TY - JOUR A1 - Ji, Y. A1 - Becker, S. A1 - Lu, Z. A1 - Mezhov, Alexander A1 - von Klitzing, R. A1 - Schmidt, Wolfram A1 - Stephan, D. T1 - Effect of resting time on rheological properties of glass bead suspensions - Depletion and bridging force among particles N2 - The effect of resting time on the rheological properties of cement suspensions is generally explained by early formed structure and overconsumption of polycarboxylate superplasticizers (PCEs). In this paper, we propose that the influence of resting time on the rheological properties is closely related to size variation of non-absorbed PCE. To identify this, glass bead suspensions were prepared with various amounts of PCE and ionic solution, and their rheological properties were evaluated at various times. We found that the yield stress increases with time at higher PCE concentrations and higher ionic strength solutions. Adsorbed PCE during resting tends to bridge the particles rather than disperse them. In addition, it was found that hydrodynamic radius of PCE increased with resting time, and depletion forces resulting from non-absorbed PCE size changes correlate well with the increased yield stress. KW - Depletion force KW - Ionic stregth KW - PCE KW - Rheology KW - Resting time PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587193 DO - https://doi.org/10.1111/jace.19469 SN - 0002-7820 SN - 1551-2916 VL - 107 IS - 1 SP - 624 EP - 639 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-58719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Z. A1 - Becker, S. A1 - Leinitz, Sarah A1 - Schmidt, Wolfram A1 - von Klitzing, R. A1 - Stephan, D. T1 - Interaction of Different Charged Polymers with Potassium Ions and Their Effect on the Yield Stress of Highly Concentrated Glass Bead Suspensions N2 - The interaction of different charged polymers, namely anionic polycarboxylate superplasticizer (PCE) and neutral polyethylene glycol (PEG) with potassium ions, and their effect on the yield stress of highly concentrated glass bead suspension (GBS), were studied under different concentrations of potassium ions ([K+]). It was found that, compared to the neutral PEG, the negatively charged PCE can be adsorbed on glass beads (GB), and then decreases the yield stress of GBS. The increasing concentration of free polymer in the interstitial liquid phase with the increased polymer dosage leads to the higher yield stress of GBS, which may be caused by the higher Depletion force. In addition, this effect is also related to the charge density of the polymer and the [K+] in the solution. Along with the increase in [K+], the yield stress of GBS increases significantly with the addition of PCE, but this cannot be observed with PEG, which indicates that potassium ions can interact with negatively charged PCE instead of the neutral PEG. At last, the interparticle Forces between two single GB with adsorbed PCE in solutions containing [K+] and PCE were measured by colloidal probe atomic force microscopy to better understand the interaction of the charged polymer with counterions. KW - Yield stress KW - Free polymer KW - Charge density KW - Depletion force KW - Potassium ions PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506015 DO - https://doi.org/10.3390/ma13071490 SN - 1996-1944 VL - 13 IS - 7 SP - 1490, 1 EP - 1490, 16 PB - MDPI AN - OPUS4-50601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Becker, S. A1 - Lu, Z. A1 - Leinitz, Sarah A1 - Schmidt, Wolfram A1 - Stephan, D. A1 - von Klitzing, R. ED - Mechtcherine, V. ED - Khayat, K. ED - Secrieru, E. T1 - Particle Interactions in Silica Systems in Presence of Superplasticizer N2 - The flowability of cement paste is of great importance in today’s construction industry and is influenced by additives such as superplasticizers (SP). One type of SPs are polycarboxylate ether type SPs. These additives electrostatically bind with the negatively charged carboxylic groups at the backbone to the positively charged clinker phases. To model positively charged clinker phases with adsorbed SP, silicon Wafers are pre-coated with cationic polyethylenimine (PEI) and SP is adsorbed onto the coated surface (Si/PEI/SP). Two different polycarboxylate ether type (PCE) SP are compared – one for ready-mix concrete and one for precast concrete. In this preliminary study the interaction forces between Si/PEI/SP surface and a silica microsphere (colloidal probe) are investigated under mild physico-chemical conditions (pH *6, ion concentration <10−5 M) using Colloidal Probe Atomic Force Microscopy (CP-AFM). The interaction force between the model surfaces is attractive for low concentration of SP. The force changes from attractive to repulsive by increasing amount of SP. The force upon approach reveals a biexponential behavior. The exponential decay at large and short surface separations are attributed to electrostatic and steric interactions, respectively. The steric forces of the SP for ready-mix concrete show a steeper onset than the SP for precast concrete. The quantification of these interaction forces will be compared to rheological measurements of similar systems. Furthermore, the parameters will be changed to better approach the conditions in real systems, i.e. higher pH and ionic strength. This helps to understand how the forces on the nanoscale influence the macroscopic rheology. KW - Interfacial forces KW - Silica beads KW - Superplasticizer KW - AFM PY - 2019 SN - 978-3-030-22565-0 DO - https://doi.org/10.1007/978-3-030-22566-7 SN - 2211-0844 VL - 23 SP - 571 EP - 579 PB - Springer ET - 1 AN - OPUS4-49183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Lu, Z. A1 - Becker, S. A1 - Leinitz, Sarah A1 - von Klitzing, R. A1 - Schmidt, Wolfram A1 - Stephan, D. ED - Mechtcherine, V. ED - Khayat, K. ED - Secrieru, E. T1 - Rheological properties of silica beads in the presence of different polymers and electrolyte N2 - Properties of interstitial liquid phase in cement paste, including the species and concentrations of polymers and ion etc., play an important role for the rheological properties of cementitious materials. In order to better understand their effect, an inert model substance, spherical silica beads (SBs) with defined surface and granulometry were used in the presence of electrolytes (CaCl2) and/or different polymers, including polycarboxylate superplasticizer (PCE) and polyethylene glycol (PEG). It was found the presence of Ca2+ greatly increases the viscosity and yield stress of silica beads paste (SBP), which is proportional to the [Ca2+]. For the effect of PCE, the addition of PCE is beneficial to the flowability of SBP, but a high dosage of PCE leads to a reversal effect. Furthermore, the yield stress firstly increases and then decreases with increasing [Ca2+] under the same dosage of PCE. The addition of PEG always increases the yield stress of SBP, regardless of the ion concentration and the presence or not of PCE. KW - Rheological properties KW - Ions KW - Superplasticizer KW - Silica beads PY - 2019 SN - 978-3-030-22565-0 SN - 978-3-030-22566-7 DO - https://doi.org/10.1007/978-3-030-22566-7_72 SN - 2211-0844 VL - 23 SP - 619 EP - 627 PB - Springer ET - 1 AN - OPUS4-49185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Leinitz, Sarah A1 - Lu, Z. A1 - Becker, S. A1 - Stephan, D. A1 - von Klitzing, R. A1 - Schmidt, Wolfram ED - Mechtcherine, V. ED - Khayat, K. ED - Secrieru, E. T1 - Influence of different accelerators on the rheology and early hydration of cement paste N2 - Special applications like pumping, spraying or printing of concrete require the precise adjustment of very specific rheological properties at different time steps during the casting process. Superplasticizers such as polycarboxylate ethers (PCE) can be used to obtain the required flowability, which, possibly in combination with additional rheology modifying admixtures, generate the required specified consistency. However, after the application, the concrete should change the rheological properties immediately in order to avoid deformations at rest. Therefore, the use of accelerators can be effective. Accelerators influence the hydration of cementitious materials, and thus the rheological properties over the course of time and the setting. In this paper, the influence of different accelerators on the rheology and early hydration of cement paste as well as the interaction of accelerator and PCE are presented. Methods like rheometry, needle penetration tests and practical Tests like spread flow were applied. The used accelerators showed accelerating behavior on the cement pastes without and in the presence of PCE. At the same time an influence on the rheology could be observed. This effect was less in the mixes with PCE, especially at the highest water/cement ratio (w/c). KW - Rheology KW - Cement paste KW - Accelerator KW - Superplasticizer KW - Setting PY - 2019 SN - 978-3-030-22565-0 DO - https://doi.org/10.1007/978-3-030-22566-7 SN - 2211-0844 VL - 23 SP - 106 EP - 115 PB - Springer ET - 1 AN - OPUS4-49139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Heídari, M. A1 - von Klitzing, R. A1 - Schönhals, Andreas T1 - Unveiling the dynamics of self-assembled layers of thin films of poly(vinyl methyl ether) (PVME) by nanosized relaxation spectroscopy N2 - A combination of nanosized dielectric relaxation (BDS) and thermal spectroscopy (SHS) was utilized to characterize the dynamics of thin films of Poly(vinyl methyl ether) (PVME) (thicknesses: 7 nm – 160 nm). For the BDS measurements, a recently designed nano-structured electrode system is employed. A thin film is spin-coated on an ultra-flat highly conductive silicon wafer serving as the bottom electrode. As top electrode, a highly conductive wafer with non-conducting nanostructured SiO2 nano-spacers with heights of 35 nm or 70 nm is assembled on the bottom electrode. This procedure results in thin supported films with a free polymer/air interface. The BDS measurements show two relaxation processes, which are analyzed unambiguously for thicknesses smaller than 50 nm. The relaxation rates of both processes have different temperature dependencies. One process coincidences in its position and temperature dependence with the glassy dynamics of bulk PVME and is ascribed to the dynamic glass transition of a bulk-like layer in the middle of the film. The relaxation rates were found to be thickness independent as confirmed by SHS. Unexpectedly, the relaxation rates of the second process obey an Arrhenius-like temperature dependence. This process was not observed by SHS and was related to the constrained fluctuations in a layer, which is irreversibly adsorbed at the substrate with a heterogeneous structure. Its molecular fluctuations undergo a confinement effect resulting in the localization of the segmental dynamics. To our knowledge, this is the first report on the molecular dynamics of an adsorbed layer in thin films. KW - Broadband dielectric spectroscopy KW - AC-nanochip calorimetry KW - Nanostructured capacitors KW - Thin films PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acsami.6b14404 DO - https://doi.org/10.1021/acsami.6b14404 SN - 1944-8244 VL - 9 IS - 8 SP - 7535 EP - 7546 PB - ACS Publications CY - Washington DC AN - OPUS4-39291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Heidari, M. A1 - von Klitzing, R. A1 - Napolitano, S. A1 - Sferrazza, M. A1 - Schönhals, Andreas T1 - Decoupling of dynamic and thermal glass transition in thin films of a PVME/PS blend N2 - The discussions on the nanoconfinement effect on the glass transition and glassy dynamics phenomena have yielded many open questions. Here, the thickness dependence of the thermal glass transition temperature of thin films of a PVME/PS blend is investigated by ellipsometry. Its thickness dependence was compared to that of the dynamic glass transition (measured by specific heat spectroscopy), and the deduced Vogel temperature (T0). While and T0 showed a monotonous increase, with decreasing the film thickness, the dynamic glass transition temperature () measured at a finite frequency showed a non-monotonous dependence that peaks at 30 nm. This was discussed by assuming different cooperativity length scales at these temperatures, which have different sensitivities to composition and thickness. This non-monotonous thickness dependence of disappears for frequencies characteristic for T0. Further analysis of the fragility parameter, showed a change in the glassy dynamics from strong to fragile, with decreasing film thickness. KW - Thin polymeric films KW - Ellipsometry KW - Specific heat spectroscopy PY - 2017 DO - https://doi.org/10.1021/acsmacrolett.7b00625 SN - 2161-1653 VL - 6 IS - 10 SP - 1156 EP - 1161 PB - ACS Publications AN - OPUS4-42266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -