Monday. 16 September
Table 1. Characteristic procedurę and obtained rcsults on the cxamplc of ZnO nanopow der
1. Mcasurcd para- |
2. Mcasurcment tcch- |
3. Rcsult |
Morphology visualiz- |
Scanning Electron Micro- |
Agglomerates of single-ciystal nanoparticles |
Phase composition |
X-Ray Diffraction Analys- |
Hexagonal ZnO |
Specific Surface |
BET |
42 m2/g |
Density |
Helium Pycnomctry |
5.1 g/cm5 |
Average particie (agglomerate) size |
Disperswe Light Sculter-ing |
~85 nm |
Nanoparticle Tracing |
~90 nm | |
Zeta-potcntial |
Electrophoretic Light Scattering |
34.7 mV |
morc tlian 1300 nano-goods. produccd by near 600 companics which arc locatcd in 30 countries [ 11. One can find nanomaterials in electronic, cosmetics, fabrics. auloino(ive or medical products. Despite such widespread usage. unlil recently ihere was not current dcfinition of nanomaterials in the framewoik of REACH. Only at lite end of 2011. Europcan Commission adoptcd (lic Rccommcndation on the dcfinition [2], according to which "Nanomaterial" means: “A natura!, incidental or manufactured materia! containing particles, in an unbound stale or as an aggregate or as an agglomerate and where.for 50 Hor morę of the particles in the number size distribution, one or morę external dimensions is in the size rangę I nm - lOOnm". Such dcfinition implics indispcnsablc parameters dcscribing nanomaterials. namely nano-particlcs size and their size distribution. However, product reąuirements or hcalth cffccts. usually dctcrminc other parameters such as: Speciftc Surface Area. particie shapc. surface chemistry. Experiencc has shown, tliat characteristic of nanoparticles is a very compIex issue due to the fact Ihat a large number of different ineasurement techniques are a\ ailablc. Thafs w ity generał standards in the nanoparticle character-ization area were not developed till now. Within the International Or-ganisation for Standardisalion (ISO) there are only standards relating to the specific nanofonns. and particular ineasurement techniques [3, 4], Morę generał standard is plaiuied (o be published only this year |3). Thcrcforc. nanomaterials are usually charactcrized according to guides recommended by Europcan Commission [6,7.8], This practicc is also used in Laboratoiy of Nanostructures of Institute of High Pres-sure Physics. In this aniele characlerization procedurę and adequate characteristic parameters are presented on the cxample of ZnO nano-powder, as a rcpresentativc nanoparticle materiał (see Tablc 1).
Acknowlcdgcmcnts
We would like to thanks to the NANOFORCE project: „Nanotechno-logy for Chemical Enterprises- how to link scientific knowlcdgc to the business in the Central Europę space". implemented through the Central Europę Program co-fmanced by ERDF.
LITERATURĘ
[1] http://www.nanotechproject.org/inventories/consumer/
[2] "Commission Recommcndations of 18 October 2011 on the definition of nanomaterial” (2011/696/EU)”
[3] “ Use of transmission clcctron lnicroscopy (TEM) in wallcd carbon nanotubes (SWCNTs), ISO/AWI TS 10797.
[4] "Characterization of single-wall caibon nanotubes using thermo-gravimetric analysis”, ISO/TS 11308:2011.
[5] "Vocabulary- Part 6: Nano-object cliaracterization". ISO/DTS 80004-6.
[6] "Requirements on measurements for the implementation of the European Commission definition of the term 'nanomaterial". Linsinger T.. Rocbben G.. Gilliland D.. Calzolai L., Rossi F., Gibson N.. Klein C„ JRC Reference Report, July 2012.
[7] "Nanomaterials under REACH - Nanosilver as a casc study”, Proken M„ E. J„ et al„ RIVM Report, 2009.
[8] "Guidancc Manuał for the Tcsting of Manufactured Nanomaterials:
OECD’s Sponsorship Programme: FIRST REVISION".
ENV/JM/MONO(2009)20/REV. 02-Jun-2010.
11:55 Invitedoral
Crystallitc size determination from diffraction data: a do-it-yoursclf tutorial.
Stanisław Gierlolka
Polish Academy of Sciences, Institute of High Pressure Physics (UNIPRESS), Sokołowska 29/37, Warszawa 01-142, Poland e-mail: xrayl@unipress.waw.pl
A method of determination of the size distribution of nanocrystals from X-Ray diffraction data will be presented. A brief introduction into ex-perimental techniques w ill be given and the essential theoretical issues will be explained. A practical demonstration of the data analysis with an application of freely available software will be carried out. Lirnita-tions of the method and possible pilfalls will be discussed. Some par-ticularly peculiar and cliallenging cases of data analysis will be presented.
12:15 Imitedoral
Rcliablc XRD characterization in production or high-throughput laboratory regime
PielaszekResearch (PR), Popiołów lOa, Warszawa 04-847, Poland e-mail: roman@pielaszek.net
In industrial orproject-oriented research laboratories. X-Ray Diffraction (XRD) is often seen as "morę art then science" technique due to
• wide variation between rcsults from XRD vs. well-establishcd metliods (SEM/TEM/DLS),
• large margin for interpretalion. dispules and ambiguities.
• relatively high costs.
Indeed. within nanomaterials research area. therc arc legilimate rcasons to think so. as nanocrystals violate assumptions of a number of estab-lished diffraction theoremsdriving them towards unslableness oreven singularities. Experienced XRD experts are trained to deal with the matter. but industrial or high-throughput research laboratories requirc
Programme