Types of Nuclear Magnetic Resonance Spectroscopy Solid-state NMRs are used for chemical analysis to recognize any changes in the structure during phase transitions and different transformations in a solid state.
Phosphorus Nuclear Magnetic Resonance In the solid-state NMR, phosphorus is one of the isotopes used to study the molecules and structures of different samples. Adjustability Extensive variety of processes can be investigated through NMR due to the flexibility of the particular technique that can be applied. Detailed Structural Analysis Over the period, NMR has played a major responsibility in determining the mechanisms and chemical connections at a molecular level.
Presence of High Magnetic Field Surroundings Is Essential An unavoidable outcome when performing the NMR technique is the requirement to perform in a surrounding which has a high magnetic field. Conclusions Considering the potential advantages of the NMR technique, it can be concluded with authority that it has become a preferred choice of technique for any diagnosis, treatment planning, maintenance of treatment and also to see the behavior of foreign materials interaction with the human body.
Financial Support and Sponsorship Nil. Footnotes Conflicts of Interest None declared. References 1. Moseley I. Chichester, New York: John Wiley; Encyclopedia of Nuclear Magnetic Resonance. Diagnostics Basel ; 7 02 :E Role of salivary biomarkers in oral cancer detection.
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J Am Chem Soc. Fast resonance assignment and fold determination of human superoxide dismutase by high-resolution proton-detected solid-state MAS NMR spectroscopy. Angew Chem Int Ed Engl. Nuclear magnetic resonance imaging: current capabilities.
West J Med. Review on fluoride, with special emphasis on calcium fluoride mechanisms in caries prevention Eur J Oral Sci 05 Pt — In vivo monitoring of changes in 5-fluorouracil metabolism induced by metho-trexate measured by 19F NMR spectroscopy. Magn Reson Med. A review] Schweiz Monatsschr Zahnmed. Precise and accurate quantitative 13 C NMR with reduced experimental time. Magnetic resonance imaging versus computed tomography in the evaluation of soft tissue tumors of the extremities.
Ann Surg. Hammer B E. Industrial applications of nuclear magnetic resonance. Sens Rev. Duer Cambridge M J. Cambridge, UK: Wiley-Blackwell; Pickard C J, Mauri F.
All-electron magnetic response with pseudopotentials: NMR chemical shifts. Application of nuclear magnetic resonance spectroscopy to bone diagenesis. J Archaeol Sci. Field focusing nuclear magnetic resonance FONAR : visualization of a tumor in a live animal Science — Warren K E. NMR spectroscopy and pediatric brain tumors. Multimodality correlative study of canine brain tumors.
Proton magnetic resonance spectroscopy, positron emission tomography, and histology. Invest Radiol. Proton nuclear magnetic resonance spectroscopy of primary cells derived from nervous tissue. J Neurochem. Budinger T F. Image analysis in critical care medicine. Crit Care Med. The energy transfer takes place at a wavelength that corresponds to radio frequencies and when the spin returns to its base level, energy is emitted at the same frequency.
The signal that matches this transfer is measured in many ways and processed in order to yield an NMR spectrum for the nucleus concerned. Many nuclei such as deuterium 2 H or hydrogen-2 have a higher spin and are therefore quadrupolar and although they yield NMR spectra, their energy diagram and some of their properties are different.
The precise resonant frequency of the energy transition is dependent on the effective magnetic field at the nucleus. This field is affected by electron shielding which is in turn dependent on the chemical environment. As a result, information about the nucleus' chemical environment can be derived from its resonant frequency. In general, the more electronegative the nucleus is, the higher the resonant frequency. Other factors such as ring currents anisotropy and bond strain affect the frequency shift.
It is customary to adopt tetramethylsilane TMS as the proton reference frequency. This is because the precise resonant frequency shift of each nucleus depends on the magnetic field used.
The frequency is not easy to remember for example, the frequency of benzene might be In the case of the 1 H NMR spectrum of ethyl benzene fig. The aromatic phenyl group is the most electron donating electropositive so has the highest chemical shift. The methylene CH 2 falls somewhere in the middle. However, if the chemical shift of the aromatics were due to electropositivity alone, then they would resonate between four and five ppm.
The values of diffusion coeffs. Fitting the diffusion coeffs. Therefore, DOSY is proposed as a versatile tool for achieving a simple estn. An advantage of the method is that the same sample used for the NMR characterization can be used for the mol. Other water sol.
Diffusion-separated nuclear magnetic resonance spectroscopy of polymer mixtures Macromolecules , 31 , — DOI: Diffusion coeff. After Fourier transformation in the acquisition dimension and an inverse Laplace transform ILT with respect to the square of the gradient strength, 2D spectra are obtained that show the chem. Since polymers may have broad, nonsym. However, the calcn. DOSY spectra recorded from industrial polypropylene and polystyrene samples and mixts.
Fluorescence correlation spectroscopy in polymer science RSC Adv. Diffusion and conformation of peptide-functionalized polyphenylene dendrimers studied by fluorescence correlation and C NMR spectroscopy Biomacromolecules , 8 , — DOI: Coherent Scattering by one Reptating Chain J.
The time-dependent neutron scattering correlation functions Sq t for one deuterated polymer chain, moving inside an entangled melt of chem. The region of interest corresponds to wave-vectors q such that D-1 » q » R where D is the tube diam. In this regime the results disagree strongly with the author's earlier prediction The function Sq t breaks up into two parts. The other part [Sqc t ], with much larger amplitude, describes a slow, global creep of the chain inside its tube, assocd.
The characteristic time for this creep process is independent of q, and is the overall reptation time Trep. Polymers and Neutron Scattering ; Clarendon Press : Organic solar cells: An overview J. Materials Research Society. A review of the current status of org.
Different prodn. This was achieved by the introduction of new materials, improved material engineering, and more sophisticated device structures. Though efficiencies of these thin-film org. The 2 competitive prodn. The field of org. Long-scale evolution of thin liquid films Rev. American Physical Society.
Macroscopic thin liq. They can be composed of common liqs. When the films are subjected to the action of various mech. Such films can display rupture phenomena creating holes, spreading of fronts, and the development of fingers.
In this review a unified math. As a result of this long-wave theory, a math. The basics of the long-wave theory are explained.
If, in addn. A general nonlinear evolution equation or equations are then derived and various particular cases are considered. Each case contains a discussion of the linear stability properties of the base-state solns. The cases reducing to a single highly nonlinear evolution equation are first examd. These include: a films with const.
The dynamics of the films with a spatial dependence of the base-state soln. These include the examples of nonuniform temp. Problems which reduce to a set of nonlinear evolution equations are considered next. Those include a the dynamics of free liq. The spreading of drops on a solid surface and moving contact lines, including effects of heat and mass transport and van der Waals attractions, are then addressed.
Several related topics such as falling films and sheets and Hele-Shaw flows are also briefly discussed. The results discussed give motivation for the development of careful expts. Many refs. Effects of confinement on material behaviour at the nanometre size scale J. Institute of Physics Publishing. In this article, the effects of size and confinement at the nanometer size scale on both the melting temp.
Although there is an accepted thermodn. However, the main thrust of the work is a review of the field of confinement and size effects on the glass transition temp. We present in detail the dynamic, thermodn. We survey the observations that show that the glass transition temp. Indeed, different behaviors have been obsd. It seems that the existing theories of Tg are unable to explain the range of behaviors seen at the nanometer size scale, in part because the glass transition phenomenon itself is not fully understood.
Importantly, here we conclude that the vast majority of the expts. What is currently lacking appears to be an overall view, which accounts for the range of observations. The field seems to be exptl.
Driven polymer translocation through a narrow pore Biophys. Biophysical Society. Motivated by expts. We show that there is a range of polymer lengths in which the system is approx. From this description, general features of the distribution of times for the polymer to pass through the pore may be deduced.
We also introduce a more microscopic model. This model provides a phys. Finally, we point out that the exptl. We study changes in the dynamics of polymer chains confined to cylindrical nanochannels within aluminum oxide membranes.
Specifically, a proton time-domain NMR technique is used to assess the effect of transient wall contacts on the time-averaged orientational order of poly butadiene segments in melts with different mol. In the relevant temp. We show that the pore walls exert a significant orientation effect on the chains, measured in terms of a time-averaged order parameter with a related length scale of one to a few nanometers, coexisting for high mol.
MW inhomogeneously with bulk-like behavior in the pore center. Low MW with fewer than about 10 entanglements as well as low MW liqs. We support our findings by a simulation model based upon one-dimensional curvilinear chain diffusion along the primitive path.
The study is complemented by deuterium NMR expts. In poly propylene , the populations of the conformations are related to specific configurations detd. Above the glass transition temp. The non-exponentiality of the correlation functions and the motional rates are similar of those of the diffuse reorientations obsd.
Although trans and gauche define the preferred conformations within the distribution of rotational angles for poly propylene , the dynamics are not suitably described by motions of the atoms on a diamond lattice. This is demonstrated in particular by the absence of long term orientational memory in 3D exchange NMR expts. A behavior intermediate between large-angle jumps and isotropic rotational diffusion is obsd.
Length scale of dynamic heterogeneities at the glass transition determined by multidimensional nuclear magnetic resonance Phys.
Tracht, U. We directly measure the equil. The spatial information is gained from a proton spin diffusion expt. Heterogeneity at the glass transition: a review J. Solids , , 81 — DOI: The main purpose is to provide an introduction to theor.
Realizing that there is no consensus in regard to the various scenarios of the glass transition starting form rather different assumptions we try to give a balanced overview, although we also compare and interrelate some of the approaches. Spatially heterogeneous dynamics in supercooled liquids Annu. Annual Reviews Inc.
Although it has long been recognized that dynamics in supercooled liqs. As a liq. In this review, the exptl. In particular, the following questions are addressed: How large are the heterogeneities.
How long do they last. How much do dynamics vary between the fastest and slowest regions. Why do these heterogeneities arise.
The answers to these questions influence practical applications of glass-forming materials, including polymers, metallic glasses, and pharmaceuticals. The initial steps toward optical detection and spectroscopy of single mols. Spectral signatures relating to the fluctuations of the no.
In the early 90s, many fascinating phys. In the room temp. Because each single fluorophore acts a light source roughly 1 nm in size, microscopic observation and localization of individual fluorophores is a key ingredient to imaging beyond the optical diffraction limit. Combining this with active control of the no. The background leading up to these observations is described and current developments are summarized.
Flier, Bente M. Such high temps. This enables temp. To ensure that polymer chains were relaxed, a mol. We found significant heterogeneities in the motion of single PDI probe mols. An anal. Up to the glass transition temp. In the range between 0 and 40 K above Tg,bulk the fraction of mobile probe mols. In nm thin films mobility is obsd. The fractions of mobile probe mols. Results of these simulations indicate that the obsd. Heterogeneity in polymer melts from melting of polymer crystals Nat.
Rastogi, Sanjay; Lippits, Dirk R. The resulting topol. By controlled synthesis the no. Ultimately, crystals composed of single chains are feasible, where the chains are fully sepd.
If such sepn. Here we show that through slow and carefully controlled melting such polymer crystals form a heterogeneous melt with more entangled regions, where the chains are mixed, and less entangled ones, composed of individually sepd. Chain reptation, required for the homogenization of the entanglement distribution, is found to be considerably hindered. The long-lived heterogeneous melt shows decreased melt viscosity and provides enhanced drawability on crystn.
This novel route to create heterogeneous melt should be applicable to polymers in general. Liu, Kangsheng; de Boer, Ele L. In past studies have been performed to follow chain dynamics in an equil. Here we show that in linear Ultra-High Mol. The high temp. On increasing the annealing time in melt, the enthalpy of the lower melting temp. However, independent of the equil. A com. To ascertain that entanglements are the cause for the obsd.
This observation strengthens the concept that in the presence of a suitable filler, chain dynamics is arrested to an extent that the nonequil. Glass transition in thin supported polystyrene films probed by temperature-modulated ellipsometry in vacuum Phys. E , 86 , DOI: Efremov, Mikhail Yu. Glass transition in thin nm thick spin-cast polystyrene films on silicon surfaces is probed by ellipsometry in a controlled vacuum environment.
A temp. A clear glass transition is detected in films with thicknesses as low as nm. The glass transition temp. Tg shows no substantial dependence on thickness for coatings greater than 20 nm. Thinner films demonstrate moderate Tg depression achieving 18 K for thicknesses nm. Less than 4 nm thick samples are excluded from the Tg comparison due to significant thickness nonuniformity surface roughness.
The transition in nm thick films demonstrates excessive broadening. For some samples, the broadened transition is clearly resolved into two sep. The thickness dependence of the glass transition can be well described by a simple 2-layer model. It is also shown that Tg depression in 5 nm thick films is not sensitive to a wide range of exptl. The past 20 years have seen a substantial effort to understand dynamics and the glass transition in thin polymer films. In this perspective, we consider developments in this field and offer a consistent interpretation of some major findings.
We discuss recent expts. Enhanced mobility near the free surface allows a qual. Tg in thin films. For thin films, knowledge of Tg by itself is less useful than for bulk materials. Because of this, new exptl.
Polymer brushes on flat and curved surfaces: How computer simulations can help to test theories and to interpret experiments J. Blob concepts and resulting scaling relations are outlined, and various versions of the SCF theory are summarized: the classical approxn. The phys. Also, alternative theories, such as the single chain mean field theory and the d.
Both mol. Also extensions such as brush-brush interactions or nanoparticles inside of brushes as well as the soly. Pertinent exptl. Glass transition of poly ethylmethacrylate admixed and bound to nanoparticles J. Reptation of Stars J. Adams, C. Each arm of the polybutadiene stars has a monodisperse mol.
Although the FIDs from the core and near the free end are always distinctly different, the FIDs from the other sections are only clearly distinguishable above ca. This is interpreted in terms of the mol. The deuterium FIDs have been analyzed according to an exact soln. A review is given of the academic and industrial aspects of the prepn. These materials are attracting considerable interest in polymer science research. Hectorite and montmorillonite are among the most commonly used smectite-type layered silicates for the prepn.
Smectites are a valuable mineral class for industrial applications because of their high cation exchange capacities, surface area, surface reactivity, adsorptive properties, and, in the case of hectorite, high viscosity and transparency in soln.
In their pristine form they are hydrophilic in nature, and this property makes them very difficult to disperse into a polymer matrix. The most common way to remove this difficulty is to replace interlayer cations with quaternized ammonium or phosphonium cations, preferably with long alkyl chains. A wide range of polymer matrixes is covered in this review, with special emphasis on biodegradable polymers. This new family of composite materials frequently exhibits remarkable improvements of material properties when compared with the matrix polymers alone or conventional micro- and macro-composite materials.
Improvements can include a high storage modulus, both in solid and melt states, increased tensile and flexural properties, a decrease in gas permeability and flammability, increased heat distortion temp. Effect of filler particle size on the properties of model nanocomposites Macromolecules , 41 , — DOI: Results are presented concerning the effect of the increasing particle size on the thickness of the interphase, i.
The behavior of the mass d. The effect of temp. Long simulations have been carried out to det. It is established that, within errors, the interphase thickness is independent of the size of the nanoparticle for the range of particle sizes analyzed.
This information is particularly important for the second stage of the project where it is used in continuum micromech. The confrontation between continuum and atomistic approaches will be the subject of a future publication. Hybrid sol-gel-derived polymers: Applications of multifunctional materials Chem. Multinuclear solid-state-NMR studies of hybrid organic-inorganic materials Adv. Fischer, E. Makromolekulare Chemie, Supplement , 12 Polym.
Specific Prop. Two effects are of outstanding importance for the mech. A model to explain the effect in terms of the free vol. Sub-Tg dynamics in polycarbonate by neutron scattering and its relation with secondary gamma relaxation J.
Geometry of phenylene motion in polycarbonate from NMR spectroscopy and neutron scattering J. Schmidt-Rohr, K. The mol. The identity of the motions obsd. The selective-excitation "3D" NMR spectrum proves that, for every mobile side group, a relatively well-defined motion between two potential-energy min. Consistently, anal. This is ascribed to the fact that the asym. These findings explain both the dielec. Polymer ultradrawability: the crucial role of alpha-relaxation chain mobility in the crystallites Acta Polym.
After reviewing refs. An explanation of the varying ultra drawability of semicryst. The chain motions provide a mechanism by which hot drawing of these polymers can extend an initially formed fiber morphol.
A second class of polymers, including nylons, poly ethylene terephthalate , syndiotactic polypropylene, isotactic polystyrene, and isotactic poly 1-butene form I lack a cryst. On this basis, the authors can explain which polymers are drawable to high draw ratios, given a sufficiently low level of entanglement. The motion through the crystallites is thermally activated and the applied stress only biases the direction of the jumps; this explains the crucial role of temp.
The behavior of the crystal-fixed, poorly drawable polymers strongly suggests that melting, straight chain pull-out, and sliding on crystal planes are not significantly operative during ultradrawing, and that weak intermol.
Various stages of drawing are distinguished and other models of ultradrawability are discussed critically. Morphological differences in semicrystalline polymers: Implications for local dynamics and chain diffusion Phys. E , 76 , DOI: The local dynamics in the noncryst. The activation enthalpy for chain diffusion, however, is the same, indicating that entropic differences in the noncryst.
Restricted segmental mobility can facilitate medium-range chain diffusion: A NMR study of morphological influence on chain dynamics of polyethylene Macromolecules , 41 , — DOI: The influence of the morphol. The geometrical restrictions of the conformational transitions are probed via anisotropic NMR interactions, i. As they are averaged out under MAS, recoupling techniques are applied to yield sideband patterns or quasi-static NMR spectra, from which residual anisotropies are detd.
Chain diffusion is probed by 13C exchange NMR. As expected, the local conformational transitions are more restricted in the soln. Moreover, the motional narrowing obsd. This facilitates the chain diffusion between the cryst. The implications of these results for the understanding of crystal thickening and cold drawing are discussed. Analysis of the temperature dependence of the dielectric alpha-relaxation in the model of a paraffin-ketone mixed crystal Prog. Colloid Polym. To det.
There was a close correspondence between the temp. The increase of the relaxation frequency with temp. Potential energy calcns. Understanding the structure formation of an ordered domain in the early stage of crystn. In this study, we investigate the chain trajectory of isotactic polypropylene iPP formed via rapid and deep quenching, using solid-state NMR spectroscopy. Comparisons of exptl.
Therefore, long flexible polymer chains naturally fold in the early stage of crystn. Over the last half century, a chain-folding structure of semicryst. Recently, 13CC double quantum DQ NMR spectroscopy combined with 13C selective isotope labeling has been developed to investigate re-entrance sites of the folded chains, mean values of adjacent re-entry no.
This viewpoint highlights the versatile approaches of using solid-state ss NMR and isotope labeling for revealing i chain trajectory in melt- and soln. Polymers with complex architecture by living anionic polymerization Chem. A review on synthetic methods for prepn.
General methods for the synthesis of star polymers, multifunctional initiators and linking agents, difunctional monomers, and synthesis of star-block copolymers are discussed. Functionalized stars, initiators, terminating agents, asym. Miktoarm star polymer synthesis, including chlorosilane method, divinylbenzene method, diphenylethylene deriv. Comb-shaped polymer prepn. Dynamics of block copolymers: Theory and experiment Annu. Annual Reviews. A review, with refs. Topics covered include collective- and self-diffusion, linear viscoelastic properties, and nonlinear rheol.
Self-concentrations and effective glass transition temperatures in polymer blends Macromolecules , 33 , — DOI: In a miscible polymer blend the local environment of a monomer of type A will, on av. As a result, the local dynamics of the 2 chains may exhibit different dependences on temp.
By assigning a length scale or vol. For example, the Kuhn length of the chain, lK, is assocd. An effective local compn. As lower Tg polymers are generally more flexible, the assocd. An effective glass transition temp. This anal. Furthermore, this approach can reconcile other features of miscible blend dynamics, including the asym. Polyolefin miscibility: Solid-state NMR investigation of phase behavior in saturated hydrocarbon blends Macromolecules , 36 , — DOI: Nieuwendaal, Ryan C.
Joseph; Toney, Michael F. It is shown that variations in common P3HT-PCBM BHJ processing parameters such as spin-coating speed and thermal annealing can significantly affect domain size distributions, which in turn affect power conversion efficiency. The 1H spin diffusion NMR results show that a significant population of domains tens of nanometers in size is a common characteristic of samples with higher efficiencies.
High-efficiency solution processable polymer photovoltaic cells by self-organization of polymer blends Nat. Converting solar energy into electricity provides a much-needed soln. Polymer solar cells showed potential to harness solar energy in a cost-effective way.
Significant efforts are underway to improve their efficiency to the level of practical applications. Here, the authors report highly efficient polymer solar cells based on a bulk heterojunction of polymer poly 3-hexylthiophene and methanofullerene. Controlling the active layer growth rate results in an increased hole mobility and balanced charge transport.
Together with increased absorption in the active layer, this results in much-improved device performance, particularly in external quantum efficiency. The power-conversion efficiency of 4. The soln. The high efficiency achieved in this work brings these devices one step closer to commercialization. Solid-state NMR techniques are used to study the microphase structure of polystyrene-Me Ph siloxane diblock copolymers with different compns.
The proton NMR spectra display motionally narrowed lines of the siloxane component at ambient temps. The mobility of the segments in the copolymers is different, however, from that in the homopolymer. This can be related to the shift of the glass transition temp. Tg for the siloxane-rich phase, not detected by DSC.
By measuring the proton spin diffusion with 13C detection, combining a dipolar filter with line-narrowing techniques, the microdomain dimensions are evaluated quant. The results are compared with the phase sepn. In addn. NMR spectroscopy. Clough, Andrew; Sigle, Jessica L. Gradient copolymers can exhibit phys. Property variations should depend upon differences in the mol. Here we describe exptl. In total, the expts. We show that the synthesis conditions can be changed to vary the partitioning of each gradient copolymer component in a systematic way and propose that the interphase between the hard and soft domains is responsible for differential partitioning.
Advanced solid-state NMR techniques exploiting 1H spin diffusion are described, which rely on selecting 1H magnetization of one of the components from 1H chem. To monitor the progression of 1H spin diffusion, the higher resoln.
For evaluation of the data, full quasi-anal. To obtain quant. To this end, the domain sizes in polystyrene I -poly Me methacrylate systems including sym. Calibration of H-1 NMR spin diffusion coefficients for mobile polymers through transverse relaxation measurements Macromolecules , 32 , — DOI: Independent calibration of H-1 spin-diffusion coefficients in amorphous polymers by intramolecular polarization transfer Macromolecules , 36 , — DOI: Structural studies of nanophase-separated poly 2-hydroxyethyl methacrylate -l-polyisobutylene amphiphilic conetworks by solid-state NMR and small-angle x-ray scattering Macromolecules , 36 , — DOI: Characterization of interfaces in core-shell polymers by advanced solid-state NMR methods Macromolecules , 29 , — DOI: Gradient copolymers Colloid Polym.
Gradient copolymers represent a relative new class of copolymers contg. Due to their structural relation to block copolymers, microphase-segregated structures can be formed in bulk, in soln. The article reviews the prepn. Systematic variation of comonomer concn. Controlled self-assembly of gradient copolymers into desired morphologies is theor. Building on previous work where improved methods were used to elucidate heterogeneous comonomer partitioning in styrene-butadiene gradient copolymers [Clough Macromols.
Importantly, the chem. The resulting tapered and inverse tapered block copolymers contain nanometer length scale interfaces that differ from one another and differ dramatically from that obsd. Evidence is presented that butadiene can reside in rigid environments, styrene can reside in mobile environments, and their relative amts. The connection between the mol. Structure, mobility, and interface characterization of self-organized organic-inorganic hybrid materials by solid-state NMR J.
Fuzzy nanoassemblies: Toward layered polymeric multicomposites Science , , — DOI: Science Washington, D. Multilayer films of org. However, both the Langmuir-Blodgett technique and chemisorption from soln. An alternative approach fabrication of multilayers by consecutive adsorption of polyanions and polycations is far more general and has been extended to other materials such as proteins or colloids. Because polymers are typically flexible mols.
What is really driving cell-surface interactions? Layer-by-layer assembled films may help to answer questions concerning cell attachment and response to biomaterials Biointerphases , 11 , DOI: Layer-by-layer assembled films may help to answer questions concerning cell attachment and response to biomaterials. Sergeeva, Yulia N. American Institute of Physics. Layer-by-layer LbL assembled multicomponent films offer the opportunity to control and to fine-tune cell attachment and behavior on solid surfaces [Layer-by-Layer Films for Biomedical Applications, edited by Picart et al.
Wiley, Weinheim, and El-Khouri et al. At the same time, these films allow for quite detailed physicochem. In this report, the authors investigate cell adhesion and cytocompatibility of compositionally and morphol. Human adult dermal fibroblasts were chosen as a model because of the need for chem. The growth and the stability of the multilayer films in the incubation media were studied dissipation- enhanced quartz crystal micobalance QCM-D and ellipsometry.
The QCM-D signals obsd. The authors used contact angle measurements with water to study the contribution of the chem.
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