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Polypropylene/polyhedral oligomeric silsesquioxane nanocomposites – study of free volumes, crystallinity degree and mass flow rate

Niemczyk A., Dziubek K., Czaja K., Szatanik R., Szołyga M., Dutkiewicz M., Marciniec B.

Polimery

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2016

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T. 61, nr 9

610--615

EN

Polypropylene/polyhedral oligomeric silsesquioxane (PP/POSS) nanocomposites were prepared by the melt blending method. Positron Annihilation Lifetime Spectroscopy (PALS) was used to study the effects of the structure and of the amount of POSS on the free volumes in PP. The PALS parameters: o-Ps lifetime and its intensity, were compared to the crystallinity degree and to the mass flow rate (MFR) of nanocomposites. The presence of POSS nanofillers affected the PP microstructure and the size and number of free volumes in the polymer. The crystallinity degree was decreased and the intensity of o-Ps component was increased by increasing POSS contents. The MFR values increased for nanocomposites, thus POSS nanoparticles can act as plasticizers and generate more free volumes in PP.

PL

Nanokompozyty polipropylen/poliedryczne oligomeryczne silseskwioksany (PP/POSS) przygotowano metodą mieszania w stanie stopionym polimeru. Wpływ struktury oraz ilości zastosowanych nanonapełniaczy POSS na objętości swobodne w polipropylenie określono z zastosowaniem spektroskopii czasów życia pozytonów (PALS). Ustalono zależności pomiędzy parametrami PALS: czasem życia o-Ps (τ3) inatężeniem (I3) składowej o-Ps oraz wartościami stopnia krystaliczności (Xc) i masowego wskaźnika szybkości płynięcia (MFR) badanych materiałów. Obecność nanonapełniaczy POSS wpłynęła na liczbę i rozmiary objętości swobodnych w polimerze, co spowodowało zmianę mikrostruktury osnowy polipropylenowej. Wraz ze zwiększaniem zawartości napełniaczy POSS zmniejszał się stopień krystaliczności kompozytów, zwiększało natężenie składowej o-Ps, adodatkowo wzrastała wartość MFR – nanocząstki POSS pełniły w układzie rolę plastyfikatorów.

2

Principles of positron porosimetry

Zaleski R.

Nukleonika

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2015

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Vol. 60, No. 4, part 1

795--800

EN

The paper deals with positron porosimetry (PP), which is based on positron annihilation lifetime spectroscopy (PALS). The numerical analysis of positron lifetime spectra for PP is more demanding than in most of other applications of PALS. The resulting intensity distributions of ortho-positronium (o-Ps) lifetimes are interpreted in terms of the extended Tao-Eldrup (ETE) model, which provides the dependence between the o-Ps lifetime and pore size. Additionally, the relation between the intensity of an o-Ps component and the pore volume allows obtaining pore size distribution (PSD). The value of the empirical parameter Δ, which is dependent on material, can be estimated from the temperature dependence of an o-Ps lifetime. The most unique feature of PP among other techniques that allow determination of PSDs is its ability to perform measurements in almost any conditions. This makes this method suitable for various in situ studies. In this review article, both the capabilities and the limitations of PP are discussed. The methods to overcome some of the limitations are presented.

3

PALS investigations of matrix Vycor glass doped with molecules of luminescent dye and silver nanoparticles. Discrepancies from the ETE model

Gorgol M., Jasińska B., Reisfeld R.

Nukleonika

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2015

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Vol. 60, No. 4, part 1

717--720

EN

A thermal stability of three materials: undoped reference Vycor glass, glass filled with ROT-305 red dye, and silver nanoparticles was investigated by positron annihilation lifetime spectroscopy (PALS) in a broad temperature range (from 93 to 473 K). The attempt of pore size calculations from the ortho-positronium lifetime data was performed using the extended Tao-Eldrup (ETE) model. Below room temperature, a significant decrease in lifetime values of the longest-lived component was found for all the samples. This effect could not be explained by thermal shrinkage of the material and is probably caused by interaction of -Ps with a Vycor glass matrix. The greatest discrepancy from the ETE model predictions was observed for the reference glass. Doping the base material with dye molecules and silver nanoparticles resulted in similar small decrease in this discrepancy. After reheating the samples to the room temperature, the PALS components returned to the initial values. In the temperature range of 293–473 K, quite good agreement between PALS results and the ETE model predictions was observed for the reference glass and the glass incorporated with dye molecules. The observed small discrepancy in this range could possibly be partly explained by thermal expansion of the material. For the glass doped with silver nanoparticles, a significant change in PALS parameters was observed in the temperature range from 403 to 473 K.

4

Porosity structure in photon active glasses

Jasińska B., Śniegocka M., Reisfeld R., Zigansky E.

Nukleonika

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2013

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Vol. 58, No. 1

241-244

EN

Two kinds of photon active glasses were investigated using positron annihilation lifetime spectroscopy (PALS). Both kinds of glasses were prepared using a sol-gel technique, doped by complex of ruthenium tris bipyridyl chloride. Glasses differed from the initial matrix: the first one was prepared using silicon oxide while the second one - zircon oxide. The ortho-positronium (o-Ps) lifetime and intensities were determined from lifetime spectra. Different porosity structure concluded from PALS measurements was found in both cases. In the silica based glasses small free volumes (angstrom size) and pores (from 1 to 10 nm) existed in the material. On the contrary, in zirconia based glasses small intermolecular voids were produced in the structure only, independently of the way of material preparation.

5

Photoluminescence and positron annihilation lifetime studies on pellets of ZnO nanocrystals

Karbowski A., Fedus K., Patyk J., Bujak Ł., Służewski K., Karwasz G.

Nukleonika

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2013

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Vol. 58, No. 1

189-194

EN

We explore the interrelationships between the X-ray diffraction patterns, the photoluminescence spectra and the positron lifetimes obtained from circular pellets composed of commercial ZnO nanoparticles. The experimental results are studied as a function of thermal treatment at different temperatures. X-ray diffractograms reveal the temperature- independent wurtzite phase structure of nanocrystals and show huge enlargement of ZnO grains after annealing at temperatures higher than 700 centigrade. Photoluminescence measurements exhibit two emission bands : a near band edge emission in UV (small tilde 378 nm) and a defect-related broad visible peak with a maximum in the green region ( small tilde 502 nm). The significant enhancement of the green emission at the expense of UV luminescence is observed after sample sintering at 800 and 1000 centigrade. The positron annihilation lifetime spectroscopy (PALS) is applied in order to study the thermally induced evolution of defects. The lifetime components show a step-like dependence on the thermal treatment, but do not follow exactly the variation in crystallographic phases and only vaguely follow differences in photoluminescence. The positron data indicate therefore some additional structural and/or defect changes. The possible origin of green luminescence from ZnO pellets is discussed.

6

PALS investigation of resorcinol under high pressure

Tydda M., Jasińska B., Pieniążek A.

Nukleonika

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2013

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Vol. 58, No. 1

195-198

EN

Two kinds of measurements were conducted with resorcinol at high pressure : the first one with the use of a mechanical press and the second one with the use of a gaseous compressor. In the second case, due to some gas penetrating the material structure, the lifetime spectra obtained were difficult to analyze. The free volumes in resorcinol were influenced both by high pressure and the gas coming into the crystallographic structure.

7

Ortho-positronium migration in mesopores of MCM-41, MSF and SBA-3

Zaleski R., Błażewicz A., Kierys A.

Nukleonika

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2013

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Vol. 58, No. 1

235-240

EN

Three materials: MCM-41, MSF and SBA-3 with a very similar pore diameter but different lengths of cylindrical pores were investigated using the nitrogen sorption method and positron annihilation lifetime spectroscopy. The size of primary pores and interparticle spaces obtained by both methods is similar. However, volume ratios between the discussed kinds of pores found by the above-mentioned methods differ significantly. Such discrepancy is the result of both ortho-positronium migration and the inaccessibility of the pores for nitrogen. Comparing the results of nitrogen sorption and positron annihilation lifetime spectroscopy allows us to estimate that connectivity between the primary pores and the interparticle spaces is the highest in MCM-41 and lowest in SBA-3.