论文标题
使用udeft(均匀驱动的平衡傅立叶变换)对$ {}^{29} $ si NMR实验的提高灵敏度和量化
Improved sensitivity and quantification for ${}^{29}$Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform)
论文作者
论文摘要
我们证明了使用Udeft(均匀驱动平衡傅立叶变换)技术的可能性,以提高一维$ {}^{29} $ si NMR实验的灵敏度和量化魔法旋转(MAS)。我们得出UDEFT和单脉冲(SP)实验的信噪比的分析表达,从而累积了瞬态和稳态状态的贡献。 Using numerical spin dynamics simulations and experiments on ${}^{29}$Si-enriched amorphous silica and borosilicate glass, we show that 59${}_{180}$298${}_{0}$59${}_{180}$ refocusing composite $π$-pulse and the adiabatic使用TANH/TAN调制的反演提高了UDEFT技术的鲁棒性,对RF感染,偏移和化学移动各向异性。这些脉冲与两步相循环结合限制了脉冲缺陷和刺激回声产生的伪影。 SP,UDEFT和CPMG(Carr-Purcell Meiboom-Gill)技术的灵敏度在实验化和非官能化介孔二氧化硅上进行了比较。此外,对火焰材料的实验证明,Udeft技术可以更好地量化$ {}^{29} $ SI位点,其灵敏度比SP方法更高。
We demonstrate the possibility to use UDEFT (Uniform Driven Equilibrium Fourier Transform) technique in order to improve the sensitivity and the quantification of one-dimensional ${}^{29}$Si NMR experiments under Magic-Angle Spinning (MAS). We derive an analytical expression of the signal-to-noise ratios of UDEFT and single-pulse (SP) experiments subsuming the contributions of transient and steady-state regimes. Using numerical spin dynamics simulations and experiments on ${}^{29}$Si-enriched amorphous silica and borosilicate glass, we show that 59${}_{180}$298${}_{0}$59${}_{180}$ refocusing composite $π$-pulse and the adiabatic inversion using tanh/tan modulation improve the robustness of UDEFT technique to rf-inhomogeneity, offset, and chemical shift anisotropy. These pulses combined with a two-step phase cycling limit the pulse imperfections and the artifacts produced by stimulated echoes. The sensitivity of SP, UDEFT and CPMG (Carr-Purcell Meiboom-Gill) techniques are compared experimentally on functionalized and non-functionalized mesoporous silica. Furthermore, experiments on a flame retardant material prove that UDEFT technique provides a better quantification of ${}^{29}$Si sites with higher sensitivity than SP method.