Magic-angle spinning NMR spectra of satellite transitions for quadrupolar nuclei in solids

Jakobsen, Hans J.; Skibsted, Jørgen; Bildsøe, Henrik; Nielsen, Niels Chr.

doi:10.1016/0022-2364(89)90333-8

Cited by 111 publications

(182 citation statements)

References 7 publications

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“…These salts display a single, well-defined, noncubic local environment for 23 Na in their structure [39], and should, therefore, exhibit an I SSE /I CB ratio close to the theoretical value of 1.5. Values of 1.43 and 1.39 were observed for each salt, respectively, which lie within a margin of 7% from the limiting value.…”

mentioning

confidence: 56%

“…Because of their orientation dependence, the satellite transitions merge into a broad component for nonoriented solids (e.g., ceramics). Due to magic angle spinning (MAS), this otherwise broad component splits into a series of narrower peaks [39,40], called the spinning sideband envelope (SSE). Under these conditions the central component is called the center band (CB).…”

mentioning

confidence: 99%

“…1(a)] provides an SSE which resembles a broad Gaussian without the characteristic spectral features of a single welldefined quadrupolar interaction tensor [30,39]. Hence, it reflects a distribution in the magnitude of components from the EFG tensor [43], which indicates partial disorder in the local structure of this material.…”

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confidence: 99%

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Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiO
Groszewicz
¹
,
Breitzke
²
,
Dittmer
³

et al. 2014
Phys. Rev. B
58
1
34
0
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We address the unsolved question on the structure of relaxor ferroelectrics at the atomic level by characterizing lead-free piezoceramic solid solutions (100 − x)(Bi 1/2 Na 1/2 )TiO 3 -xBaTiO 3 (BNT-xBT) (for x = 1, 4, 6, and 15). Based on the relative intensity between spectral components in quadrupolar perturbed 23 Na nuclear magnetic resonance, we present direct evidence of the coexistence of cubic and polar local symmetries in these relaxor ferroelectrics. In addition, we demonstrate how the cubic phase vanishes whenever a ferroelectric state is induced, either by field cooling or changing the dopant amount, supporting the relation between this cubic phase and the relaxor state. Relaxor ferroelectrics have been intensively studied in the past 30 years because of their intriguing structural and dielectric features [1][2][3]. Despite that, the nature of their ground state remains an open question [4][5][6][7][8][9][10][11][12]. Several models have been proposed to describe this puzzling class of materials [1,[5][6][7][8]13], two of which are mainly concerned with the structure of the ground state of relaxors [4].The random field (RF) model proposes a single-phase structure broken up into ferroelectric nanodomains. These nanodomains are kept small under the constraint of quenched random electric fields which originate from chemical disorder [7,14]. The other model introduced the concept of "polar nanoregions" (PNRs) [13]. When relaxors are cooled below the Burns temperature, small and randomly oriented polarized regions (PNRs) appear within the otherwise nonpolar crystal structure. Upon further cooling, PNRs grow in size and number [11], but their percolation is prevented by structural disorder and random electric fields [8,10,12]. This behavior would imply the coexistence of PNRs and a nonpolar matrix, in contrast to the single-phase structure proposed by the RF model.An induced ferroelectric state can be established in relaxors when a strong electric field is applied. This state features macroscopic polarization and breaking of the cubic average symmetry [5,11,[15][16][17]. While the RF model suggests that this transformation and the formation of macroscopic ferroelectric domains are caused only by reorientation of previously nanometric ferroelectric domains, an additional mechanism is required when PNRs are considered. In that case, a long-range ferroelectric state can only be established if the nonpolar matrix becomes polarized, being incorporated by the growing PNRs.Two questions are raised by contrasting these two models: (1) Does the microscopic structure of relaxor ferroelectrics consist only of ferroelectric nanodomains or do regions of lower local symmetry (PNRs) coexist with a nonpolar matrix of * gerd.buntkowsky@chemie.tu-darmstadt.de † roedel@ceramics.tu-darmstadt.de undistorted structure? (2) How does the microscopic structure of relaxors evolve upon electric poling?In spite of their relevance, such questions have remained unsolved largely because the structural characterization of relaxors is a c...

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confidence: 56%

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confidence: 99%

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Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiO
Groszewicz
¹
,
Breitzke
²
,
Dittmer
³

et al. 2014
Phys. Rev. B
58
1
34
0
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“…Следует отметить, что ядра алюминия являются хорошим ЯМР-зондом с высоким гиромаг-нитным отношением (γ/2π = 11.094 MHz/T) и спином ядра I = 5/2, что позволяет изучать также и локальное зарядовое окружение. Известно [15][16][17][18], что этот метод давно и успешно используется для изучения особенно-стей кристаллической структуры, зарядового окружения как в поликристаллических образцах Al 2 O 3 с различной кристаллической структурой, так и в нанокристалличе-ских образцах.…”

Section: Introductionunclassified

Особенности кристаллической структуры и магнитных свойств наночастиц Al-=SUB=-2-=/SUB=-O-=SUB=-3-=/SUB=- по данным ЯМР -=SUP=-27-=/SUP=-Аl

Михалев¹,

Гермов²,

Ермаков³

et al. 2017

Физика Твердого Тела

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Измерена намагниченность при комнатной температуре, получены спектры ЯМР 27 Аl в серии наночастиц Al 2 O 3 c разным размером частицы. Полевая зависимость намагниченности свидетельствует о наличии у небольшой части образца дальнего ферромагнитного порядка при комнатной температуре, однако относительный объем этого вклада очень мал (меньше 1%) и, вероятно, это связано с примесной фазой. В спектрах ЯМР отсутствует линия от металлического алюминия, наличие которого в этих нанооксидах ранее предполагалось в поверхностном слое наночастиц по данным других методик. Получены данные о фазовом составе и зарядовом распределении в различных фазах наночастиц Al 2 O 3 . Изменение среднего размера частиц (в ∼ 3 раза) лишь незначительно изменяет их фазовый состав.Работа выполнена в рамках государственной программы, тема " Спин" № 01201463330 с финансовой поддержкой по проектам РФФИ № 16-02-00416 и 14-02-00032. Измерения намагниченности выполнены в рамках темы " Магнит" № 01201463228.

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“…Recent advances in the design of very high-speed (vR < 20 kHz) and stable (±5 Hz) spinning devices and probes have proven extremely useful for studies of half-integer quadrupolar nuclei in solids [5][6][7]. Using these probes, the complete spinning-side-band patterns for the satellite transitions extending over large spectral width were observed for several solids [8][9][10]. In addition, the computer simulation of the complete spinning-side-band manifolds for the satellite transitions allows quadrupole coupling constant and asymmetry parameters to be determined with high accuracy [10].…”

Section: Introductionmentioning

confidence: 99%

Single-Quantum NMR Spinning-Side-Band Patterns for Spin-3/2 System

et al. 1997

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The NMR response of an isolated spin-3/2 system with an axially symmetric quadrupolar interaction under magic-angle sample spinning to an ideal radio-frequency pulse using irreducible tensor operators is evaluated analytically. The excited single-quantum spin coherences are modulated by the sample spinning. The effects of spinning frequency, quadrupole coupling constant and the orientation of quadrupolar interaction relative to rotor axis on the spinning-side-band patterns are simulated. High-resolution single-quantum spinning-side-band pattern detected for 23 Νa (I = 3/2) nuclei in sodium nitrate powder is compared with the simulation based on the theory and the quadrupole coupling is estimated.

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Magic-angle spinning NMR spectra of satellite transitions for quadrupolar nuclei in solids

Cited by 111 publications

References 7 publications

Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiO
Groszewicz
¹
,
Breitzke
²
,
Dittmer
³

et al. 2014
Phys. Rev. B
58
1
34
0
View full text Add to dashboard Cite

Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiO
Groszewicz
¹
,
Breitzke
²
,
Dittmer
³

et al. 2014
Phys. Rev. B
58
1
34
0
View full text Add to dashboard Cite

Особенности кристаллической структуры и магнитных свойств наночастиц Al-=SUB=-2-=/SUB=-O-=SUB=-3-=/SUB=- по данным ЯМР -=SUP=-27-=/SUP=-Аl

Single-Quantum NMR Spinning-Side-Band Patterns for Spin-3/2 System

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Magic-angle spinning NMR spectra of satellite transitions for quadrupolar nuclei in solids

Cited by 111 publications

References 7 publications

Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiOGroszewicz1, Breitzke2, Dittmer3 et al. 2014Phys. Rev. B581340View full textAdd to dashboardCite

Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiOGroszewicz1, Breitzke2, Dittmer3 et al. 2014Phys. Rev. B581340View full textAdd to dashboardCite

Особенности кристаллической структуры и магнитных свойств наночастиц Al-=SUB=-2-=/SUB=-O-=SUB=-3-=/SUB=- по данным ЯМР -=SUP=-27-=/SUP=-Аl

Single-Quantum NMR Spinning-Side-Band Patterns for Spin-3/2 System

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Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiO
Groszewicz
¹
,
Breitzke
²
,
Dittmer
³

et al. 2014
Phys. Rev. B
58
1
34
0
View full text Add to dashboard Cite

Nanoscale phase quantification in lead-free(Bi1/2Na1/2)TiO3−BaTiO
Groszewicz
¹
,
Breitzke
²
,
Dittmer
³

et al. 2014
Phys. Rev. B
58
1
34
0
View full text Add to dashboard Cite