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A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed., RST/Neutron and Positron Methods in Materials

The spin-echo small-angle neutron scattering (SESANS) technique utilises a series of inclined magnetic fields before and after the sample to encode the scattering angle into the polarisation to obtain a much higher resolution than in conventional SANS. The analogous technique (spin echo modulated SANS (SEMSANS)) implements spin manipulations before the sample only to encode the scattering into an intensity modulation. The technique can be combined with SANS to expand the length scale range probed from 1 nm to microns. Using McStas we show that using a series of four magnetic Wollaston prisms in two orthogonal pairs with a 90° rotation can be utilised to create SEMSANS modulations in 2-D. These modulations can also be of different periods in each encoding direction. This method can be applied to anisotropic scattering samples. Also this allows for the simultaneous measurement at two orthogonal independent spin-echo lengths. This technique yields directly information about the structure of oriented structures., RID/TS/Instrumenten groep, ImPhys/Microscopy Instrumentation & Techniques, RST/Neutron and Positron Methods in Materials

A novel spin echo small-angle neutron scattering (SESANS) concept based on a rotationally symmetric magnetic field geometry is introduced. The proposed method is similar to the conventional linear SESANS technique but uses longitudinal precession fields and field gradients in a radial direction, as typically found in neutron spin echo (NSE) spectrometers. Radial SESANS could thus be implemented as an add-on to NSE setups. The neutron trajectory through the instrument is encoded with the help of radial gradients generated by radial shifters, which are coils placed in the beam area similar to Fresnel coils. The present work introduces the setup of the instrument and explores its performance and the relationship between the encoded momentum transfer and the precession angle. The results indicate that radial SESANS is only sensitive to scattering along the radial direction and thus measures the projected correlation function along this direction as a function of the spin echo length, defined similarly to linear SESANS. For an evaluation of the performance of the setup, the case of scattering from solid spheres is considered and the results calculated for the radial and linear SESANS cases are compared. Also discussed is the implementation of the radial magnetic field geometry in spin echo modulated small-angle neutron scattering., RST/Neutron and Positron Methods in Materials

Spin-echo small-angle neutron scattering (SESANS) yields structural information on length scales from 30 nanometres up till 20 micrometres. These length scales match nicely those of colloids, protein networks and fat droplets, which are present in many food materials. This makes SESANS an excellent probe to study food materials. An interesting feature of SESANS is the real space character of the raw data. Several examples of quantitative neutron scattering studies on food materials are shortly reviewed., RST/Neutron and Positron Methods in Materials

For the further development of spin-echo techniques to label elastic scattering it is necessary to perform simulations of the Larmor precession of neutron spins in a magnetic field. The details of some of these techniques as implemented at the reactor in Delft are simulated. First, the workings of the magnetized foil flipper are simulated. A full virtual spin-echo small-angle neutron scattering instrument is built and tested without and with a realistic scattering sample. It is essential for these simulations to have a simulated sample that also describes the transmitted beam of unscattered neutrons, which usually is not implemented for the simulation of conventional small-angle neutron scattering (SANS) instruments. Finally, the workings of a spin-echo modulated small-angle neutron scattering (SEMSANS) instrument are simulated. The simulations are in good agreement with theory and experiments. This setup can be extended to include realistic magnetic field distributions to fully predict the features of future Larmor labelling elastic-scattering instruments. Configurations can now be simulated for more complicated combinations of SANS with SEMSANS., RST/Neutron and Positron Methods in Materials

Small angle scattering is frequently applied to study the anisotropy in complex soft matter systems. One emerging application is to probe the multi-scale structure in food matrices; while few models are available to describe the anisotropic scattering pattern in a quantitative, yet simple manner. For this purpose, anisotropy is introduced to the Guinier–Porod model to study the scattering from non-spherical objects with a preferred orientation. This generalised anisotropic Guinier–Porod model can be adapted to approximate the sector scattering from both cylinders and ellipsoids (both prolate and oblate). In practice, it is applied to describe the anisotropic scattering from fibres in a meat analogue made of calcium caseinate. A good agreement is found between fitted dimensions of the fibres and those observed from the microscopy image. The effect of orientation distribution on the shape and intensity of the scattering pattern is further discussed and three means to obtain the orientation distribution of the symmetry axis are proposed. Given the model is straightforward and the fitting remains phenomenological, it provides a novel approach to extract information from complex food systems., RST/Neutron and Positron Methods in Materials, RST/Fundamental Aspects of Materials and Energy

By introducing hydrophilic polymers into silicone medical devices, highly beneficial biomedical properties can be realized. An established solution to introduce hydrophilic polymers is to form an interpenetrating polymer network (IPN) by performing the hydrogel synthesis in the presence of silicone swollen in supercritical carbon dioxide. The precise distribution of the two polymers is not known, and determining this is the goal of this study. Neutron scattering and microscopy were used to determine the distribution of the hydrophilic guest polymer. Atomic force microscopy revealed that the important length scale on the surface of these materials is 10–100 nm, and spin-echo small-angle neutron scattering (SESANS) on IPNs submerged in D2O revealed structures of the same scale within the interior and enabled quantification of their size. SESANS with hydration by D2O proved to be the only scattering technique that could determine the structure of the bulk of these types of materials, and it should be used as an important tool for characterizing polymer medical devices., RST/Neutron and Positron Methods in Materials, RST/Technici Pool, Technici Pool

Spray-drying is a widely used industrial technique and has shown an immense potential in the fields of nanoscience and technology. This is due to its ability to synthesize microgranules consisting of correlated nanostructures using evaporation induced assembly through bottom-up approach. Although the nature of correlation among the constituent nanoparticles and their size distribution could earlier be obtained by conventional Small-angle Scattering (SAS) technique, a statistically averaged quantitative measure of the shell thickness and hollowness of the formed granules remained a challenge. In this work, we have used Spin-echo Small-angle Neutron Scattering (SESANS) technique to characterize spray-dried nanostructured microgranules having different hollowness. It is shown that this non-destructive technique provided precise quantification of the granular sizes and hollowness by utilizing polarization property of neutrons in real space directly., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

Spin-echo small-angle neutron scattering (SESANS) yields structural information on length scales from 30 nanometres up till 20 micrometres. These length scales match nicely those of colloids, protein networks and fat droplets, which are present in many food materials. This makes SESANS an excellent probe to study food materials. An interesting feature of SESANS is the real space character of the raw data. Several examples of quantitative neutron scattering studies on food materials are shortly reviewed., RST/Neutron and Positron Methods in Materials

Small angle scattering is frequently applied to study the anisotropy in complex soft matter systems. One emerging application is to probe the multi-scale structure in food matrices; while few models are available to describe the anisotropic scattering pattern in a quantitative, yet simple manner. For this purpose, anisotropy is introduced to the Guinier–Porod model to study the scattering from non-spherical objects with a preferred orientation. This generalised anisotropic Guinier–Porod model can be adapted to approximate the sector scattering from both cylinders and ellipsoids (both prolate and oblate). In practice, it is applied to describe the anisotropic scattering from fibres in a meat analogue made of calcium caseinate. A good agreement is found between fitted dimensions of the fibres and those observed from the microscopy image. The effect of orientation distribution on the shape and intensity of the scattering pattern is further discussed and three means to obtain the orientation distribution of the symmetry axis are proposed. Given the model is straightforward and the fitting remains phenomenological, it provides a novel approach to extract information from complex food systems., RST/Neutron and Positron Methods in Materials, RST/Fundamental Aspects of Materials and Energy

For the further development of spin-echo techniques to label elastic scattering it is necessary to perform simulations of the Larmor precession of neutron spins in a magnetic field. The details of some of these techniques as implemented at the reactor in Delft are simulated. First, the workings of the magnetized foil flipper are simulated. A full virtual spin-echo small-angle neutron scattering instrument is built and tested without and with a realistic scattering sample. It is essential for these simulations to have a simulated sample that also describes the transmitted beam of unscattered neutrons, which usually is not implemented for the simulation of conventional small-angle neutron scattering (SANS) instruments. Finally, the workings of a spin-echo modulated small-angle neutron scattering (SEMSANS) instrument are simulated. The simulations are in good agreement with theory and experiments. This setup can be extended to include realistic magnetic field distributions to fully predict the features of future Larmor labelling elastic-scattering instruments. Configurations can now be simulated for more complicated combinations of SANS with SEMSANS., RST/Neutron and Positron Methods in Materials

Spray-drying is a widely used industrial technique and has shown an immense potential in the fields of nanoscience and technology. This is due to its ability to synthesize microgranules consisting of correlated nanostructures using evaporation induced assembly through bottom-up approach. Although the nature of correlation among the constituent nanoparticles and their size distribution could earlier be obtained by conventional Small-angle Scattering (SAS) technique, a statistically averaged quantitative measure of the shell thickness and hollowness of the formed granules remained a challenge. In this work, we have used Spin-echo Small-angle Neutron Scattering (SESANS) technique to characterize spray-dried nanostructured microgranules having different hollowness. It is shown that this non-destructive technique provided precise quantification of the granular sizes and hollowness by utilizing polarization property of neutrons in real space directly., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

By introducing hydrophilic polymers into silicone medical devices, highly beneficial biomedical properties can be realized. An established solution to introduce hydrophilic polymers is to form an interpenetrating polymer network (IPN) by performing the hydrogel synthesis in the presence of silicone swollen in supercritical carbon dioxide. The precise distribution of the two polymers is not known, and determining this is the goal of this study. Neutron scattering and microscopy were used to determine the distribution of the hydrophilic guest polymer. Atomic force microscopy revealed that the important length scale on the surface of these materials is 10–100 nm, and spin-echo small-angle neutron scattering (SESANS) on IPNs submerged in D2O revealed structures of the same scale within the interior and enabled quantification of their size. SESANS with hydration by D2O proved to be the only scattering technique that could determine the structure of the bulk of these types of materials, and it should be used as an important tool for characterizing polymer medical devices., RST/Neutron and Positron Methods in Materials, RST/Technici Pool, RID/TS/Technici Pool

The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., Instrumenten groep, RST/Neutron and Positron Methods in Materials, RST/Technici Pool, Technici Pool

SESANS data analysis has been implemented in the SasView software package, allowing SESANS experiments to be analyzed using a numerical Hankel transformation of isotropic small-angle scattering (SAS) models. The error of the numerical approximation is three orders of magnitude below typical experimental errors. All advanced data fitting features of SasView (multi-model fitting, batch fitting, and simultaneous/constrained fitting) are now also available for SESANS and this is demonstrated by examples of fitting SAS models to SESANS measurements., RST/Radiation, Science and Technology, RST/Neutron and Positron Methods in Materials, Instrumenten groep, Bedrijfsondersteuning

Phospholipid gum mesostructures formed in crude soybean oil after water degumming (WD) and enzymatic degumming (ED) were studied at a range of phospholipid and water concentrations. For ED, phospholipase C (PLC), phospholipase A2 (PLA2) and a mixture of phospholipases Purifine 3G (3G) were used. Both WD and ED resulted in lamellar liquid-crystalline phases, however, of different topology. The dependence of the bilayer spacings (as observed by SANS and SAXS) on the ratio between amount of water and amphiphilic lipids differed for WD and PLA2 ED vs PLC and 3G ED. This difference was also observed for dynamics at molecular scale as observed by time-domain (TD) NMR and attributed to partial incorporation of diglycerides and free fatty acids into gum bilayers after PLC and 3G ED. Feasibility of using TD-NMR relaxometry for quantification of the gum phase and estimation of degumming efficiency was demonstrated., RST/Neutron and Positron Methods in Materials

Pronounced fibres are formed through simple shearing of a dense calcium caseinate dispersion. Both mechanical tests and scanning electron microscopy images demonstrate that the material is anisotropic. It is hypothesised that calcium caseinate aggregates, under shear, align into micro-fibres and bundle further into a hierarchical structure. Yet no direct evidence at the sub-micron length scale can support the assumption. Small angle neutron scattering (SANS) experiments were conducted on calcium caseinate samples prepared at different conditions. Analysis of the SANS data revealed that the micro-fibres have a diameter of ∼100nm and a length of ∼300nm. The addition of enzyme and air contributed to longer and thinner micro-fibres. Furthermore, the extent of fibre alignment at the micro-scale and the macroscopic anisotropy index followed the same trends with varying processing conditions. It is concluded that the material does indeed possess a hierarchical structure and the micro-fibres are responsible for the anisotropy on the macro-scale., RST/Neutron and Positron Methods in Materials

The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RID/TS/Instrumenten groep, RST/Neutron and Positron Methods in Materials, RST/Technici Pool, RID/TS/Technici Pool

Phospholipid gum mesostructures formed in crude soybean oil after water degumming (WD) and enzymatic degumming (ED) were studied at a range of phospholipid and water concentrations. For ED, phospholipase C (PLC), phospholipase A2 (PLA2) and a mixture of phospholipases Purifine 3G (3G) were used. Both WD and ED resulted in lamellar liquid-crystalline phases, however, of different topology. The dependence of the bilayer spacings (as observed by SANS and SAXS) on the ratio between amount of water and amphiphilic lipids differed for WD and PLA2 ED vs PLC and 3G ED. This difference was also observed for dynamics at molecular scale as observed by time-domain (TD) NMR and attributed to partial incorporation of diglycerides and free fatty acids into gum bilayers after PLC and 3G ED. Feasibility of using TD-NMR relaxometry for quantification of the gum phase and estimation of degumming efficiency was demonstrated., RST/Neutron and Positron Methods in Materials

SESANS data analysis has been implemented in the SasView software package, allowing SESANS experiments to be analyzed using a numerical Hankel transformation of isotropic small-angle scattering (SAS) models. The error of the numerical approximation is three orders of magnitude below typical experimental errors. All advanced data fitting features of SasView (multi-model fitting, batch fitting, and simultaneous/constrained fitting) are now also available for SESANS and this is demonstrated by examples of fitting SAS models to SESANS measurements., RST/Radiation, Science and Technology, RST/Neutron and Positron Methods in Materials, RID/TS/Instrumenten groep, RID/Algemeen/Bedrijfsondersteuning

Pronounced fibres are formed through simple shearing of a dense calcium caseinate dispersion. Both mechanical tests and scanning electron microscopy images demonstrate that the material is anisotropic. It is hypothesised that calcium caseinate aggregates, under shear, align into micro-fibres and bundle further into a hierarchical structure. Yet no direct evidence at the sub-micron length scale can support the assumption. Small angle neutron scattering (SANS) experiments were conducted on calcium caseinate samples prepared at different conditions. Analysis of the SANS data revealed that the micro-fibres have a diameter of ∼100nm and a length of ∼300nm. The addition of enzyme and air contributed to longer and thinner micro-fibres. Furthermore, the extent of fibre alignment at the micro-scale and the macroscopic anisotropy index followed the same trends with varying processing conditions. It is concluded that the material does indeed possess a hierarchical structure and the micro-fibres are responsible for the anisotropy on the macro-scale., RST/Neutron and Positron Methods in Materials

We investigate the morphological development of polystyrene (PS)-C 60 nanocomposites along the length of a prototype co-rotating twin-screw extruder with sampling capabilities. The effects of C 60 concentration and output on the morphological evolution along the extruder are studied employing a suite of characterization techniques covering a wide range of length-scales, thereby shedding new light on the dispersion mechanism in this model system. We show that the relatively new spin-echo small-angle neutron scattering (SESANS) technique is well suited to probe both the distribution and the dispersion of C 60 . SESANS complements optical microscopy (OM) data as it covers sampling areas several orders of magnitude larger than OM. The multi-scale morphological information conveyed by OM, SESANS, SANS and rheological data shows that for larger outputs, C 60 agglomerates are eroded as they travel along the extruder, resulting in C 60 dispersion and distribution at both molecular and micrometric levels. The picture is more complex when smaller feed rates are used, as the evolution of C 60 dispersion depends on the C 60 loading. For larger C 60 contents, agglomeration develops along the extruder, whereas dispersion is improved for smaller C 60 contents. Overall, it is concluded that an over-high feed rate in extrusion does not necessarily result in a bigger size of the nanoparticle agglomerates because of the complex interplay between stresses and residence time., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Technici Pool, Technici Pool, RST/Neutron and Positron Methods in Materials, RST/Fundamental Aspects of Materials and Energy

A time of flight MIEZE spectrometerstudyis presented. The instrumentuses solenoid radio frequency(RF)spin flipperswithsquare pole shoes and a magnetic yoke. These flippers can achieve higherstaticfields than conventional resonant RF spin flippers, which employ an air core.High fields are crucial for the construction of a high resolution and compact MIEZE spectrometer.Using both types of flipperstwo MIEZE spectrometer configurationsare constructed and comparedon the same beam line. It was demonstratedthat the pole shoe/solenoid coil RF flipperscan achieve a MIEZE signal, which is similarin quality to theconventionalreferencesetup.The highest obtained modulation frequency was 100kHz., Instrumenten groep, RST/Neutron and Positron Methods in Materials, Technici Pool

This paper reports on the two-scale fractal structure of chromatin organization in the nucleus of the HeLa cell. Two neutron scattering methods, small-angle neutron scattering (SANS) and spin-echo SANS, are used to unambiguously identify the large-scale structure as being a logarithmic fractal with the correlation function (r) - ln(r/E). The smaller-scale structural level is shown to be a volume fractal with dimension DF = 2.41. By definition, the volume fractal is self-similar at different scales, while the logarithmic fractal is hierarchically changed upon scaling. As a result, the logarithmic fractal is more compact than the volume fractal but still has a rather high surface area, which provides accessibility at all length scales. Apparently such bi-fractal chromatin organization is the result of an evolutionary process of optimizing the compactness and accessibility of gene packing. As they are in a water solution, the HeLa nuclei tend to agglomerate over time. The large-scale logarithmic fractal structure of chromatin provides the HeLa nucleus with the possibility of penetrating deeply into the adjacent nucleus during the agglomeration process. The interpenetration phenomenon of the HeLa nuclei shows that the chromatin-free space of one nucleus is not negligible but is as large as the volume occupied by chromatin itself. It is speculated that it is the logarithmic fractal architecture of chromatin that provides a comfortable compartment for this most important function of the cell., RST/Neutron and Positron Methods in Materials, RST/Technici Pool, Technici Pool

We present an investigation of the dynamics of calcium caseinate as a function of hydration, solvent isotope (H2O and D2O) and drying methods (roller drying and spray drying), using quasi-elastic neutron scattering (QENS). These factors are key to the formation of fibres in this material which makes it a potential candidate as a next-generation meat analogue. Using a phenomenological model, we find that the relaxation times of the dry spray dried powder decrease with increasing temperatures, while they do not change for the roller dried powder. The spectra of the hydrated samples reveal two independent picosecond processes, both reflecting localized re-orientational motions. We hypothesize that the faster motion is due to the external protein groups that are hydrophilic and the slower motion is due to the internal groups that are hydrophobic. The solvent effect of D2O is not limited to the external groups but prevails to the internal groups where less protons are mobile compared to the H2O hydrated samples. Higher temperatures narrow the number difference in mobile protons, possibly by altering the weak interactions inside the protein aggregates. These findings suggest that a harsh and longer drying process contributes to less active protein side-groups and highlight the hydrophobic effect of D2O on the fibre formation in calcium caseinate., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

Microemulsion systems consisting of D2O, an alkane, an anionic internal olefin sulfonate surfactant, salt and secondary butyl alcohol (SBA) as co-solvent are studied in a systematic way. In four different sample sets, either the salt content, SBA content or alkane carbon number was varied in order to study the effects of the individual compounds on the structure sizes making up the microemulsion. Using complementary small-angle neutron scattering techniques SANS and Spin-Echo SANS, it was found that the microemulsion systems exhibit the largest structures in the optimum state (domain size of d/2 =144 nm in the model by Teubner and Strey), where the structure is considered bicontinuous. In comparison, at under- and over-optimum states where the structures consist of emulsified spherical droplets, the smallest measured diameter was 2R = 44 nm. Furthermore, the structure sizes in bicontinuous microemulsions decrease exponentially (down to d/2 =15 nm for pentadecane and 5 wt% SBA) as function of both SBA content and alkane carbon number. The observed trends in structure sizes combined with the trends observed in the area per surfactant molecule, are qualitatively explained with the extended Winsor R-ratio, the HLD-NAC model and surfactant film flexibility arguments., ImPhys/OpleidingTechnische Natuurkunde, RST/Neutron and Positron Methods in Materials

A versatile cell for X-ray and neutron scattering experiments on samples under shear has been designed. To our knowledge, it is the first shear cell which can be used for both SAXS and SANS in respectively synchrotron or reactor beamlines. The cell is mainly intended for scattering experiments in so-called “1–2 plane geometry” but can also be modified into cone–plate and plate–plate rheological geometries, giving access to the 1–3 scattering plane. The latter two geometries, however, can only be used with neutron scattering. The final cell design is compact, which allows it to be used even with lab-based X-ray sources. A special thermostatic shell allows for the temperature control of the samples under investigation in the range from 5 up to 100 °C. Several X-ray and neutron scattering experiments performed with the cell have helped in better understanding of the structuring under shear of food materials, such as: cellulose suspensions, fat crystal networks and milk proteins., RST/Neutron and Positron Methods in Materials, Electronic and Mechanical Support Division, EMSD EEMCS Project engineers1

We investigate the morphological development of polystyrene (PS)-C 60 nanocomposites along the length of a prototype co-rotating twin-screw extruder with sampling capabilities. The effects of C 60 concentration and output on the morphological evolution along the extruder are studied employing a suite of characterization techniques covering a wide range of length-scales, thereby shedding new light on the dispersion mechanism in this model system. We show that the relatively new spin-echo small-angle neutron scattering (SESANS) technique is well suited to probe both the distribution and the dispersion of C 60 . SESANS complements optical microscopy (OM) data as it covers sampling areas several orders of magnitude larger than OM. The multi-scale morphological information conveyed by OM, SESANS, SANS and rheological data shows that for larger outputs, C 60 agglomerates are eroded as they travel along the extruder, resulting in C 60 dispersion and distribution at both molecular and micrometric levels. The picture is more complex when smaller feed rates are used, as the evolution of C 60 dispersion depends on the C 60 loading. For larger C 60 contents, agglomeration develops along the extruder, whereas dispersion is improved for smaller C 60 contents. Overall, it is concluded that an over-high feed rate in extrusion does not necessarily result in a bigger size of the nanoparticle agglomerates because of the complex interplay between stresses and residence time., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Technici Pool, RID/TS/Technici Pool, RST/Neutron and Positron Methods in Materials, RST/Fundamental Aspects of Materials and Energy

A time of flight MIEZE spectrometerstudyis presented. The instrumentuses solenoid radio frequency(RF)spin flipperswithsquare pole shoes and a magnetic yoke. These flippers can achieve higherstaticfields than conventional resonant RF spin flippers, which employ an air core.High fields are crucial for the construction of a high resolution and compact MIEZE spectrometer.Using both types of flipperstwo MIEZE spectrometer configurationsare constructed and comparedon the same beam line. It was demonstratedthat the pole shoe/solenoid coil RF flipperscan achieve a MIEZE signal, which is similarin quality to theconventionalreferencesetup.The highest obtained modulation frequency was 100kHz., RID/TS/Instrumenten groep, RST/Neutron and Positron Methods in Materials, RID/TS/Technici Pool

We present an investigation of the dynamics of calcium caseinate as a function of hydration, solvent isotope (H2O and D2O) and drying methods (roller drying and spray drying), using quasi-elastic neutron scattering (QENS). These factors are key to the formation of fibres in this material which makes it a potential candidate as a next-generation meat analogue. Using a phenomenological model, we find that the relaxation times of the dry spray dried powder decrease with increasing temperatures, while they do not change for the roller dried powder. The spectra of the hydrated samples reveal two independent picosecond processes, both reflecting localized re-orientational motions. We hypothesize that the faster motion is due to the external protein groups that are hydrophilic and the slower motion is due to the internal groups that are hydrophobic. The solvent effect of D2O is not limited to the external groups but prevails to the internal groups where less protons are mobile compared to the H2O hydrated samples. Higher temperatures narrow the number difference in mobile protons, possibly by altering the weak interactions inside the protein aggregates. These findings suggest that a harsh and longer drying process contributes to less active protein side-groups and highlight the hydrophobic effect of D2O on the fibre formation in calcium caseinate., Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

This paper reports on the two-scale fractal structure of chromatin organization in the nucleus of the HeLa cell. Two neutron scattering methods, small-angle neutron scattering (SANS) and spin-echo SANS, are used to unambiguously identify the large-scale structure as being a logarithmic fractal with the correlation function (r) - ln(r/E). The smaller-scale structural level is shown to be a volume fractal with dimension DF = 2.41. By definition, the volume fractal is self-similar at different scales, while the logarithmic fractal is hierarchically changed upon scaling. As a result, the logarithmic fractal is more compact than the volume fractal but still has a rather high surface area, which provides accessibility at all length scales. Apparently such bi-fractal chromatin organization is the result of an evolutionary process of optimizing the compactness and accessibility of gene packing. As they are in a water solution, the HeLa nuclei tend to agglomerate over time. The large-scale logarithmic fractal structure of chromatin provides the HeLa nucleus with the possibility of penetrating deeply into the adjacent nucleus during the agglomeration process. The interpenetration phenomenon of the HeLa nuclei shows that the chromatin-free space of one nucleus is not negligible but is as large as the volume occupied by chromatin itself. It is speculated that it is the logarithmic fractal architecture of chromatin that provides a comfortable compartment for this most important function of the cell., RST/Neutron and Positron Methods in Materials, RST/Technici Pool, RID/TS/Technici Pool

Microemulsion systems consisting of D2O, an alkane, an anionic internal olefin sulfonate surfactant, salt and secondary butyl alcohol (SBA) as co-solvent are studied in a systematic way. In four different sample sets, either the salt content, SBA content or alkane carbon number was varied in order to study the effects of the individual compounds on the structure sizes making up the microemulsion. Using complementary small-angle neutron scattering techniques SANS and Spin-Echo SANS, it was found that the microemulsion systems exhibit the largest structures in the optimum state (domain size of d/2 =144 nm in the model by Teubner and Strey), where the structure is considered bicontinuous. In comparison, at under- and over-optimum states where the structures consist of emulsified spherical droplets, the smallest measured diameter was 2R = 44 nm. Furthermore, the structure sizes in bicontinuous microemulsions decrease exponentially (down to d/2 =15 nm for pentadecane and 5 wt% SBA) as function of both SBA content and alkane carbon number. The observed trends in structure sizes combined with the trends observed in the area per surfactant molecule, are qualitatively explained with the extended Winsor R-ratio, the HLD-NAC model and surfactant film flexibility arguments., ImPhys/Practicum support, RST/Neutron and Positron Methods in Materials

A versatile cell for X-ray and neutron scattering experiments on samples under shear has been designed. To our knowledge, it is the first shear cell which can be used for both SAXS and SANS in respectively synchrotron or reactor beamlines. The cell is mainly intended for scattering experiments in so-called “1–2 plane geometry” but can also be modified into cone–plate and plate–plate rheological geometries, giving access to the 1–3 scattering plane. The latter two geometries, however, can only be used with neutron scattering. The final cell design is compact, which allows it to be used even with lab-based X-ray sources. A special thermostatic shell allows for the temperature control of the samples under investigation in the range from 5 up to 100 °C. Several X-ray and neutron scattering experiments performed with the cell have helped in better understanding of the structuring under shear of food materials, such as: cellulose suspensions, fat crystal networks and milk proteins., RST/Neutron and Positron Methods in Materials, Electronic and Mechanical Support Division, EMSD EEMCS Project engineers1

Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

RST/Neutron and Positron Methods in Materials

Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

Green Open Access added to TU Delft Institutional Repository ‘You share, we take care!’ – Taverne project https://www.openaccess.nl/en/you-share-we-take-care Otherwise as indicated in the copyright section: the publisher is the copyright holder of this work and the author uses the Dutch legislation to make this work public., RST/Neutron and Positron Methods in Materials

RST/Neutron and Positron Methods in Materials

Submicron- and micron-scale structures of composite hydrogels based on bacterial cellulose (BC) and polyacrylamide (PAAm) were studied by spin-echo small-angle neutron scattering (SESANS) and cryo-scanning electron microscopy (cryo-SEM). These hydrogels possessing the structure of interpenetrating polymer network were synthesized via free-radical polymerization of acrylamide carried out in the pellicle of BC swollen in the reaction solution. No neutron scattering was observed for the samples swollen in heavy water to the equilibrium state, but the SESANS signal appeared when TbCl3 salt was added to the solvent. It is the unusual effect, which may be very helpful for SESANS studying of other hydrogel systems. The SESANS dependences obtained for these samples revealed the anisotropy of mesostructure for the hydrogels under investigation. Density inhomogeneities on the characteristic scale of 11.5 ± 0.5 μm were detected in one fixed orientation of the sample, i.e., with the growth plane of BC parallel to the plane formed by the neutron beam and the spin-echo length. The uniaxial anisotropy revealed agrees with a recently proposed model, which attributes this behavior to the existence of tunnel-like oriented structures inside BC. The evidence of such type of mesostructure anisotropy of BC and BC-PAAm hydrogels was obtained by using the cryo-SEM method., Accepted Author Manuscript, RST/Neutron and Positron Methods in Materials, Technici Pool

Small-angle neutron scattering (SANS) on nuclei of chicken erythrocytes demonstrates the cubic dependence of the scattering intensity Q−3 in the range of momentum transfer Q∈10−3–10−2nm−1. Independent spin-echo SANS measurements give the spin-echo function, which is well described by the exponential law in a range of sizes (3×102)–(3×104) nm. Both experimental dependences reflect the nature of the structural organization of chromatin in the nucleus of a living cell, which corresponds to the correlation function γ(r)=ln(ξ/r) for r<ξ, where ξ=(3.69±0.07)×103 nm, the size of the nucleus. It has the specific scaling property of the logarithmic fractal γ(r/a)=γ(r)+ln(a), i.e., the scaling down by a gives an additive constant to the correlation function, which distinguishes it from the mass fractal, which is characterized by multiplicative constant., RST/Neutron and Positron Methods in Materials

Spin-echo small-angle scattering (SESANS) technique is a method to measure the structure of materials from nano- to micrmeter length scales. This method could be important for studying the packaging of DNA in the eukaryotic cell. We measured the SESANS function from chicken erythrocyte nuclei which is well fitted by the exponential function G(z) = exp(-z/ξ), where ξ is the correlation length of a nucleus (in experimental data ξ = 3, 3 μm). The exponential decay of G(z) corresponds to the logarithmic pair correlation function γ(r) = ln(ξ/r). As the sensitivity of the SESANS signal depends on the neutron wavelength, we propose the SESANS setup with the changeable wavelength in the range from 2 to 12 Å. Such option allows one to study in great detail the internal structure of the biological cell in the length scale from 10-2 μm to 10 μm., RST/Neutron and Positron Methods in Materials

Spin-Echo Modulated Small Angle Neutron Scattering with spatial resolution, i.e. quantitative Spin-Echo Dark Field Imaging, is an emerging technique coupling neutron imaging with spatially resolved quantitative small angle scattering information. However, the currently achieved relatively large modulation periods of the order of millimeters are superimposed to the images of the samples. So far this required an independent reduction and analyses of the image and scattering information encoded in the measured data and is involving extensive curve fitting routines. Apart from requiring a priori decisions potentially limiting the information content that is extractable also a straightforward judgment of the data quality and information content is hindered. In contrast we propose a significantly simplified routine directly applied to the measured data, which does not only allow an immediate first assessment of data quality and delaying decisions on potentially information content limiting further reduction steps to a later and better informed state, but also, as results suggest, generally better analyses. In addition the method enables to drop the spatial resolution detector requirement for non-spatially resolved Spin-Echo Modulated Small Angle Neutron Scattering, Technici Pool, RST/Neutron and Positron Methods in Materials

Spin-Echo Modulated Small Angle Neutron Scattering with spatial resolution, i.e. quantitative Spin-Echo Dark Field Imaging, is an emerging technique coupling neutron imaging with spatially resolved quantitative small angle scattering information. However, the currently achieved relatively large modulation periods of the order of millimeters are superimposed to the images of the samples. So far this required an independent reduction and analyses of the image and scattering information encoded in the measured data and is involving extensive curve fitting routines. Apart from requiring a priori decisions potentially limiting the information content that is extractable also a straightforward judgment of the data quality and information content is hindered. In contrast we propose a significantly simplified routine directly applied to the measured data, which does not only allow an immediate first assessment of data quality and delaying decisions on potentially information content limiting further reduction steps to a later and better informed state, but also, as results suggest, generally better analyses. In addition the method enables to drop the spatial resolution detector requirement for non-spatially resolved Spin-Echo Modulated Small Angle Neutron Scattering, RID/TS/Technici Pool, RST/Neutron and Positron Methods in Materials

We investigated the effect of the feeding formulation (premixed powders of pure components versus solvent-blended mixture) of polystyrene–C60 composites on the dispersion and reagglomeration phenomena developing along the barrel of a twin-screw extruder. The dispersion of C60 in the PS matrix is studied over different length scales using a combination of optical microscopy, spin-echo small-angle neutron scattering (SESANS), small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS). When a solvent-blended mixture is used as the feeding formulation, the inlet material contains essentially molecularly dispersed C60 as revealed by the nanodomains with very small phase contrast. However, C60 reagglomeration occurs along the extruder, creating a morphology still containing only nanodomains but with much higher phase contrast. In the case of mixed powders, the material evolves from the initial macroscopic mixture of pure polystyrene and C60 into a composite simultaneously containing micro- and nanoaggregates of C60 as well as C60 molecularly dispersed in the matrix. Our results show that the two different initial feeding formulations with widely different initial morphologies converge along the extruder, through opposite morphological pathways, into a similar final nanomorphology which is dictated by the interplay between the thermodynamics of the system and the flow. Correlations between the morphological evolution along the extruder and the thermorheological properties of the composites are identified., RST/Neutron and Positron Methods in Materials, RST/Fundamental Aspects of Materials and Energy

Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved by ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI., Technici Pool, RST/Neutron and Positron Methods in Materials

Spin-Echo Modulated Small Angle Neutron Scattering (SEMSANS) in Time-of-Flight (ToF) mode has been shown to be a promising technique for measuring (very) small angle neutron scattering (SANS) signals and performing quantitative Dark-Field Imaging (DFI), i.e., SANS with 2D spatial resolution. However, the wavelength dependence of the modulation period in the ToF spin-echo mode has so far limited the useful modulation periods to those resolvable with the limited spatial resolution of the detectors available. Here we present our results of an approach to keep the period of the induced modulation constant for the wavelengths utilised in ToF. This is achieved by ramping the magnetic fields in the coils responsible for creating the spatially modulated beam in synchronisation with the neutron pulse, thus keeping the modulation period constant for all wavelengths. Such a setup enables the decoupling of the spatial detector resolution from the resolution of the modulation period by the use of slits or gratings in analogy to the approach in grating-based neutron DFI., RID/TS/Technici Pool, RST/Neutron and Positron Methods in Materials

recent years, the interest in fluidization as a mean to process nanoparticles is strongly increasing. Due to the small size of the nanoparticles, which makes van der Waals forces predominate, they do not fluidize as single particles but as agglomerates. Various researchers using settling experiments and bed expansion measurements conclude that fluidized agglomerates are fractal structures with a single fractal dimension of 2.5. Based on microscopy results, Wang et al. “Powder Technology 124, 152–C159 (2002)” propose a hierarchical structure, which seems in contradiction with the use of only one fractal dimension as a descriptor of the whole structure. Moreover, it is not clear whether the structure presented by the agglomerates ex-situ is the same during fluidization. Hence, in this work we have characterized in-situ the internal structure of fluidized agglomerates by means of spin-echo small-angle neutron scattering (SESANS). We show that the structure of the agglomerates present at least two fractal dimensions. One of them is ? 2.1 and characterizes the primary strong agglomerates. The second one is ? 2.8 and characterizes the larger agglomerates formed by the primary agglomerates., ChemE/Chemical Engineering, Applied Sciences

recent years, the interest in fluidization as a mean to process nanoparticles is strongly increasing. Due to the small size of the nanoparticles, which makes van der Waals forces predominate, they do not fluidize as single particles but as agglomerates. Various researchers using settling experiments and bed expansion measurements conclude that fluidized agglomerates are fractal structures with a single fractal dimension of 2.5. Based on microscopy results, Wang et al. “Powder Technology 124, 152–C159 (2002)” propose a hierarchical structure, which seems in contradiction with the use of only one fractal dimension as a descriptor of the whole structure. Moreover, it is not clear whether the structure presented by the agglomerates ex-situ is the same during fluidization. Hence, in this work we have characterized in-situ the internal structure of fluidized agglomerates by means of spin-echo small-angle neutron scattering (SESANS). We show that the structure of the agglomerates present at least two fractal dimensions. One of them is ? 2.1 and characterizes the primary strong agglomerates. The second one is ? 2.8 and characterizes the larger agglomerates formed by the primary agglomerates., ChemE/Chemical Engineering, Applied Sciences

We report on measurements of spatial beam modulation of a polarized neutron beam induced by triangular precession regions in time-of-flight mode and the application of this novel technique spin-echo modulated small-angle neutron scattering (SEMSANS) to small-angle neutron scattering in the very small angle range. It is shown that this method can be implemented straight-forwardly in order to extend the accessible size range of structures to be investigated by SANS towards a microscopic scale by applying a divergent beam and measuring the real space correlation function. The novel approach of SEMSANS enables the application of sophisticated sample environment and measurements of magnetic samples (in contrast to the analogue method SESANS)., Reactor Instituut Delft, Applied Sciences