Inversion-recovery Measurements Research Articles

No-wait inversion—a novel model for T1 mapping from inversion recovery measurements without the waiting times

Introduction: Quantification of longitudinal relaxation time T1 gained interest as an important MR-inducible tissue property for tissue characterization. Standard inversion recovery (IR) measurements for T1 determination take a prohibitively long time, and signal models assume a perfect inversion. Acceleration is possible by using the Look–Locker (LL) technique or other accelerated, model-based algorithms. However, the calculation of real T1 values from LL acquisitions necessitates the knowledge of equilibrium magnetization M0. Thus, usually, a waiting time to allow for free relaxation between global inversion pulses must be implemented. This study aims to introduce a novel model-based fitting approach for T1 mapping without the need for such waiting times.Methods: Single-inversion spiral LL spoiled gradient echo acquisitions were performed in a phantom and eight healthy volunteers using a 1.5T magnetic resonance imaging (MRI) scanner. The measurements comprised two parts, one without magnetization preparation and a second featuring a global inversion pulse preparation before each of the 35 slices. Acquisition was performed without any waiting time in between slices, i.e., before the inversion pulses. T1 maps were calculated based on an iterative model-based reconstruction algorithm which combines the information from these two measurements, with and without inversion.Results: Accurate T1 maps were obtained in phantom and volunteer measurements. ROI-based mean T1 values differ by an average of 1.5% in the phantom and 5% in vivo between reference measurements and the proposed method. The combined fit benefits from both the information obtained in the inversion prepared and the unprepared measurements. The former provides a large dynamic range for accurate model-based fitting of the relaxation process, while the latter provides equilibrium magnetization M0, necessary to obtain accurate T1 values from a LL-like acquisition.Conclusion: The proposed model of a combined fit of an inversion-prepared and an unprepared measurement allows for robust fast T1 mapping, even in cases of imperfect inversion due to skipped waiting times for magnetization recovery. Thus, it can render long waiting times in between inversion pulses redundant.

Assessing effects of scanner upgrades for clinical studies.

Scanner upgrades due to software and hardware changes are an inevitable part of MR research and, without quality assurance protocols, can jeopardize studies. To evaluate changes in T1 relaxation time by inversion recovery (IR) and variable flip angle (VFA) measurements on a 3T system that underwent an "everything but the magnet" upgrade. Longitudinal. An International Society of Magnetic Resonance in Medicine / National Institute of Standards and Technology (ISMRM/NIST) system phantom with repeated measurements across multiple (n = 3) days. T1 IR, VFA at 3T. The T1 measurements by IR and VFA were compared with the nuclear magnetic resonance (NMR) measurements, which constitute the known values for the ISMRM/NIST system phantom, to determine the measurement error. Descriptive. The T1 VFA measurement errors were distributed around zero (-15% to +10%) on the original system and then the errors were distributed entirely above zero post-upgrade (+5% to 30%). The T1 IR results had a dramatic increase in error distribution (±5% original, ±20% post-upgrade) prior to the identification of signal saturation as an issue. Once the signal saturation was accounted for, the T1 IR errors decreased to ±10% post-upgrade. The T1 VFA measurement differences between the original and post-upgrade systems can be entirely attributed to contributions from B1 . The T1 IR measurements demonstrate the need for quantitative quality assurance (QA) processes. The site under study passed the QA protocols in place, which did not identify the increased T1 error, nor the signal saturation issue. To improve on this study, we would make systematic, quantitative measurements at intervals less than a year and following any hardware or software upgrade. 1 Technical Efficacy: Stage 2 J. Magn. Reson. Imaging 2019. J. Magn. Reson. Imaging 2019;50:1948-1954.

Morphology effects on spin-dependent transport and recombination in polyfluorene thin films

We have studied the role of spin-dependent processes on conductivity in polyfluorene (PFO) thin films by preforming continuous wave (cw) electrically detected magnetic resonance (EDMR) spectroscopy at temperatures between 10 K and room temperature using microwave frequencies between about 1 GHz and 20 GHz, as well as pulsed EDMR at the $X$ band (10 GHz). Variable frequency EDMR allows us to establish the role of spin-orbit coupling in spin-dependent processes whereas pulsed EDMR allows for the observation of coherent spin motion effects. We used PFO for this study in order to allow for the investigation of the effects of microscopic morphological ordering since this material can adopt two distinct intrachain morphologies: an amorphous (glassy) phase, in which monomer units are twisted with respect to each other, and an ordered (\ensuremath{\beta}) phase, where all monomers lie within one plane. In thin films of organic light-emitting diodes, the appearance of a particular phase can be controlled by deposition parameters and solvent vapor annealing, and is verified by electroluminescence spectroscopy. Under bipolar charge-carrier injection conditions, we conducted multifrequency cw EDMR, electrically detected Rabi spin-beat experiments, and Hahn echo and inversion-recovery measurements. Coherent echo spectroscopy reveals electrically detected electron-spin-echo envelope modulation due to the coupling of the carrier spins to nearby nuclear spins. Our results demonstrate that, while conformational disorder can influence the observed EDMR signals, including the sign of the current changes on resonance as well as the magnitudes of local hyperfine fields and charge-carrier spin-orbit interactions, it does not qualitatively affect the nature of spin-dependent transitions in this material. In both morphologies, we observe the presence of at least two different spin-dependent recombination processes. At room temperature and 10 K, polaron-pair recombination through weakly spin-spin coupled intermediate charge-carrier pair states is dominant, while at low temperatures, additional signatures of spin-dependent charge transport through the interaction of polarons with triplet excitons are seen in the half-field resonance of a triplet spin-1 species. This additional contribution arises since triplet lifetimes are increased at lower temperatures. We tentatively conclude that spectral broadening induced by hyperfine coupling is slightly weaker in the more ordered \ensuremath{\beta}-phase than in the glassy phase since protons are more evenly spaced, whereas broadening effects due to spin-orbit coupling, which impacts the distribution of $g$-factors, appear to be somewhat more significant in the \ensuremath{\beta}-phase.

Discrimination of Surface and Bulk Structure of Crystalline Hydroxyapatite Nanoparticles by NMR

Solid state 1H and 31P NMR spectroscopy was used to characterize well-crystallized hydroxyapatite samples of different stoichiometry prepared by a precipitation route. The aim of the paper was to investigate the bulk structural features of samples with different stoichiometry and to discriminate signals related to the surface from those related to the bulk. Thanks to the implementation of (i) in situ thermal pretreatment at 623 K, (ii) filling of the NMR rotor in a controlled atmosphere, (iii) relative proton enrichment of the surface performed under controlled isotopic H-D exchanges, and (iv) specific NMR sequences including inversion recovery measurements, two-dimensional HETCOR and DQSQ spectra, new resolved NMR signals originating from the surface and from the bulk were identified alongside already reported signals associated with adsorbed water, structural phosphates, and OH groups. In particular, considering the influence of the stoichiometry, it was possible to identify a specific signature associa...

(31)P-MRS of healthy human brain: ATP synthesis, metabolite concentrations, pH, and T1 relaxation times.

The conventional method for measuring brain ATP synthesis is (31)P saturation transfer (ST), a technique typically dependent on prolonged pre-saturation with γ-ATP. In this study, ATP synthesis rate in resting human brain is evaluated using EBIT (exchange kinetics by band inversion transfer), a technique based on slow recovery of γ-ATP magnetization in the absence of B1 field following co-inversion of PCr and ATP resonances with a short adiabatic pulse. The unidirectional rate constant for the Pi → γ-ATP reaction is 0.21 ± 0.04 s(-1) and the ATP synthesis rate is 9.9 ± 2.1 mmol min(-1) kg(-1) in human brain (n = 12 subjects), consistent with the results by ST. Therefore, EBIT could be a useful alternative to ST in studying brain energy metabolism in normal physiology and under pathological conditions. In addition to ATP synthesis, all detectable (31)P signals are analyzed to determine the brain concentration of phosphorus metabolites, including UDPG at around 10 ppm, a previously reported resonance in liver tissues and now confirmed in human brain. Inversion recovery measurements indicate that UDPG, like its diphosphate analogue NAD, has apparent T1 shorter than that of monophosphates (Pi, PMEs, and PDEs) but longer than that of triphosphate ATP, highlighting the significance of the (31)P-(31)P dipolar mechanism in T1 relaxation of polyphosphates. Another interesting finding is the observation of approximately 40% shorter T1 for intracellular Pi relative to extracellular Pi, attributed to the modulation by the intracellular phosphoryl exchange reaction Pi ↔ γ-ATP. The sufficiently separated intra- and extracellular Pi signals also permit the distinction of pH between intra- and extracellular environments (pH 7.0 versus pH 7.4). In summary, quantitative (31)P MRS in combination with ATP synthesis, pH, and T1 relaxation measurements may offer a promising tool to detect biochemical alterations at early stages of brain dysfunctions and diseases.

Chemical Shielding Anisotropies for Chloroform Exchanging between a Free Site and a Complex with Cryptophane-D: A Cross-Correlated NMR Relaxation Study.

The case of (13)C-labeled chloroform exchanging between a free site in solution and the encaged site within the cryptophane-D cavity is investigated using the measurements of longitudinal cross-correlated relaxation rates, involving the interference of the dipole-dipole and chemical shielding anisotropy interactions. A compact theoretical expression is provided, along with an experimental protocol, based on INEPT (insensitive nuclei enhanced by polarization)-enhanced double-quantum-filtered inversion recovery measurements. The analysis of the build-up curves results in a set of cross-correlated relaxation rates for both the (13)C and (1)H spins at the two sites. It is demonstrated that the results can be given a consistent interpretation in terms of molecular-level properties, such as rotational correlation times, the Lipari-Szabo order parameter, and interaction strength constants. The analysis yields the bound-site carbon-13 chemical shielding anisotropy, ΔσC = -58 ± 8 ppm, in good agreement with most recent liquid-crystal measurements and the corresponding proton shielding anisotropy, ΔσH = 14 ± 2 ppm.

Quantitative theory for the longitudinal relaxation time of blood water.

To propose and evaluate a model for the blood water T1 that takes into account the effects of hematocrit fraction, oxygenation fraction, erythrocyte hemoglobin concentration, methemoglobin fraction, and plasma albumin concentration. Whole blood and lysed blood T1 data were acquired at magnetic fields of 3 Tesla (T), 7T, 9.4T, and 11.7T using inversion-recovery measurements and a home-built blood circulation system for maintaining physiological conditions. A quantitative model was derived based on multivariable fitting of this data. Fitting of the model to the data allowed determination of the different parameters describing the blood water T1 such as those for the diamagnetic and paramagnetic effects of albumin and hemoglobin, and the contribution of methemoglobin. The model correctly predicts blood T1 at multiple fields, as verified by comparison with existing literature. The model provides physical and physiological parameters describing the effects of hematocrit fraction, oxygenation, hemoglobin concentration, methemoglobin fraction, and albumin concentration on blood water T1 . It can be used to predict blood T1 at multiple fields. Magn Reson Med 76:270-281, 2016. © 2015 Wiley Periodicals, Inc.

Characterization and Suppression Techniques for Degree of Radiation Damping in Inversion Recovery Measurements

Radiation damping is a phenomenon in which transverse nuclear magnetization couples with the current in a coil used in nuclear magnetic resonance experiments. This results in an additional magnetic field that increases the relaxation pathway for the magnetization, which then relaxes back to equilibrium more quickly. Radiation damping has been shown to affect longitudinal relaxation time (T1) measurement in inversion recovery experiments. In this work, we demonstrate that the extent of radiation damping depends upon the T1 of the sample. Radiation damping difference spectroscopy is used to characterize the severity of radiation damping, while gradient inversion recovery is used for radiation damping suppression in T1 measurements. At field strength of 9.4 T, for the radiation damping characteristic time (Trd) of 50 ms, these investigations show non-negligible radiation damping effects for T1 values greater than Trd, with severe distortions for T1 longer than about 150 ms, showing reasonable agreement with the predicted Trd. We also report a discrepancy between published expressions for the characteristic radiation damping time.

Visualization of Cortical Lamination Patterns with Magnetic Resonance Imaging

The ability to image the cortex laminar arrangements in vivo is one of the holy grails of neuroscience. Recent studies have visualized the cortical layers ex vivo and in vivo (on a small region of interest) using high-resolution T(1)/T(2) magnetic resonance imaging (MRI). In this study, we used inversion-recovery (IR) MRI to increase the sensitivity of MRI toward cortical architecture and achieving whole-brain characterization of the layers, in vivo, in 3D on humans and rats. Using the IR measurements, we computed 3D signal intensity plots along the cortex termed corticograms to characterize cortical substructures. We found that cluster analyses of the multi-IR images along the cortex divides it into at least 6 laminar compartments. To validate our observations, we compared the IR-MRI analysis with histology and revealed a correspondence, although these 2 measures do not represent similar quantities. The abilities of the method to segment the cortex into layers were demonstrated on the striate cortex (visualizing the stripe of Gennari) and on the frontal cortex. We conclude that the presented methodology can serve as means to study and characterize individual cortical architecture and organization.

Shortened Modified Look-Locker Inversion recovery (ShMOLLI) for clinical myocardial T1-mapping at 1.5 and 3 T within a 9 heartbeat breathhold.

BackgroundT1 mapping allows direct in-vivo quantitation of microscopic changes in the myocardium, providing new diagnostic insights into cardiac disease. Existing methods require long breath holds that are demanding for many cardiac patients. In this work we propose and validate a novel, clinically applicable, pulse sequence for myocardial T1-mapping that is compatible with typical limits for end-expiration breath-holding in patients.Materials and methodsThe Shortened MOdified Look-Locker Inversion recovery (ShMOLLI) method uses sequential inversion recovery measurements within a single short breath-hold. Full recovery of the longitudinal magnetisation between sequential inversion pulses is not achieved, but conditional interpretation of samples for reconstruction of T1-maps is used to yield accurate measurements, and this algorithm is implemented directly on the scanner. We performed computer simulations for 100 ms<T1 < 2.7 s and heart rates 40-100 bpm followed by phantom validation at 1.5T and 3T. In-vivo myocardial T1-mapping using this method and the previous gold-standard (MOLLI) was performed in 10 healthy volunteers at 1.5T and 3T, 4 volunteers with contrast injection at 1.5T, and 4 patients with recent myocardial infarction (MI) at 3T.ResultsWe found good agreement between the average ShMOLLI and MOLLI estimates for T1 < 1200 ms. In contrast to the original method, ShMOLLI showed no dependence on heart rates for long T1 values, with estimates characterized by a constant 4% underestimation for T1 = 800-2700 ms. In-vivo, ShMOLLI measurements required 9.0 ± 1.1 s (MOLLI = 17.6 ± 2.9 s). Average healthy myocardial T1 s by ShMOLLI at 1.5T were 966 ± 48 ms (mean ± SD) and 1166 ± 60 ms at 3T. In MI patients, the T1 in unaffected myocardium (1216 ± 42 ms) was similar to controls at 3T. Ischemically injured myocardium showed increased T1 = 1432 ± 33 ms (p < 0.001). The difference between MI and remote myocardium was estimated 15% larger by ShMOLLI than MOLLI (p < 0.04) which suffers from heart rate dependencies for long T1. The in-vivo variability within ShMOLLI T1-maps was only 14% (1.5T) or 18% (3T) higher than the MOLLI maps, but the MOLLI acquisitions were twice longer than ShMOLLI acquisitions.ConclusionShMOLLI is an efficient method that generates immediate, high-resolution myocardial T1-maps in a short breath-hold with high precision. This technique provides a valuable clinically applicable tool for myocardial tissue characterisation.

Inversion recovery measurements of exciton fine-structure beats in a single quantum dot

We present a method for time-resolving the coherent precession of the spin of a single neutral exciton confined to an InAs/GaAs quantum dot. A pair of circularly polarized π pulses are used to pump and probe the exciton spin, rather than a pair of interferometrically stable π/2-pulses in a quantum interference type experiment, faster, technically simpler, measurements of the small 15 μeV exciton fine-structure can be made in the photocurrent regime. A small change in the fine-structure splitting with vertically applied electric-field is observed.

Proton NMR relaxation as a probe for setting cement pastes

We report a 20-MHz proton nuclear magnetic resonance T1 relaxation study of cement paste hydration in the early stages of setting, using different centimeter-sized samples of cements of various origins and different water-to-cement ratios. In every sample, during the first few minutes of hydration, it is found that inverse Laplace processing of inversion-recovery measurements systematically exhibits at least two T1 values: a long one, around 100 ms, whose value correlates well with water content and which may be attributed to bulk water surrounding cement grains; and a short one, around 2 ms, which is quite insensitive to water-to-cement ratio and which may be attributed to water embedded in floculated cement grains before setting occurs. The time evolution of the longest T1 value for several hours is also shown to exhibit a characteristic five-stage behavior that is well correlated with known stages of the hydration process: initial reaction, induction period, acceleration period, deceleration period and slow hydration reaction. These results are compared with calorimetric measurements and electrical conductivity literature.

Investigation of water bound to photosystem I with multiquantum filtered O17 nuclear magnetic resonance

A new analytical approach was developed to characterize the properties of water molecules bound to macromolecules in solution using 17 O nuclear magnetic resonance (NMR) relaxation. A combination of conventional (single-quantum) and triple-quantum filtered Hahn echo and inversion recovery measurements was employed. From measured relaxation rate constants, the fraction and the correlation time of bound H2 17 O molecules and the relaxation rate constant of bulk water in solution were calculated. This was done by solving analytically a set of nonlinear equations describing the overall relaxation rate constants in the presence of chemical exchange between bulk and bound water. The analytical approach shows the uniqueness of the solution for a given set of three relaxation rate constants. This important result sheds light on the data reduction problem from 17 O NMR experiments on biological systems. Water bound in photosystem I isolated from the wild type and rubA variant of the cyanobacterium Synechocystis species PCC 7002 was investigated for the first time. The analysis revealed that photosystem I isolated from the wild type binds 1720+/-110 water molecules, whereas photosystem I isolated from the rubA variant binds only 1310+/-170. The accuracy of the method proposed can be increased by further 17 O enrichment. The methodology, established for the first time in this work, allows the study of a diverse range of biological samples regardless of their size and molecular weight. Applied initially to photosystem I, this novel method has important consequences for the future investigation of the assembly of biological molecules.

Electron spin relaxation of copper(II) complexes in glassy solution between 10 and 120 K

The temperature dependence, between 10 and 120 K, of electron spin–lattice relaxation at X-band was analyzed for a series of eight pyrrolate–imine complexes and for ten other copper(II) complexes with varying ligands and geometry including copper-containing prion octarepeat domain and S100 type proteins. The geometry of the CuN 4 coordination sphere for pyrrolate–imine complexes with R = H, methyl, n-butyl, diphenylmethyl, benzyl, 2-adamantyl, 1-adamantyl, and tert-butyl has been shown to range from planar to pseudo-tetrahedral. The fit to the recovery curves was better for a distribution of values of T 1 than for a single time constant. Distributions of relaxation times may be characteristic of Cu(II) in glassy solution. Long-pulse saturation recovery and inversion recovery measurements were performed. The temperature dependence of spin–lattice relaxation rates was analyzed in terms of contributions from the direct process, the Raman process, and local modes. It was necessary to include more than one process to fit the experimental data. There was a small contribution from the direct process at low temperature. The Raman process was the dominant contribution to relaxation between about 20 and 60 K. Debye temperatures were between 80 and 120 K. For samples with similar Debye temperatures the coefficient of the Raman process tended to increase as g z increased, as expected if modulation of spin–orbit coupling is a major factor in relaxation rates. Above about 60 K local modes with energies in the range of 260–360 K (180–250 cm −1) dominated the relaxation. For molecules with similar geometry, relaxation rates were faster for more flexible molecules than for more rigid ones. Relaxation rates for the copper protein samples were similar to rates for small molecules with comparable coordination spheres. At each temperature studied the range of relaxation rates was less than an order of magnitude. The spread was smaller between 20 and 60 K where the Raman process dominates, than at higher temperatures where local modes dominate the relaxation. Spin echo dephasing time constants, T m, were calculated from two-pulse spin echo decays. Near 10 K T m was dominated by proton spins in the surroundings. As temperature was increased motion and spin–lattice relaxation made increasing contributions to T m. Near 100 K spin–lattice relaxation dominated T m.

Inversion recovery measurements in the presence of radiation damping and implications for evaluating contrast agents in magnetic resonance

Relaxation measurements performed at high magnetic field in magnetic resonance (MR) may be adversely affected by the influence of radiation damping in concentrated samples such as water. We consider how the measured value of T1 is affected by this phenomenon for a gadolinium-doped water sample and for an undoped water sample and consider the implications for evaluating contrast agents. A simple method involving the application of a pulsed field gradient to de-phase residual transverse components of the magnetization is shown to be an effective method for suppressing this effect. Given the central role that measurement of the T1 of water plays in the assessment of contrast agents as well as a host of other MR applications, care should always be employed when measuring and interpreting T1 measurements at high magnetic fields.

NMR studies of peptide T, an inhibitor of HIV infectivity, in an aqueous environment

The synthetic octapeptide peptide T (ASTTTNYT) has been shown to interfere with binding of the HIV-1 envelope glycoprotein gp120 to the chemokine receptor R5, thus preventing viral infection. This study investigated the degree of conformational order of two analogs of peptide T, one biologically active (D-Ala peptide T amide) and one inactive (D-Ala, D-Tyr peptide T amide) using nuclear magnetic resonance (NMR) spectroscopy in an aqueous environment, both in solution and in the frozen solid state. Standard solution NMR techniques such as DQFCOSY, HMQC, ROESY and inversion recovery measurements have been utilized to characterize these peptides. Solid state NMR experiments were likewise employed to study the peptides in a frozen glycerol:water mixture. The NMR results indicate that the monomeric form of both peptide T analogs have considerable conformational heterogeneity. Solid state NMR studies indicate aggregation of D-Ala peptide T, possibly into a beta-sheet structure, at concentrations higher than 10 mM.

A novel method for analysis of TOMROP data.

To develop an efficient method for extracting maps of the corrected T1 from images generated using the T One by Multiple Read Out Pulses (TOMROP) sequence. An expression is developed for the true T1 in terms of the parameters from a three-parameter fit of the TOMROP data. Solutions of gadodiamide in normal saline with concentrations of 0.0, 0.06, 0.11, 0.23, 0.46, and 0.91 mM were prepared and T1 measurements were performed using both the inversion recovery (IR) and the TOMROP methods. The TOMROP data were analyzed using the proposed technique and the results compared to those from the IR measurements. The T1 estimates generated from the TOMROP data using the proposed method were consistent with the IR results. However, systematic errors were observed in the T1 estimates when the repetition time was not sufficient for full recovery of axial magnetization. Relaxation times determined using the proposed method were within 1% of the spectroscopiclly determined values for T1 values in the range of 0.28-2.8 seconds when a suitable delay was employed. The proposed method of analysis was found to yield accurate T1 estimates when the assumptions used in the analysis were not violated.

Effect of increased repetition time TR on precision of inversion-recovery T1 measurements

The effect of increased repetition time, TR, on the precision of inversion-recovery measurements of the spin-lattice relaxation time, T1, was calculated theoretically, simulated numerically, and measured experimentally. All three methods yielded similar results. With constant inversion times, the T1 precision was independent of TR. Therefore, 1) multiple-slice inversion-recovery fast-spin-echo T1 maps should be made one slice at a time, not with interleaved acquisition, and 2) once the longest inversion time ti has been set, TR should be set just enough longer than the longest ti to allow data acquisition.

Investigation of solute–solvent interactions in a dithiophosphoroorganic carbohydrate derivative by means of X-ray analysis and solid state NMR

Bis[6-O,6′-O-(1,2∶3,4-diisopropylidene-α-D-galactopyranosyl)thiophosphoryl] disulfide 1 (C48H76O24P2S4) crystallized from polar and/or nonpolar solvents forms different inclusion complexes and solvates. The X-ray data for complexes of 1 with propan-2-ol (1a) and acetone (1b) are reported. From DSC measurements it is apparent that with loss of the solvent, crystals undergo complex rearrangements below the melting point forming the 1c modification. Each form is characterized by 31P CP/MAS experiment. The analysis of the 31P δii principal elements of the chemical shift tensor suggests that distinction of δ33 for different modifications is related to O–H· · ·SP and C–H· · ·SP intermolecular contacts. 2H NMR spectroscopy is employed to investigate the mechanism of phase reorientation and molecular dynamics of methyls of the isopropylidene blocking groups. At ambient temperature, the C3v jump of the methyl group and additional small-amplitude motion of the five membered ring is deduced from line-shape analysis of a 2H QUADECHO experiment. During the change of sample composition at 370 K, fast molecular motion of the methyl groups is observed while the SP–S–S–PS backbone remains rigid. From variable temperature 2H T1 inversion–recovery measurements it is concluded that the Ea of the C3v jump strongly depends on molecular packing.

Pulsed Esr Studies on Microcrystalline Silicon

ABSTRACTTwo-pulse-echo field-sweep spectra of boron-doped samples show in addition to dangling bonds (DB) a very broad feature of approximately 500 G width. This feature is the sum of several lines whose relative intensities change with doping and temperature. The total intensity increases with doping. The spin-lattice relaxation time TI of the resonance at g=1.998 referred to as conduction electrons (CE) has been studied for undoped and P-doped microcrystalline silicon. The discrepancy between T1 values previously reported has been resolved and the values for CE are at least two orders of magnitude smaller than those of the DB. In undoped samples cross-relaxation between the CE and DB spin systems might explain the similar T1 values obtained for CE and DB in inversion recovery measurements.