5 “Advanced technical ceramics”. The measurements took place from 12/2021 to 03/2022. The aim of the interlaboratory comparison was the proficiency assessment of the participating laboratories.
Management and realization of PT were performed in accordance with DIN EN ISO/IEC 17043:2010.
The basis of the harmonized measuring procedure and the instructions for the interlaboratory comparison was the standard ISO 13320:2020.
The statistical analysis was performed in accordance with DIN ISO 13528:2020 by use of the software PROLab Plus (QuoData GmbH, Dresden, Germany).
A group of 44 laboratories from 17 countries participated in the PT. Laser diffraction analyzers produced by 7 different manufacturers were used. The three test materials were commercial products. Overall, the measured characteristic values of the particle distributions (d10, d50 and d90) were in the size range between 0.5 and 25 μm. The final report contains all individual results in an anonymous way.
The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019).
The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services.
Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider.
The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics.
The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS.
The information contained in this document is structured in 3 main sections, as follows:
• Catalogue structure. This section describes in short the main characteristics of the CoS 2019.
• Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019.
• Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties.
Spray drying is a widely used process step in ceramic technology to
convert fine grained raw powders to free-flowing granules. Type and
amount of the organic additives (dispersants, binders and plasticizers)
define viscosity and stability of the slurry, the granulate structure and
the compaction behaviour.
Alumina and Zirconia powders were characterized with regard to
particle size, shape and specific surface area (BET). Zeta-potential
measurements by Stabino® were used to investigate the effect of
different dispersants on slurry stability. Unfortunately, this method is
restricted to suspensions with less than about 30% by weight of solid
content. The multi-sample analytical centrifuge LUMiSizer® overcomes
this problem. This device enables analysis of the separation behaviour
of suspensions over a wide range of solid content. On the basis of
position and time resolved photometric detection of transmitted light,
it is possible to determine the instability index, the sedimentation
velocity, and the sediment height in dependence of type and amount
of organic additives at various centrifugal accelerations. Additional
information is obtained from the shape of the transmission profiles.
Based on LUMiSizer® measurements, suitable additive concentrations
were derived. Thereby, the number of investigations by viscometry and
spray drying experiments can be significantly reduced.
Finally, it was possible to produce alumina, zirconia and ZTA aqueous
slurries with up to 80 weight-% of solid. The optimized suspensions
were successfully spray dried and the resulted granules show good
compaction behaviour.
Novel approaches of tunable devices for millimeter wave applications based on liquid crystal (LC) are presented. In the first part of the paper, a novel concept of a tunable LC phase shifter realized in Low Temperature Cofired Ceramics technology is shown while the second part of the paper deals with a tunable high-gain antenna based on an LC tunable reflectarray. The reflectarray features continuously beam scanning in between ±25°. Also first investigations on radiation hardness of LCs are carried out, indicating that LCs might be suitable for space applications.
The EU recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. Within the European Project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nanomaterial or non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered.
One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nanomaterial or non-nanomaterial. The correct identification of a nanomaterial by VSSA method (positive test) is accepted by the EU recommendation.
However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape. For particles containing micro-pores or having a microporous coating, false positive results will be produced.
Furthermore, broad particle size distributions – as typically for ceramic materials – as well as multi-modal size distributions make necessary to adjust the threshold.
Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and
improve the method.
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming (SEM, TEM).
Within the European project NanoDefine (www.nanodefine.eu) a two-tier approach has been developed, whereby firstly a screening method is applied for the rough classification as a nano-/non-nanomaterial, and for borderline cases a confirmatory method (imaging methods or field flow fractionation) must be considered.
One of the measurement methods well suited to particulate powder is the determination of volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The correct identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method is associated also by some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions of the particles. For particles containing micro-pores or having a microporous coating false positive results will be produced. Furthermore, broad particle size distributions make necessary to adjust the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach will be tested (in relation with SEM and TEM measurements) in order to expand the actual knowledge and to improve this good available and agglomeration tolerant method.
If the particle size decreases, the ratio of surface area to volume increases considerably. This provides benefits for all surface-driven processes that run faster or at lower temperatures than larger particles. However, handling and characterization of the nanopowders are much more difficult. Particularly polydisperse powders with irregular shape, as grinding products, represent a challenge. Granulometry in the submicron and nanoscale often leads to incorrect results without knowledge of particle morphology.
This presentation demonstrates potentials of using the volume-specific surface area (SV or VSSA) in the granulometric characterization of nanopowders, for instance, correlations between the volume-specific surface area and the median particle size are discussed considering the particle morphology and the model of the logarithmic normal distribution.
Moreover, the presentation deals with the optimal dispersion of nanopowders during sample preparation. Indirect ultrasound device with defined cooling was developed to prevent both contamination by sonotrode abrasion and sample changes by heat.
Successful granulometric characterization of nanopowders demands both improved dispersion technology and very often an effective combination of two or more measurement methods.
This chapter first gives an introduction to the concepts of SSA and volume-specific surface area (VSSA) and an outline of the BET method. It continues with a discussion of the relationship between particle size, shape, and the VSSA, followed by an overview of instrumentation, experimental methods, and standards. Finally, sections on the use of the VSSA as a tool to identify nanomaterials and non-nanomaterials and its role in a regulatory context provide some insight on the importance of VSSA in the current Regulation of nanomaterials.