Characterization of Calcium Aluminate Hydrates and Related Hydrates of Cement Pastes by <sup>27</sup>Al MQ-MAS NMR

Faucon, P.; Charpentier, Thibault; Bertrandie, D.; Nonat, André; Virlet, J.; Petit, Jean‐Claude

doi:10.1021/ic9800076

Cited by 101 publications

(152 citation statements)

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“…Purity of the C 3 A sample was confirmed via XRD measurement. Pure C 4 AH x was prepared according to Faucon et al [18] by reacting C 3 A with saturated lime solution at low temperature (~ 5°C) under exclusion of air to avoid carbonation. The resulting precipitate was centrifuged and after washing with cold water, white crystals were obtained.…”

Section: Methodsmentioning

confidence: 99%

Formation of an Inorganic‐Organic Host‐Guest Material by Intercalation of Acetone Formaldehyde Sulfite Polycondensate into a Hydrocalumite Structure

Plank

Hoessle

2010

Zeitschrift anorg allge chemie

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Formation of an inorganic-organic host-guest material by intercalation of acetone formaldehyde sulfite polycondensate into a hydrocalumite structure. Zeitschrift für Anorganische und Allgemeine Chemie, 2010, 636 (8) There, the novel Ca-Al-LDH phase shows a morphology of intergrown platelets which is typical for layered calcium aluminate hydrates. Depending on the preparation method, ultrathin foils with 20 nm -50 nm thickness were observed. TEM images also support presence of a layered structure. IntroductionDispersants such as e.g. polycarboxylates (PCE) and ß-naphthalenesulfonate-formaldehyde based polycondensates (BNS) which are widely used as superplasticizers in concrete have been reported to intercalate into cement hydrates under favorable conditions [1][2][3][4]. Upon hydration which is often referred to as rehydration [5], the cement clinker phase tricalcium aluminate (Ca 3 Al 2 O 6 , abbreviation C 3 A) can form layered double hydroxides of the hydrocalumite type. Anionic superplasticizer polymers of various structure and molecular weight can counterbalance the charge of the cationic sheets and intercalate between the layers. In this study, a linear acetone formaldehyde sulfite polycondensate (AFS) [6] has been synthesized and was used in rehydration experiments with tricalcium aluminate. Its chemical structure is presented in Figure 1. Because of the structural similarity of AFS with other polycondensates (e.g. BNS) it seemed possible to obtain novel organomineral phases from the reaction of AFS with C 3 A. Results and Discussion XRD analysisThe Ca-Al-AFS-LDH composite was synthesized by reacting 1 g of tricalcium aluminate with 100 mL of a 2 wt.% aqueous AFS solution for 24 hours at room temperature under nitrogen protection to avoid carbonation of the product. The XRD pattern for the Ca-Al-AFS-LDH is shown in Figure 2. At 3.3° 2θ a reflection is observed which can be attributed to the [00l] reflections of the layered material. The corresponding d value which represents the basal spacing in the intercalate is 27 Å. One weak harmonic is observed at d = 13.5 Å (6.5° 2θ). Further reflections for [hk0] of the host-guest system can be found at approx. 31.5° 2θ and for [0k0] at about 55.8° 2θ. This XRD pattern confirms the intercalation of AFS into the Ca-Al-LDH host structure and a certain stacking regularity of the tactoid. Similar d values were reported for organic sulfonated compounds such as e.g. poly(vinyl sulfonate) and poly(styrene sulfonate) [12] and alkyl sulfonates [13]. There, basal spacings in the range of 13.2 Å -19.6 Å and 27.0 Å -32.3 Å, respectively were found. For comparison, the XRD pattern of synthesized C 4 AH 13 is shown in Figure 2. It exhibits a [00l] reflection at 11.2° 2θ which corresponds to a basal spacing of only 7.9 Å, compared to 27 Å for the intercalate. Thus it is shown that incorporation of AFS significantly increases the interlayer distance. The steric size of AFS, the elemental composition of the intercalate as shown below and the d value obtained from XRD suggest that t...

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Section: Methodsmentioning

confidence: 99%

Formation of an Inorganic‐Organic Host‐Guest Material by Intercalation of Acetone Formaldehyde Sulfite Polycondensate into a Hydrocalumite Structure

Plank

Hoessle

2010

Zeitschrift anorg allge chemie

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“…Otherwise, we have to use conventions whose apparent carrier frequencies are always positive. This is the reason for which conventions C z [38,59,96,98,[106][107][108] and C k(1) [17,29,68,72,77,87,91,93,97,98,[109][110][111] are the most applied.…”

Section: Theorymentioning

confidence: 99%

Procedures for Labeling the High-Resolution Axis of Two-Dimensional MQ-MAS NMR Spectra of Half-Integer Quadrupole Spins

Millot

Man

2002

Solid State Nuclear Magnetic Resonance

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The increasing development and application of the multiple-quantum MAS NMR for halfinteger quadrupole spins has led to various RF pulse sequences for improving the excitation of multiple-quantum coherences and their conversion to single-quantum coherences. As a result, several conventions for labeling the F1 dimension of a 2D MQ-MAS spectrum appear in the literature. The corresponding relations for extracting the isotropic chemical shift, the quadrupole coupling constant, and the asymmetry parameter from experimental data are not always provided. We analyze these various conventions systematically and propose a new one, similar to that introduced by J.-P. Amoureux and C. Fernandez (2000, Solid State NMR 10, 339-343). These various conventions are illustrated with 27 Al (I = 5/2) nuclei in aluminum acetylacetonate Al(CH 3 COCHCOCH 3 ) 3 . Another experimental problem often met, the aliasing of peaks in the 2D spectrum, is analyzed and illustrated with 27 Al (I = 5/2) in NH 4 Y zeolite and 23 Na (I = 3/2) in sodium pyrophosphate Na 4 P 2 O 7 . © 2002 Elsevier Science (USA)

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“…With this energy, the substitution of SO 4 with Si tetrahedra. [5][6][7][8][9][10][11][12][13][14] A comparison of the calculated values with the experimental results could be conducted by considering more relaxed atoms with the surrounding water molecules in the calculation procedures.…”

Section: Reaction Possibilitymentioning

confidence: 99%

“…[5][6][7][8][9][10][11][12][13][14] However, there is no clear evidence regarding the interaction of C-S-H gel and AFt in these experimental as well as in the theoretical studies. These substitutions generally take place in the structure of C-S-H gel by substituting with paired and bridging Si tetrahedra especially at C/S>1.…”

Section: Introductionmentioning

confidence: 99%

Ab InitioCalculations for the Substitutions of Al(OH)^-₄and SO^2-₄with Si Tetrahedra

Rahman¹,

Nagasaki²,

Tanaka³

2001

Journal of Nuclear Science and Technology

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We have studied the interaction phenomena for the substitutions of Al(OH) − 4 and SO 2− 4 with both paired and bridging Si tetrahedra likely to be occurred in C-S-H gel coexisting with ettringite system. Gaussian 94 program has been used to obtain the total energy of the molecule in the optimized structure employing HF/3-21G * level of theory. It has been investigated that the net charge on the substitution site causes the modification of the original structure during the substitution. The substitutions of Al(OH)

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Characterization of Calcium Aluminate Hydrates and Related Hydrates of Cement Pastes by ²⁷Al MQ-MAS NMR

Cited by 101 publications

References 42 publications

Formation of an Inorganic‐Organic Host‐Guest Material by Intercalation of Acetone Formaldehyde Sulfite Polycondensate into a Hydrocalumite Structure

Formation of an Inorganic‐Organic Host‐Guest Material by Intercalation of Acetone Formaldehyde Sulfite Polycondensate into a Hydrocalumite Structure

Procedures for Labeling the High-Resolution Axis of Two-Dimensional MQ-MAS NMR Spectra of Half-Integer Quadrupole Spins

Ab InitioCalculations for the Substitutions of Al(OH)^-₄and SO^2-₄with Si Tetrahedra

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Characterization of Calcium Aluminate Hydrates and Related Hydrates of Cement Pastes by 27Al MQ-MAS NMR

Cited by 101 publications

References 42 publications

Formation of an Inorganic‐Organic Host‐Guest Material by Intercalation of Acetone Formaldehyde Sulfite Polycondensate into a Hydrocalumite Structure

Formation of an Inorganic‐Organic Host‐Guest Material by Intercalation of Acetone Formaldehyde Sulfite Polycondensate into a Hydrocalumite Structure

Procedures for Labeling the High-Resolution Axis of Two-Dimensional MQ-MAS NMR Spectra of Half-Integer Quadrupole Spins

Ab InitioCalculations for the Substitutions of Al(OH)-4and SO2-4with Si Tetrahedra

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Characterization of Calcium Aluminate Hydrates and Related Hydrates of Cement Pastes by ²⁷Al MQ-MAS NMR

Ab InitioCalculations for the Substitutions of Al(OH)^-₄and SO^2-₄with Si Tetrahedra