Abstract

The intention of this discussion is as a simple introduction for general—non-nuclear magnetic resonance (NMR)-specialist—materials scientists, to make them aware as to how some of the materials science measurements that they need to make might possibly be addressed by simple physical measurements using low-cost time-domain NMR apparatus. The intention is to include a minimum of complex NMR detail, while enabling general material-scientists to see that simple easily understood time-domain NMR might be of use to them. That is how I have tried to structure this discussion. It seems to me be generally forgotten how much of materials science is actually physics, as opposed to chemistry, and the extent to which simple time-domain NMR may be used to make measurements of the physical properties of materials. There frequently seems to be an assumption that if NMR is mentioned that it is chemical analysis methods that are under discussion, or possibly magnetic resonance imaging (MRI). These are both extremely powerful techniques, but to forget about the physics that often governs the properties of the sample can be a significant mistake. Key material science properties are often described in different fields using the terms mobility/dynamics/stiffness/viscosity/rigidity of the sample. These properties are usually dependent on atomic and molecular motion in the sample. We will discuss a method, time-domain NMR, that appears often to be ignored, to obtain quantitative or comparative information on these properties. The intention of this paper is not to probe the material properties of some interesting system, but to discuss in as clear a manner as possible a particular technique, “low-field time-domain NMR”, to bring this technique and its advantages to the attention of other material scientists. Thus we discuss time-domain NMR and MRI, as methods of measuring the physical properties of liquid and solid materials. Time-domain NMR is also a good technique for measuring pore-size distributions from the nano-meter to microns, using a technique known as NMR cryoporometry (NMRC). Standard MRI protocols may be combined with NMRC, so that spatial resolution of pore dimensions may also be obtained. Low-field time-domain NMR is, at its fundamentals, a very approachable and easily comparative technique, where the material properties may often be extracted from the time-domain data much more simply than from say high-field high-resolution spectral data. In addition, low-field time-domain NMR apparatus is typically a factor of 10 to 100 times cheaper than high-field high-resolution solid-state NMR systems.

Highlights

  • Key NMR concepts1.1 NMR on the benchtop and in the fieldWe will discuss time-domain nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI), as methods of measuring the physical properties of liquid and solid materials

  • When an NMR measurement is made on a sample that has been placed in a strong steady B o magnetic field, a strong radio frequency (RF) pulse may be applied that perturbs the nuclear magnetism from its equilibrium position along the main B o field

  • We have extended the NMR cryoporometry (NMRC) technique for measuring distributions of pore sizes over 3 orders of magnitude in pore dimensions

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Summary

NMR on the benchtop and in the field

We will discuss time-domain nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI), as methods of measuring the physical properties of liquid and solid materials. We consider why analyse the data in the time-domain measurements, as opposed to transforming the captured time-domain data to the frequencydomain and analysing it there. The discussion will be very practical, giving many examples. Two tables of instrumental details on a number of common benchtop NMR spectrometers are given in Sect. 2. The examples have mainly been prepared using a compact example, the lab-tools Mk3 timedomain NMR spectrometer [22, 24], see Fig. 1 and Sect. 27, 28, 29, needed a wide-bore NMR time-domain imaging system. Some of the other benchtop NMR spectrometers have additional features that are useful for specific measurement needs

Time‐domain NMR for material science
Why does time‐domain NMR provide a direct method to determining the physical motion in the sample ?
NMR relaxation times: the mechanisms by which decays take place in NMR and MRI measurements
NMR relaxation (NMRR)
Using NMR to study the properties of structured or porous materials, and materials in these pores
NMR imaging (MRI)
NMR relaxometry
NMR cryoporometry (NMRC)
Example low‐field time‐domain NMR spectrometers
Compact NMR magnets
Using a time‐domain NMR spectrometer to measure mobility/dynamics/stiffness/ viscosity/rigidity
Lab‐tools T‐D NMR spectrometer with peltier cooled variable‐temperature NMR probe
NMR Mk3 cryoporometer
Motion of the molecules in Brittle Ice, studied using NMR T 2 measurements
Using time‐domain NMR to study the properties of polymers
Using time‐domain NMR to study the properties of hydrocarbons in nano‐pores
Program requirements for process control
2.10 NMR used to measure the self‐diffusion constants in liquids
2.12 Using time‐domain NMR spectrometers to make MRI images
NMR cryoprometry for measuring nano‐ to micro‐ pore size distributions
NMRC measurement of poresize distributions in 3 porous rock types
NMR cryoporometric measurements on biochars, with different preparation methods
NMR cryoporometric measurements on five biochars, with different heat treatment temperatures (HTTs)
Combining NMRC and MRI protocols
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