Neutron Reflectometry Measurements Research Articles

AutoRefl: active learning in neutron reflectometry for fast data acquisition

Neutron reflectometry (NR) is a powerful technique for interrogating the structure of thin films at interfaces. Because NR measurements are slow and instrument availability is limited, measurement efficiency is paramount. One approach to improving measurement efficiency is active learning (AL), in which the next measurement configurations are selected on the basis of information gained from the partial data collected so far. AutoRefl, a model-based AL algorithm for neutron reflectometry measurements, is presented in this manuscript. AutoRefl uses the existing measurements of a function to choose both the position and the duration of the next measurement. AutoRefl maximizes the information acquisition rate in specific model parameters of interest and uses the well defined signal-to-noise ratio in counting measurements to choose appropriate measurement times. Since continuous measurement is desirable for practical implementation, AutoRefl features forecasting, in which the optimal positions of multiple future measurements are predicted from existing measurements. The performance of AutoRefl is compared with that of well established best practice measurements for supported lipid bilayer samples using realistic digital twins of monochromatic and polychromatic reflectometers. AutoRefl is shown to improve NR measurement speeds in all cases significantly.

Syntropic spin alignment at the interface between ferromagnetic and superconducting nitrides.

The magnetic correlations at the superconductor/ferromagnet (S/F) interfaces play a crucial role in realizing dissipation-less spin-based logic and memory technologies, such as triplet-supercurrent spin-valves and 'π' Josephson junctions. Here we report the observation of an induced large magnetic moment at high-quality nitride S/F interfaces. Using polarized neutron reflectometry and DC SQUID measurements, we quantitatively determined the magnetization profile of the S/F bilayer and confirmed that the induced magnetic moment in the adjacent superconductor only exists below T C. Interestingly, the direction of the induced moment in the superconductors was unexpectedly parallel to that in the ferromagnet, which contrasts with earlier findings in S/F heterostructures based on metals or oxides. First-principles calculations verified that the unusual interfacial spin texture observed in our study was caused by the Heisenberg direct exchange coupling with constant J∼4.28 meV through d-orbital overlapping and severe charge transfer across the interfaces. Our work establishes an incisive experimental probe for understanding the magnetic proximity behavior at S/F interfaces and provides a prototype epitaxial 'building block' for superconducting spintronics.

Interface Effect on the Out‐of‐Plane Spin‐Orbit Torque in the Ferromagnetic CoPt Single Layers

AbstractField‐free switching of a perpendicularly magnetized heavy metal/ferromagnetic metal bilayer or single alloy layer through spin‐orbit torque (SOT) provides a potential way for next‐generation spintronic devices with fast speed and high efficiency. Here, a sizable symmetry dependence of field‐free magnetization switching via an out‐of‐plane torque in CoxPt100−x single layers is reported. It is found that the sign of in‐plane SOT in CoxPt100−x when x ≤ 25 is positive. However, it changes to negative when x > 25, while the out‐of‐plane SOT changes its sign when x > 30. The polarized neutron reflectometry measurement further suggests an interface layer with rich Pt content near the substrate, which could have a strong interface effect on the out‐of‐plane SOT. The sign of the out‐of‐plane SOT, and then the polarity of the field‐free magnetization switching, is determined by the competition between the out‐of‐plane torques arising from the bulk and interface parts in the CoxPt100−x single layers. It is expected that such interface effect of the out‐of‐plane torque is desirable to the applications in spin logic devices using symmetry dependence of field‐free magnetization switching in the ferromagnetic CoPt single layers.

Mesoscale self-organization of polydisperse magnetic nanoparticles at the water surface.

In this study, we investigated the self-ordering process in Langmuir films of polydisperse iron oxide nanoparticles on a water surface, employing in situ x-ray scattering, surface pressure-area isotherm analysis, and Brewster angle microscopy. X-ray reflectometry confirmed the formation of a monolayer, while grazing incidence small-angle x-ray scattering revealed short-range lateral correlations with a characteristic length equal to the mean particle size. Remarkably, our findings indicated that at zero surface pressure, the particles organized into submicrometer clusters, merging upon compression to form a homogeneous layer. These layers were subsequently transferred to a solid substrate using the Langmuir-Schaefer technique and further characterized via scanning electron microscopy and polarized neutron reflectometry. Notably, our measurements revealed a second characteristic length in the lateral correlations, orders of magnitude longer than the mean particle diameter, with polydisperse particles forming circular clusters densely packed in a hexagonal lattice. Furthermore, our evidence suggests that the lattice constant of this mesocrystal depends on the characteristics of the particle size distribution, specifically the mean particle size and the width of the size distribution. In addition, we observed internal size separation within these clusters, where larger particles were positioned closer to the center of the cluster. Finally, polarized neutron reflectometry measurements provided valuable insights into the magnetization profile across the layer.

Morphology of Thin-Film Nafion on Carbon as an Analogue of Fuel Cell Catalyst Layers.

Species transport in thin-film Nafion heavily influences proton-exchange membrane (PEMFC) performance, particularly in low-platinum-loaded cells. Literature suggests that phase-segregated nanostructures in hydrated Nafion thin films can reduce species mobility and increase transport losses in cathode catalyst layers. However, these structures have primarily been observed at silicon-Nafion interfaces rather than at more relevant material (e.g., Pt and carbon black) interfaces. In this work, we use neutron reflectometry and X-ray photoelectron spectroscopy to investigate carbon-supported Nafion thin films. Measurements were taken in humidified environments for Nafion thin films (≈30-80 nm) on four different carbon substrates. Results show a variety of interfacial morphologies in carbon-supported Nafion. Differences in carbon samples' roughness, surface chemistry, and hydrophilicity suggest that thin-film Nafion phase segregation is impacted by multiple substrate characteristics. For instance, hydrophilic substrates with smooth surfaces correlate with a high likelihood of lamellar phase segregation parallel to the substrate. When present, the lamellar structures are less pronounced than those observed at silicon oxide interfaces. Local oscillations in water volume fraction for the lamellae were less severe, and the lamellae were thinner and were not observed when the water was removed, all in contrast to Nafion-silicon interfaces. For hydrophobic and rough samples, phase segregation was more isotropic rather than lamellar. Results suggest that Nafion in PEMFC catalyst layers is less influenced by the interface compared with thin films on silicon. Despite this, our results demonstrate that neutron reflectometry measurements of silicon-Nafion interfaces are valuable for PEMFC performance predictions, as water uptake in the majority Nafion layers (i.e., the uniformly hydrated region beyond the lamellar region) trends similarly with thickness, regardless of support material.

Distance tuneable integral membrane protein containing floating bilayers via in situ directed self-assembly.

Model membranes allow for structural and biophysical studies on membrane biochemistry at the molecular level, albeit on systems of reduced complexity which can limit biological accuracy. Floating supported bilayers offer a means of producing planar lipid membrane models not adhered to a surface, which allows for improved accuracy compared to other model membranes. Here we communicate the incorporation of an integral membrane protein complex, the multidomain β-barrel assembly machinery (Bam), into our recently developed in situ self-assembled floating supported bilayers. Using neutron reflectometry and quartz crystal microbalance measurements we show this sample system can be fabricated using a two-step self-assembly process. We then demonstrate the complexity of the model membrane and tuneability of the membrane-to-surface distance using changes in the salt concentration of the bulk solution. Results demonstrate an easily fabricated, biologically accurate and tuneable membrane assay system which can be utilized for studies on integral membrane proteins within their native lipid matrix.

Epitaxial graphene growth on cubic silicon carbide on silicon with high temperature neutron reflectometry: an operando study.

The growth of graphene on silicon carbide on silicon offers a very attractive route towards novel wafer-scale photonic and electronic devices that are easy to fabricate and can be integrated in silicon manufacturing. Using a Ni/Cu catalyst for the epitaxial growth of graphene has been successful in the mitigation of the very defective nature of the underlying silicon carbide on silicon, leading to a consistent graphene coverage over large scales. A more detailed understanding of this growth mechanism is warranted in order to further optimise the catalyst composition, preferably via the use of operando characterization measurements. Here, we report in situ neutron reflectometry measurements of (Ni, Cu)/SiC films on silicon wafers, annealed from room temperature to 1100 °C, which initiates graphene formation at the buried (Ni, Cu)/SiC interface. Detailed modelling of the high temperature neutron reflectometry and corresponding scattering length density profiles yield insights into the distinct physical mechanisms within the different temperature regimes. The initially smooth solid metallic layers undergo intermixing and roughening transitions at relatively low temperatures below 500 °C, and then metal silicides begin to form above 600 °C from interfacial reactions with the SiC, releasing atomic carbon. At the highest temperature range of 600-1100 °C, the low neutron scattering length density at high temperature is consistent with a silicon-rich, liquid surface phase corresponding to molten nickel silicides and copper. This liquid catalyst layer promotes the liquid-phase epitaxial growth of a graphene layer by precipitating the excess carbon available at the SiC/metal interface.

Analysis of the Diffusion in a Multilayer Structure under a Constant Heating Rate: The Calculation of Activation Energy from the In Situ Neutron Reflectometry Measurement.

Understanding mass transport in micro- and nanostructures is of paramount importance in improving the performance and reliability of the micro- and nanostructures. In this work, we solve the diffusion problem in a multilayer structure with periodic conditions under a constant heating rate via a Fourier series. Analytical relation is established between the coefficients of eigenfunctions and the intensity of X-ray or neutron Bragg peak. The logarithm of temporal variation of the intensity of X-ray or neutron Bragg peak is a linear function of the nominal diffusion time, with the nominal diffusion time being dependent on the heating rate. This linear relation is validated by experimental data. The Taylor series expansion of the linear relation to the first order of the diffusion time yields an approximately linear relation between the logarithm of temporal variation of the intensity of X-ray or neutron peak and the diffusion time for small diffusion times, which can be likely used to calculate the activation energy for the diffusion in a multilayer structure. The validation of such an approach is subjected to the fact that the characteristic time for heat conduction is much less than the characteristic time for the ramp heating as well as the characteristic time for diffusion.

In Situ Measurement of Buried Electrolyte–Electrode Interfaces for Solid State Batteries with Nanometer Level Precision

Many technologies including high-energy solid-state batteries rely on high quality solid–solid interfaces. Solid–solid interfaces are particularly difficult to study as their nature requires the interface to be buried. In this work we demonstrate the use of a combination of neutron reflectometry and in situ electrochemistry to measure the interface between Li metal and the solid electrolyte LiPON across an 8 cm2 area. Neutron reflectometry measurements confirm the interphase to be less than 7 nm thick. The neutron reflectometry data further emphasize that the interphase that forms is a chemical gradient consisting of a Li-rich layer that gradually decreases in Li content until it blends into pure LiPON. Experimental confirmation that we can make ideal solid–solid interphases less than 10 nm thick will help facilitate the adoption of high efficiency next generation solid state batteries. Further this combination of complementary techniques provides a more general methodology for studying buried solid–solid interfaces across applications.

Significantly Enhanced Room-Temperature Ferromagnetism in Multiferroic EuFeO3-δ Thin Films.

Regulating the magnetic properties of multiferroics lays the foundation for their prospective application in spintronic devices. Single-phase multiferroics, such as rare-earth ferrites, are promising candidates; however, they typically exhibit weak magnetism at room temperature (RT). Here, we significantly boosted the RT ferromagnetism of a representative ferrite, EuFeO3, by oxygen defect engineering. Polarized neutron reflectometry and magnetometry measurements reveal that saturation magnetization reaches 0.04 μB/Fe, which is approximately 5 times higher than its bulk phase. Combining the annular bright-field images with theoretical assessment, we unravel the underlying mechanism for magnetic enhancement, in which the decrease in Fe-O-Fe bond angles caused by oxygen vacancies (VO) strengthens magnetic interactions and tilts Fe spins. Furthermore, the internal relationship between magnetism and VO was established by illustrating how the magnetic structure and magnitude change with VO configuration and concentration. Our strategy for regulating magnetic properties can be applied to numerous functional oxide materials.

Tailoring the magnetic exchange interaction in MnBi2Te4 superlattices via the intercalation of ferromagnetic layers

The intrinsic magnetic topological insulator MnBi2Te4 (MBT) provides a platform for the creation of exotic quantum phenomena. Novel properties can be created by modification of the MnBi2Te4 framework, but the design of stable magnetic structures remains challenging. Here we report ferromagnet-intercalated MnBi2Te4 superlattices with tunable magnetic exchange interactions. Using molecular beam epitaxy, we intercalate ferromagnetic MnTe layers into MnBi2Te4 to create [(MBT)(MnTe)m]N superlattices and examine their magnetic interaction properties using polarized neutron reflectometry and magnetoresistance measurements. Incorporation of the ferromagnetic spacer tunes the antiferromagnetic interlayer coupling of the MnBi2Te4 layers through the exchange-spring effect at MnBi2Te4/MnTe hetero-interfaces. The MnTe thickness can be used to modulate the relative strengths of the ferromagnetic and antiferromagnetic order, and the superlattice periodicity can tailor the spin configurations of the synthesized multilayers.

Strain and charge contributions to the magnetoelectric coupling in Fe3O4/PMN-PT artificial multiferroic heterostructures

The quest to realize new kinds of data storage devices has motivated recent studies in the field of magnetoelectric heterostructures. One of the most commonly investigated systems is Fe3O4/[Pb(MgNbO3]0.7–[PbTiO3]0.3 (PMN-PT), however, the interplay between different coupling mechanisms is not yet well understood. To disentangle the role of strain and polarisation influence in Fe3O4/PMN-PT, we report on magnetoelectric coupling measurements for different orientations of the applied magnetic field and for two different substrate cuts, PMN-PT(001) and PMN-PT(011). For Fe3O4/PMN-PT(011), having the sample aligned such that the magnetic field is parallel to the [01] easy axis leads to a remanent increase of the magnetisation for each electric field cycle. On the other hand, for the magnetic field along the [100] hard axis, the magnetisation follows a butterfly-like loop characteristic of strain coupling imparted by the substrate. For Fe3O4/PMN-PT(001), the magnetoelectric effect is a superposition of the observed behaviour of both in-plane directions in Fe3O4/PMN-PT(011). The magnetisation shows an initial remanent increase followed by a butterfly like loop. Polarised neutron reflectometry measurements on Fe3O4/PMN-PT(011) shows no difference between the behaviour at the interface and the bulk of the film and no decline of the interaction further away from the shared interface. Our results demonstrate the role of strain and polarisation on the magnetisation of the Fe3O4 layer and provide a clear step towards the design of future magnetoelectric systems.

Power losses in conventional and inverted non-polymeric donor:fullerene bulk heterojunction solar cells - The role of vertical phase separation in BQR:PC71BM blends

The performance of bulk heterojunction (BHJ) organic solar cells can be affected by a range of factors including the materials combination, processing solvent, post deposition annealing, and/or whether they are used in a conventional or inverted architecture. In this study we compared conventional and inverted BHJ solar cells composed of a non-polymeric donor (5 Z ,5′ Z )‐5,5'‐[(5‴,5‴''''‐{4,8‐bis[5‐(2‐ethylhexyl)‐4‐ n -hexylthiophen‐2‐yl]benzo[1,2‐b:4,5‐b']dithiophene‐2,6‐diyl}bis{3′,3'',3‴‐trihexyl‐[2,2':5′,2'':5'',2‴‐quaterthiophene]‐5‴,5‐diyl})bis(methanylylidene)]bis[3‐ n -hexyl‐2‐thioxothiazolidin‐4‐one] (BQR) and [6,6]-phenyl-C 71 -butyric acid methyl ester (PC 71 BM) as the acceptor. It was found that the conventional device structure had power conversion efficiencies nearly two and a half times that of the inverted device, 9.0% versus 4.0%. Through a combination of Shockley equivalent circuit fitting, optical modelling, and light intensity dependent photocurrent measurements we identified that the origin of the power losses for the inverted architecture relative to the conventional device structure arose from a larger component of bimolecular recombination. Neutron reflectometry measurements showed that the origin of the larger bimolecular recombination losses for the inverted device was due to the PC 71 BM phase separating, with a PC 71 BM rich layer located near the anode reducing the hole extraction efficiency. • BQR and PC 71 BM conventional and inverted BHJ solar cells are compared. • The conventional device structure was two and a half times more efficient. • Increased bimolecular recombination identified as the origin of the power losses for the inverted architecture. • A PC 71 BM rich layer near the anode reduced the hole extraction efficiency in inverted device.

Interfacial mixing effect in a promising skyrmionic material: Ferrimagnetic Mn4N

Interfacial mixing of elements is a well-known phenomenon found in thin film deposition. For thin-film magnetic heterostructures, interfacial compositional inhomogeneities can have drastic effects on the resulting functionalities. As such, care must be taken to characterize the compositional and magnetic properties of thin films intended for device use. Recently, ferrimagnetic Mn4N thin films have drawn considerable interest due to exhibiting perpendicular magnetic anisotropy, high domain-wall mobility, and good thermal stability. In this study, we employed x-ray photoelectron spectroscopy (XPS) and polarized neutron reflectometry (PNR) measurements to investigate the interfaces of an epitaxially grown MgO/Mn4N/Pt trilayer deposited at 450 °C. XPS revealed the thickness of elemental mixing regions of near 5 nm at both interfaces. Using PNR, we found that these interfaces exhibit essentially zero net magnetization at room temperature. Despite the high-temperature deposition at 450 °C, the thickness of mixing regions is comparable to those observed in magnetic films deposited at room temperature. Micromagnetic simulations show that this interfacial mixing should not deter the robust formation of small skyrmions, consistent with a recent experiment. The results obtained are encouraging in terms of the potential of integrating thermally stable Mn4N into future spintronic devices.

Emergent Magnetic Fan Structures in Manganite Homojunction Arrays.

Devices with tunable magnetic noncollinearity are important components of superconducting electronics and spintronics, but they typically require epitaxial integration of several complex materials. The spin-polarized neutron reflectometry measurements on La1-x Srx MnO3 homojunction arrays with modulated Sr concentration reported herein have led to the discovery of magnetic fan structures with highly noncollinear alignment of Mn spins and an emergent periodicity twice as large as the array's unit cell. The neutron data show that these magnetic superstructures can be fully long-range ordered, despite the gradual modulation of the doping level created by charge transfer and chemical intermixing. The degree of noncollinearity can be effectively adjusted by low magnetic fields. Notwithstanding their chemical and structural simplicity, oxide homojunctions thus show considerable promise as a platform for tunable complex magnetism and as a powerful design element of spintronicdevices.

Signatures of superconducting triplet pairing in Ni–Ga-bilayer junctions

Ni–Ga bilayers are a versatile platform for exploring the competition between strongly antagonistic ferromagnetic and superconducting phases. We characterize the impact of this competition on the transport properties of highly-ballistic Al/Al2O3(/EuS)/Ni–Ga tunnel junctions from both experimental and theoretical points of view. While the conductance spectra of junctions comprising Ni (3 nm)–Ga (60 nm) bilayers can be well understood within the framework of earlier results, which associate the emerging main conductance maxima with the junction films’ superconducting gaps, thinner Ni (1.6 nm)–Ga (30 nm) bilayers entail completely different physics, and give rise to novel large-bias (when compared to the superconducting gap of the thin Al film as a reference) conductance-peak subseries that we term conductance shoulders. These conductance shoulders might attract considerable attention also in similar magnetic superconducting bilayer junctions, as we predict them to offer an experimentally well-accessible transport signature of superconducting triplet pairings that are induced around the interface of the Ni–Ga bilayer. We further substantiate this claim performing complementary polarized neutron reflectometry measurements on the bilayers, from which we deduce (1) a nonuniform magnetization structure in Ga in a several nanometer-thick area around the Ni–Ga boundary and can simultaneously (2) satisfactorily fit the obtained data only considering the paramagnetic Meissner response scenario. While the latter provides independent experimental evidence of induced triplet superconductivity inside the Ni–Ga bilayer, the former might serve as the first experimental hint of its potential microscopic physical origin. Finally, we introduce a simple phenomenological toy model to confirm also from the theoretical standpoint that superconducting triplet pairings around the Ni–Ga interface can indeed lead to the experimentally observed conductance shoulders, which convinces that our claims are robust and physically justified. Arranging our work in a broader context, we expect that Ni–Ga-bilayer junctions could have a strong potential for future superconducting-spintronics applications whenever an efficient engineering of triplet-pairing superconductivity is required.

Reversible Hydrogen-Induced Phase Transformations in La0.7Sr0.3MnO3 Thin Films Characterized by In Situ Neutron Reflectometry.

We report on the mechanism for hydrogen-induced topotactic phase transitions in perovskite (PV) oxides using La0.7Sr0.3MnO3 as a prototypical example. Hydrogenation starts with lattice expansion confirmed by X-ray diffraction (XRD). The strain- and oxygen-vacancy-mediated electron-phonon coupling in turn produces electronic structure changes that manifest through the appearance of a metal insulator transition accompanied by a sharp increase in resistivity. The ordering of initially randomly distributed oxygen vacancies produces a PV to brownmillerite phase (La0.7Sr0.3MnO2.5) transition. This phase transformation proceeds by the intercalation of oxygen vacancy planes confirmed by in situ XRD and neutron reflectometry (NR) measurements. Despite the prevailing picture that hydrogenation occurs by reaction with lattice oxygen, NR results are not consistent with deuterium (hydrogen) presence in the La0.7Sr0.3MnO3 lattice at steady state. The film can reach a highly oxygen-deficient La0.7Sr0.3MnO2.1 metastable state that is reversible to the as-grown composition simply by annealing in air. Theoretical calculations confirm that hydrogenation-induced oxygen vacancy formation is energetically favorable in La0.7Sr0.3MnO3. The hydrogenation-driven changes of the oxygen sublattice periodicity and the electrical and magnetic properties similar to interface effects induced by oxygen-deficient cap layers persist despite hydrogen not being present in the lattice.

Low-background neutron reflectometry from solid/liquid interfaces

Liquid cells are an increasingly common sample environment for neutron reflectometry experiments and are critical for measuring the properties of materials at solid/liquid interfaces. Background scattering determines the maximum useful scattering vector, and hence the spatial resolution, of the neutron reflectometry measurement. The primary sources of background are the liquid in the cell reservoir and the materials forming the liquid cell itself. Thus, characterization and mitigation of these background sources are necessary for improvements in the signal-to-background ratio and resolution of neutron reflectometry measurements employing liquid cells. Single-crystal silicon is a common material used for liquid cells due to its low incoherent scattering cross section for neutrons, and the path lengths of the neutron beam through silicon can be several centimetres in modern cell designs. Here, a liquid cell is constructed with a sub-50 µm thick liquid reservoir encased in single-crystal silicon. It is shown that, at high scattering vectors, inelastic scattering from silicon represents a significant portion of the scattering background and is, moreover, structured, confounding efforts to correct for it by established background subtraction techniques. A significant improvement in the measurement quality is achieved using energy-analyzed detection. Energy-analyzed detection reduces the scattering background from silicon by nearly an order of magnitude, and from fluids such as air and liquids by smaller but significant factors. Combining thin liquid reservoirs with energy-analyzed detection and the high flux of the CANDOR polychromatic reflectometer at the NIST Center for Neutron Research, a background-subtracted neutron reflectivity smaller than 10−8 from a liquid cell sample is reported.

A high temperature cell for investigating interfacial structure on the molecular scale in molten salt/alloy systems.

In this work, we describe the designand development of an in situ neutron reflectometry cell for high temperature investigations of structural changes occurring at the interface between inorganic salts, in their molten state up to 800°C, and corrosion resistant alloys or other surfaces. In the cell, a molten salt is confined by an annular ring of single crystal sapphire constrained between the sample substrate and a sapphire plate using two gold O-rings, enclosing a liquid salt volume of 20 ml, along with a dynamic cell volume to accommodate expansion of the liquid with heating. As a test case for the cell, we report on an in situ neutron reflectometry measurement of the interface between a eutectic salt mixture of MgCl2-KCl (32:68 molar ratio) and a single crystal sapphire substrate at 450°C, resulting in the formation of a 60 Å layer having a scattering length density of 1.72 × 10-6 Å-2. While the origin of this layer is uncertain, it is likely to have resulted from the salt reacting with an existing impurity layer on the sapphire substrate.

Salt-Dependent Phase Transition Behavior of Doubly Thermoresponsive Poly(sulfobetaine)-Based Diblock Copolymer Thin Films.

The water vapor-induced swelling, as well as subsequent phase-transition kinetics, of thin films of a diblock copolymer (DBC) loaded with different amounts of the salt NaBr, is investigated in situ. In dilute aqueous solution, the DBC features an orthogonally thermoresponsive behavior. It consists of a zwitterionic poly(sulfobetaine) block, namely, poly(4-(N-(3'-methacrylamidopropyl)-N,N-dimethylammonio) butane-1-sulfonate) (PSBP), showing an upper critical solution temperature, and a nonionic block, namely, poly(N-isopropylmethacrylamide) (PNIPMAM), exhibiting a lower critical solution temperature. The swelling kinetics in D2O vapor at 15 °C and the phase transition kinetics upon heating the swollen film to 60 °C and cooling back to 15 °C are followed with simultaneous time-of-flight neutron reflectometry and spectral reflectance measurements. These are complemented by Fourier transform infrared spectroscopy. The collapse temperature of PNIPMAM and the swelling temperature of PSBP are found at lower temperatures than in aqueous solution, which is attributed to the high polymer concentration in the thin-film geometry. Upon inclusion of sub-stoichiometric amounts (relative to the monomer units) of NaBr in the films, the water incorporation is significantly increased. This increase is mainly attributed to a salting-in effect on the zwitterionic PSBP block. Whereas the addition of NaBr notably shifts the swelling temperature of PSBP to lower temperatures, the collapse temperature of PNIPMAM remains unaffected by the presence of salt in the films.