A two-axis goniometer for low-temperature nuclear magnetic resonance measurements on single crystals

Shiroka, T.; Casola, Francesco; Mesot, J.; Bachmann, Walter; Ott, H. R.

doi:10.1063/1.4748861

Cited by 10 publications

(13 citation statements)

References 22 publications

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“…Further advances in SC NMR probe technology was done by Shiroka et al [13] to enable SC NMR experiments at cryogenic temperatures. Their design, shown in Fig.…”

Section: Dedicated Single-crystal Nmr Probesmentioning

confidence: 99%

“…19 for further details. Using this goniometer design, it was possible to unambiguously assign the 12 13 C-chemical shift tensors in sucrose [19,20].…”

Section: Angle-flipping Correlationsmentioning

confidence: 99%

“…18c-18d. The different phases of the spinning sidebands for different rotor pitch angles reflect the sensitivity of the method towards the actual orientation of the 13 C chemical shift tensor relative to the MAS rotor.…”

Section: Reducing the Number Of Rotation Axesmentioning

confidence: 99%

“…Just like a large number of liquid-state NMR studies have established empirical knowledge on 1 H and 13 C isotropic chemical shifts of different functional groups, a number of 13 C SC NMR studies performed decades ago have provided valuable insight into the magnitudes and common orienta- Adapted from [9] with permission.…”

Section: Carbon-13 Chemical Shift Tensorsmentioning

confidence: 99%

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Single-Crystal NMR Spectroscopy

Vosegaard¹

2021

Preprint

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Single-crystal (SC) NMR spectroscopy is a solid-state NMR method that has been used since the early days of NMR to study the magnitude and orientation of tensorial nuclear spin interactions in solids. This review first presents the field of SC NMR instrumentation, then provides a survey of software for analysis of SC NMR data, and finally it highlights selected applications of SC NMR in various fields of research. The aim of the last part is not to provide a complete review of all SC NMR literature but to provide examples that demonstrate interesting applications of SC NMR.

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“…Further advances in SC NMR probe technology was done by Shiroka et al [13] to enable SC NMR experiments at cryogenic temperatures. Their design, shown in Fig.…”

Section: Dedicated Single-crystal Nmr Probesmentioning

confidence: 99%

“…19 for further details. Using this goniometer design, it was possible to unambiguously assign the 12 13 C-chemical shift tensors in sucrose [19,20].…”

Section: Angle-flipping Correlationsmentioning

confidence: 99%

Section: Reducing the Number Of Rotation Axesmentioning

confidence: 99%

Section: Carbon-13 Chemical Shift Tensorsmentioning

confidence: 99%

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Single-Crystal NMR Spectroscopy

Vosegaard¹

2021

Preprint

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“…Thus, Wulp et al 1 and Pietzsch et al 6 employed a non-magnetic spring clamping mechanism, but their designs only provide one rotational axis. Two axes non-piezo driven goniometers have also been reported in low temperature physics experimental setups, 8,9 which are driven by worm screws/gears together with drive shafts. However, these designs are mechanically less stable compared to the piezo stages with leaf spring clamping mechanisms, for which picometer stability has been demonstrated.…”

Section: Introductionmentioning

confidence: 98%

Miniaturized high-precision piezo driven two axes stepper goniometer

Zhong

Schwarz

Wiesendanger

2014

Review of Scientific Instruments

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A miniaturized inertial stepper goniometer with two orthogonal axes (θ and φ axes) has been realized using four shear piezo based actuators arranged in a tetrahedral configuration tangent with a polished sapphire spherical rotor. The measured sensitivity is about 11.5 microdegree (μ°) per Volt. The smallest angular step size, achieved with a minimal peak-to-peak voltage Upp of 200 V is about 0.6 millidegree (m°). The crosstalk between both axes is below 10%. Our specific design is used to accurately position a glass fiber, but the concept can be utilized for many different applications as well.

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Solid‐State Nuclear Magnetic Resonance

Gerald

2017

Encyclopedia of Analytical Chemistry

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The first experimental verification of nuclear magnetic resonance (NMR) in the solid state was carried out by Edward M. Purcell, Henry C. Torrey, and Robert V. Pound in 1945. Since then, new developments have transformed this form of spectroscopy from an interesting physical curiosity at its inception to one of the most widely used analytical tools for physical, chemical, biological, and materials research and applications. The capabilities of NMR include the following: identification of molecules in all phases of matter by their atomic connectivities; probing the temperature‐dependent conformation of molecules from cyclohexane to complex 50 kDa proteins; molecular dynamics investigations from the picosecond timescale for rotation of small molecules to the second timescale for atoms diffusing throughout the three‐dimensional nanoscopic channels of zeolites; elucidation of chemical reaction mechanisms; the determination of organization, reorientation, and diffusion of molecular solids; the identification of phase changes and morphology of solids; the measurement of bond lengths and interatomic distances between nonbonded atoms; the assessment of pore size in nanoporous solids as well as the identification of adsorbates and their diffusivities; the estimation of physicochemical parameters of molecular systems such as equilibrium and kinetic rate constants, enthalpies and entropies of a reaction, and activation energies; the capability to follow a metabolic pathway taking place inside living cells; the quantification of the alignment of molecules in partially ordered systems; the determination of nanoscale domain sizes in heterogeneous materials; and the noninvasive imaging of all phases and forms of matter under various temperature, pressure, and mechanical conditions.The scope of this article is very selective, covering some of the most widely used techniques and more unusual areas of application of solid‐state NMR. These topics are covered at different levels of detail, and some are just mentioned by reference to published work. This article is not intended to present a comprehensive review of all state‐of‐the‐art NMR techniques; for these, the reader should consult references included in the text. Instead, this article provides an historical background and the fundamental concepts of magnetic resonance that preceded solid‐state NMR, a general overview of the basic principles of NMR with emphasis on the visualization of anisotropic spin interactions, a review of the most widely used methods for investigating solids by NMR, and practical information to provide a modicum of guidance for application of the methods. There are several redundancies in terminology so that different sections can be read independently.The references are an important component of the article and should be consulted for more complete and often original accounts of the theory and techniques for the application of NMR to solids. A modest attempt has been made to include original and important references, but more importantly, many have been included to provide examples of chemical and physical insights obtained in whole or in part by application of NMR techniques to the investigations of the problems. For figures and tables, if no reference or acknowledgment has been provided, the spectrum or photograph in the figure or the table is previously unpublished.The article is directed at a general audience of chemical and physical analytical scientists with an interest in NMR. In addition, NMR spectroscopists may find some interesting details of studies on metals and magnetic materials.

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A two-axis goniometer for low-temperature nuclear magnetic resonance measurements on single crystals

Cited by 10 publications

References 22 publications

Single-Crystal NMR Spectroscopy

Single-Crystal NMR Spectroscopy

Miniaturized high-precision piezo driven two axes stepper goniometer

Solid‐State Nuclear Magnetic Resonance

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