Pierrick Berruyer

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Raw data and Matlab scripts from the publication at https://doi.org/10.1021/jacs.3c01279 All codes are provided free of charge and come with no warranty. Future use (original or modified) is required to cite: Zenedo data deposit at DOI 10.5281/zenodo.7756308 Berruyer P., Cibaka-Ndaya C. , Pinon A., Sanchez C., Drisko G. L., and Emsley L.. Imaging radial distribution functions of complex particles by relayed dynamic nuclear polarization. J. Am. Chem. Soc. 2023. https://doi.org/10.1021/jacs.3c01279 The data are organized in two separated folders, each corresponding to two different samples (A and B) analyzed in the aforementioned manuscript. Below “i” denoted for “SampleA” or “SampleB”, depending on the considered samples. i_0_raw_nmr_data.zip is a ZIP folder that contains all the raw NMR data in topspin format for sample i. These data are transferred into Matlab using the script i_1_extract_nmr_data_from_topspin.m. The latter Matlab script eventually saved the NMR data within a Matlab MAT-file i_2_extracted_nmr_data.mat. The Matlab script i_3_RDNP_imaging.m used the extracted NMR data saved within the i_2_extracted_nmr_data.mat file. Note that this script uses parallel computing capabilities of Matlab and it is recommended to run it with a high performance computing (HPC) facilities. It performs the data fitting to obtain the final internal composition of the studied particles. Once the program converged, the data are automatically saved as a Matlab MAT-file under the name i_4_composition_fitted.mat. Finally, the internal structure is plotted using the Matlab script i_5_plot_from_fit.m.

EPFL Infoscience2023

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The physical properties of many modern multi-component materials are determined by their internal microstructure. Tools capable of characterizing complex nanoscale architectures in composite materials are, therefore, essential to design materials with targeted properties. Depending on the morphology and the composition, structures may be measured by laser diffraction, scattering methods, or by electron microscopy. However, it can be difficult to obtain contrast in materials where all the components are organic, which is typically the case for formulated pharmaceuticals, or multi-domain polymers. In nuclear magnetic resonance (NMR) spectroscopy, chemical shifts allow a clear distinction between organic components and can in principle provide the required chemical contrast. Here, we introduce a method to obtain radial images of the internal structure of multi-component particles from NMR measurements of the relay of nuclear hyperpolarization obtained from dynamic nuclear polarization. The method is demonstrated on two samples of hybrid core–shell particles composed of a core of polystyrene with a shell of mesostructured silica filled with the templating agent CTAB and is shown to yield accurate images of the core–shell structures with a nanometer resolution.

2023

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Recently, it has been shown that methods based on the dynamics of 1 H nuclear hyperpolarization in magic angle spinning (MAS) NMR experiments can be used to determine mesoscale structures in complex materials. However, these methods suffer from low sensitivity, especially since they have so far only been feasible with indirect detection of 1 H polarization through dilute heteronuclei such as 13C or 29Si. Here we combine relayed-DNP (R-DNP) with fast MAS using 0.7 mm diameter rotors at 21.2 T. Fast MAS enables direct 1 H detection to follow hyperpolarization dynamics, leading to an acceleration in experiment times by a factor 16. Furthermore, we show that by varying the MAS rate, and consequently modulating the 1 H spin diffusion rate, we can record a series of independent R-DNP curves that can be analyzed jointly to provide an accurate determination of domain sizes. This is confirmed here with measurements on microcrystalline L-histidinemiddotHClmiddotH2O at MAS frequencies up to 60 kHz, where we determine a Weibull distribution of particle sizes centered on a radius of 440 +/- 20 nm with an order parameter of k = 2.2.

AMER CHEMICAL SOC2022