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Sökning: LAR1:miun > Lunds universitet

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1.
  • Albani, Giorgia, et al. (författare)
  • Evolution in boron-based GEM detectors for diffraction measurements : From planar to 3D converters
  • 2016
  • Ingår i: Measurement science and technology. - : IOP Publishing. - 0957-0233 .- 1361-6501. ; 27:11
  • Tidskriftsartikel (refereegranskat)abstract
    • The so-called '3He-crisis' has motivated the neutron detector community to undertake an intense R&D programme in order to develop technologies alternative to standard 3He tubes and suitable for neutron detection systems in future spallation sources such as the European spallation source (ESS). Boron-based GEM (gas electron multiplier) detectors are a promising '3He-free' technology for thermal neutron detection in neutron scattering experiments. In this paper the evolution of boron-based GEM detectors from planar to 3D converters with an application in diffraction measurements is presented. The use of 3D converters coupled with GEMs allows for an optimization of the detector performances. Three different detectors were used for diffraction measurements on the INES instrument at the ISIS spallation source. The performances of the GEM-detectors are compared with those of conventional 3He tubes installed on the INES instrument. The conceptual detector with the 3D converter used in this paper reached a count rate per unit area of about 25% relative to the currently installed 3He tube. Its timing resolution is similar and the signal-to-background ratio (S/B) is 2 times lower.
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2.
  • Alves, Luis, et al. (författare)
  • Dissolution state of cellulose in aqueous systems. 1. Alkaline solvents
  • 2016
  • Ingår i: Cellulose. - : Springer Science and Business Media LLC. - 0969-0239 .- 1572-882X. ; 23:1, s. 247-258
  • Tidskriftsartikel (refereegranskat)abstract
    • The understanding of the state of dissolution of cellulose in a certain solvent is a critical step forward in the development of new efficient solvent systems for cellulose. Nevertheless, obtaining such information is not trivial. Recently, polarization transfer solid-state NMR (PTssNMR) was shown to be a very promising technique regarding an efficient and robust characterization of the solution state of cellulose. In the present study, combining PTssNMR, microscopic techniques and X-ray diffraction, a set of alkaline aqueous systems are investigated. The addition of specific additives, such as urea or thiourea, to aqueous NaOH based systems as well as the use of an amphiphilic organic cation, is found to have pronounced effects on the dissolution efficiency of cellulose. Additionally, the characteristics of the regenerated material are strongly dependent on the dissolution system; typically less crystalline materials, presenting smoother morphologies, are obtained when amphiphilic solvents or additives are used.
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3.
  • Alves, Luis, et al. (författare)
  • Dissolution state of cellulose in aqueous systems. 2. Acidic solvents
  • 2016
  • Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 151, s. 707-715
  • Tidskriftsartikel (refereegranskat)abstract
    • Cellulose is insoluble in water but can be dissolved in strong acidic or alkaline conditions. How well dissolved cellulose is in solution and how it organizes are key questions often neglected in literature. The typical low pH required for dissolving cellulose in acidic solvents limits the use of typical characterization techniques. In this respect, Polarization Transfer Solid State NMR (PT ssNMR) emerges as a reliable alternative. In this work, combining PT ssNMR, microscopic techniques and X-ray diffraction, a set of different acidic systems (phosphoric acid/water, sulfuric acid/glycerol and zinc chloride/water) is investigated. The studied solvent systems are capable to efficiently dissolve cellulose, although degradation occurs to some extent. PT ssNMR is capable to identify the liquid and solid fractions of cellulose, the degradation products and it is also sensitive to gelation. The materials regenerated from the acidic dopes were found to be highly sensitive to the solvent system and to the presence of amphiphilic additives in solution.
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4.
  • Alves, Luis, et al. (författare)
  • New Insights on the Role of Urea on the Dissolution and Thermally-Induced Gelation of Cellulose in Aqueous Alkali
  • 2018
  • Ingår i: GELS. - : MDPI AG. - 2310-2861. ; 4:4
  • Tidskriftsartikel (refereegranskat)abstract
    • The gelation of cellulose in alkali solutions is quite relevant, but still a poorly understood process. Moreover, the role of certain additives, such as urea, is not consensual among the community. Therefore, in this work, an unusual set of characterization methods for cellulose solutions, such as cryo-transmission electronic microscopy (cryo-TEM), polarization transfer solid-state nuclear magnetic resonance (PTssNMR) and diffusion wave spectroscopy (DWS) were employed to study the role of urea on the dissolution and gelation processes of cellulose in aqueous alkali. Cryo-TEM reveals that the addition of urea generally reduces the presence of undissolved cellulose fibrils in solution. These results are consistent with PTssNMR data, which show the reduction and in some cases the absence of crystalline portions of cellulose in solution, suggesting a pronounced positive effect of the urea on the dissolution efficiency of cellulose. Both conventional mechanical macrorheology and microrheology (DWS) indicate a significant delay of gelation induced by urea, being absent until ca. 60 degrees C for a system containing 5wt % cellulose, while a system without urea gels at a lower temperature. For higher cellulose concentrations, the samples containing urea form gels even at room temperature. It is argued that since urea facilitates cellulose dissolution, the high entanglement of the cellulose chains in solution (above the critical concentration, C*) results in a strong three-dimensional network.
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5.
  • Alves, Luis, et al. (författare)
  • On the rheology of mixed systems of hydrophobically modified polyacrylate microgels and surfactants : Role of the surfactant architecture
  • 2018
  • Ingår i: Journal of Colloid and Interface Science. - : Elsevier BV. - 0021-9797 .- 1095-7103. ; 513, s. 489-496
  • Tidskriftsartikel (refereegranskat)abstract
    • Hypothesis The rheological control of suspensions is of key interest in the formulation design. A chemically cross-linked hydrophobically modified poly(acrylic acid) (HMCL-PAA), used as rheology modifier, is pH sensitive and shows swelling behavior above a critical pH due to the ionization of the acrylic acid groups. At low pH, HMCL-PAA suspensions are liquid and turbid. The binding of surfactants to HMCL-PAA, at low pH conditions, can result in significant changes on rheology and transparency of the polymeric suspensions, due to the swelling of the microgel particles. Experiments The influence of surfactants addition on the rheological properties and transparency of HMCL-PAA suspensions was determined. A systematic study was performed using different types of surfactants (ionic, non-ionic and zwitterionic). Findings The gelation efficiency of HMCL-PAA suspensions at low pH is strongly dependent on surfactant architecture: ionic surfactants are found to be much more efficient than non-ionic or zwitterionic surfactants. Ionic surfactants lead to a liquid-to-gel transition accompanied by an increase of transparency of the suspensions. Among the ionic surfactants, anionics show stronger interactions with the polymer. Also the surfactant hydrophobicity is relevant; the more hydrophobic the surfactant, the stronger is the binding to the polymer and thus the larger the particle swelling. 
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6.
  • Alves, Luis, et al. (författare)
  • Revisiting the dissolution of cellulose in H3PO4(aq) through cryo-TEM, PTssNMR and DWS
  • 2021
  • Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 252
  • Tidskriftsartikel (refereegranskat)abstract
    • Cellulose can be dissolved in concentrated acidic aqueous solvents forming extremely viscous solutions, and, in some cases, liquid crystalline phases. In this work, the concentrated phosphoric acid aqueous solvent is revisited implementing a set of advanced techniques, such as cryo-transmission electronic microscopy (cryo-TEM), polarization transfer solid-state nuclear magnetic resonance (PTssNMR), and diffusing wave spectroscopy (DWS). Cryo-TEM images confirm that this solvent system is capable to efficiently dissolve cellulose. No cellulose particles, fibrils, or aggregates are visible. Conversely, PTssNMR revealed a dominant CP signal at 25 °C, characteristic of C-H bond reorientation with correlation time longer than 100 ns and/or order parameter above 0.5, which was ascribed to a transient gel-like network or an anisotropic liquid crystalline phase. Increasing the temperature leads to a gradual transition from CP to INEPT-dominant signal and a loss of birefringence in optical microscopy, suggesting an anisotropic-to-isotropic phase transition. Finally, an excellent agreement between optical microrheology and conventional mechanical rheometry was also obtained. 
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7.
  • Alves, L., et al. (författare)
  • Unusual extraction and characterization of nanocrystalline cellulose from cellulose derivatives
  • 2015
  • Ingår i: Journal of Molecular Liquids. - : Elsevier BV. - 0167-7322 .- 1873-3166. ; 210, s. 106-112
  • Tidskriftsartikel (refereegranskat)abstract
    • Unlike many nanomaterials, nanocrystalline cellulose (CNC) is not synthesized from molecular or atomic components but rather extracted from naturally occurring cellulose. Undoubtedly, the exploitation of CNCs will become a bridge between nanoscience and natural resource products, which could play a major role in reviving the forest industry. In this work, CNC was successfully extracted from unusual sources, hydroxypropyl methylcellulose (HPMC) and carboxymethylcellulose (CMC). The extracted crystallites were purified and further characterized by Fourier transform infrared (FTIR), scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and dynamic light scattering (DLS). The average size of the CNCs extracted from HPMC and CMC was found to be less (and with lower zeta potential) than the ones extracted from microcrystalline cellulose (MCC). On the other hand, FTIR and XRD revealed that native HPMC and CMC are unexpectedly highly crystalline and hence can be used as a source for CNCs. © 2014 Elsevier B.V.All rights reserved.
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8.
  • Amenitsch, H, et al. (författare)
  • Bile salts form lyotropic liquid crystals
  • 2003
  • Ingår i: Colloids and Surfaces A: Physicochemical and Engineering Aspects. - 0927-7757 .- 1873-4359. ; 213:1, s. 79-92
  • Tidskriftsartikel (refereegranskat)abstract
    • A reinvestigation of the phase diagrams relative to some conjugated and non-conjugated bile salts in water has demonstrated the formation of lyotropic liquid crystalline phases, in contradiction with generally accepted statements. The phase behaviour is complex and the phase diagrams are unusual, compared to most surfactants and lipids. In particular, coexistence of liquid crystalline phases with crystals has been obser ed. The formation of liquid crystalline phases requires very long equilibration times and the thermal stability of the lyotropic phases is moderate. The observed structure is tentatively assumed to be of the reverse hexagonal type. Structural relations with currently accepted models for the organisation of bile salts into micelles and solid form have been found. (C) 2002 Elsevier Science B.V. All rights reserved.
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9.
  • An, S., et al. (författare)
  • Characterization of micro pore optics for full-field X-ray fluorescence imaging
  • 2023
  • Ingår i: Journal of Instrumentation. - 1748-0221. ; 18:1
  • Tidskriftsartikel (refereegranskat)abstract
    • Elemental mapping images can be achieved through step scanning imaging using pinhole optics or micro pore optics (MPO), or alternatively by full-field X-ray fluorescence imaging (FF-XRF). X-ray optics for FF-XRF can be manufactured with different micro-channel geometries such as square, hexagonal or circular channels. Each optic geometry creates different imaging artefacts. Square-channel MPOs generate a high intensity central spot due to two reflections via orthogonal channel walls inside a single channel, which is the desirable part for image formation, and two perpendicular lines forming a cross due to reflections in one plane only. Thus, we have studied the performance of a square-channel MPO in an FF-XRF imaging system. The setup consists of a commercially available MPO provided by Photonis and a Timepix3 readout chip with a silicon detector. Imaging of fluorescence from small metal particles has been used to obtain the point spread function (PSF) characteristics. The transmission through MPO channels and variation of the critical reflection angle are characterized by measurements of fluorescence from copper and titanium metal fragments. Since the critical angle of reflection is energy dependent, the cross-arm artefacts will affect the resolution differently for different fluorescence energies. It is possible to identify metal fragments due to the form of the PSF function. The PSF function can be further characterized using a Fourier transform to suppress diffuse background signals in the image.
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10.
  • Anastasopoulos, M., et al. (författare)
  • Multi-Grid detector for neutron spectroscopy : Results obtained on time-of-flight spectrometer CNCS
  • 2017
  • Ingår i: Journal of Instrumentation. - : IOP PUBLISHING LTD. - 1748-0221 .- 1748-0221. ; 12:4
  • Tidskriftsartikel (refereegranskat)abstract
    • The Multi-Grid detector technology has evolved from the proof-of-principle and characterisation stages. Here we report on the performance of the Multi-Grid detector, the MG.CNCS prototype, which has been installed and tested at the Cold Neutron Chopper Spectrometer, CNCS at SNS. This has allowed a side-by-side comparison to the performance of 3He detectors on an operational instrument. The demonstrator has an active area of 0.2 m2. It is specifically tailored to the specifications of CNCS. The detector was installed in June 2016 and has operated since then, collecting neutron scattering data in parallel to the He-3 detectors of CNCS. In this paper, we present a comprehensive analysis of this data, in particular on instrument energy resolution, rate capability, background and relative efficiency. Stability, gamma-ray and fast neutron sensitivity have also been investigated. The effect of scattering in the detector components has been measured and provides input to comparison for Monte Carlo simulations. All data is presented in comparison to that measured by the 3He detectors simultaneously, showing that all features recorded by one detector are also recorded by the other. The energy resolution matches closely. We find that the Multi-Grid is able to match the data collected by 3He, and see an indication of a considerable advantage in the count rate capability. Based on these results, we are confident that the Multi-Grid detector will be capable of producing high quality scientific data on chopper spectrometers utilising the unprecedented neutron flux of the ESS.
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