29Si{27Al} TRAPDOR MAS NMR to distinguish Qn(mAl) sites in aluminosilicates. Test case: Faujasite-type zeolites

被引:20
作者
Greiser, S. [1 ]
Hunger, M. [2 ]
Jaeger, C. [1 ]
机构
[1] Bundesanstalt Mat Forsch & Prufung BAM, Div Struct Anal 13, Richard Willstatter Str 11, D-12489 Berlin, Germany
[2] Univ Stuttgart, Inst Chem Technol, Pfaffenwaldring 55, D-70550 Stuttgart, Germany
关键词
Solid-state NMR; Si-29{Al-27} TRAPDOR MAS NMR; Q(4)(mAl) sites; Faujasite-type zeolites; Aluminosilicates; ECHO DOUBLE-RESONANCE; ALKALINE ACTIVATION; H-1; MAS; SI-29; SPECTROSCOPY; GLASSES; SILICA; AL-27; ALUMINOPHOSPHATES; GEOPOLYMERS;
D O I
10.1016/j.ssnmr.2016.10.004
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
Si-29{Al-27} TRAPDOR MAS NMR was applied to two faujasite-type zeolites with Si/Al ratios of 1.3 (Na-X) and 2.7 (Na-Y). The aim of this test study is to show that different Q(4)(mAl) sites (m = 4, 3, 2, 1) can be distinguished by differently strong TRAPDOR effects (Delta S/S-0). Indeed, it was found that the TRAPDOR effect depends on the number m of AlO4 units connected to the Q(4) silicon tetrahedrons. For Na-X, the measured Delta S/S-0 values are 1 : 0.81 : 0.56 for Q(4)(4Al), Q(4)(3Al) and Q(4)(2Al), respectively (normalized to Q(4)(4Al)). The corresponding Delta S/S-0 values are the same for Na-Y within the error bars, although the silicon sites are different: Q(4)(3Al), Q(4)(2Al) and Q(4)(1Al) and now normalized to Q(4)(3Al) as no Q(4)(4Al) is present. Nevertheless, the proposed method opens up the possibility to distinguish overlapping Si-29 NMR signals of the Q(n)(mAl) sites in amorphous materials as the main goal of these investigations.
引用
收藏
页码:6 / 10
页数:5
相关论文
共 34 条
  • [1] Synthesis and characterisation of materials based on inorganic polymers of alumina and silica: sodium polysialate polymers
    Barbosa, VFF
    MacKenzie, KJD
    Thaumaturgo, C
    [J]. INTERNATIONAL JOURNAL OF INORGANIC MATERIALS, 2000, 2 (04): : 309 - 317
  • [2] H-1(AL-27) DOUBLE-RESONANCE EXPERIMENTS IN SOLIDS - AN UNEXPECTED OBSERVATION IN THE H-1 MAS SPECTRUM OF ZEOLITE HZSM-5
    BECK, LW
    WHITE, JL
    HAW, JF
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1994, 116 (21) : 9657 - 9661
  • [3] HETERONUCLEAR DECOUPLING IN ROTATING SOLIDS
    BENNETT, AE
    RIENSTRA, CM
    AUGER, M
    LAKSHMI, KV
    GRIFFIN, RG
    [J]. JOURNAL OF CHEMICAL PHYSICS, 1995, 103 (16) : 6951 - 6958
  • [4] Dephasing of spin echoes by multiple heteronuclear dipolar interactions in rotational echo double resonance NMR experiments
    Bertmer, M
    Eckert, H
    [J]. SOLID STATE NUCLEAR MAGNETIC RESONANCE, 1999, 15 (03) : 139 - 152
  • [5] Solid state NMR investigation of the structure of AlPO4-14A
    Brouwer, DH
    Chézeau, JM
    Fyfe, CA
    [J]. MICROPOROUS AND MESOPOROUS MATERIALS, 2006, 88 (1-3) : 163 - 169
  • [6] A MAS NMR method for measuring 13C-17O distances
    Chopin, L
    Vega, S
    Gullion, T
    [J]. JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1998, 120 (18) : 4406 - 4409
  • [7] GEOPOLYMERS - INORGANIC POLYMERIC NEW MATERIALS
    DAVIDOVITS, J
    [J]. JOURNAL OF THERMAL ANALYSIS, 1991, 37 (08): : 1633 - 1656
  • [8] 29Si NMR study of structural ordering in aluminosilicate geopolymer gels
    Duxson, P
    Provis, JL
    Lukey, GC
    Separovic, F
    van Deventer, JSJ
    [J]. LANGMUIR, 2005, 21 (07) : 3028 - 3036
  • [9] Bronsted sites and structural stabilization effect of acidic low-silica zeolite A prepared by partial ammonium exchange
    Dyballa, Michael
    Obenaus, Utz
    Lang, Swen
    Gehring, Barbara
    Traa, Yvonne
    Koller, Hubert
    Hunger, Michael
    [J]. MICROPOROUS AND MESOPOROUS MATERIALS, 2015, 212 : 110 - 116
  • [10] ENGELHARDT G, 1985, PHYS CHEM GLASSES, V26, P157