Qualitative and Quantitative Study of Stacking Faults in a Hydrazine Treated Kaolinite—Relationship with the Infrared Spectra

Barrios, J.; Plançon, A.; Cruz, M. I.; Tchoubar, C.

doi:10.1346/ccmn.1977.0250608

Cited by 62 publications

(52 citation statements)

References 20 publications

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“…Nevertheless, these reflections are notably broader than those of untreated kaolinite, even in the pattern obtained at 400~ (Figure 6). Thus, the number of layers in the diffracting domains notably decreased as a consequence of the intercalation process, a relationship first noted by Barrios et al (1977).…”

Section: Htxrd Resultsmentioning

confidence: 54%

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Thermal Behavior of the Kaolinite-Hydrazine Intercalation Complex

Cruz

Franco

2000

Clays and clay miner.

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Abstract--The intercalation complex of a low-defect ("well-crystallized") kaolinite from Cornwall, England, with hydrazine was studied by high-temperature X-ray diffraction (HTXRD), differential thermal analysis (DTA), and thermogravimetry (TG). The X-ray pattern at room temperature indicated that intercalation of hydrazine into kaolinite causes an increase of the basal spacing from 7.14 to 10.4 A, as previously reported. Heating between 25-200~ produces a structural rearrangement of the complex, which initially causes a contraction of the basal spacing from 10.4 to 9.6 A. In a second stage, the basal spacing reduces to 8.5 A. Finally, in a third stage, a reduction in spacing occurs through a set of intermediate phases, interpreted as interstratifications of intercalated and non-intercalated 1:1 layers. Evidence for these changes was observed by DTA, where three endothermic reactions are observed at low temperature. This behavior suggests that intercalated molecules occupy several well-defined sites in the interlayer of the kaolinite complex. The intercalated molecules deintercalate in an ordered fashion, which explains the successive and discontinuous contraction of the basal spacing of the complex. Heating between 200-400~ caused a limited increase in stacking order of the kaolinite structure, whereas dehydroxylation of kaolinite and the disappearance of its X-ray reflections occurred between 450-640~

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Section: Htxrd Resultsmentioning

confidence: 54%

“…The intercalation method can characterize kaolinite with various degrees of lattice disorder and intercalation reactivity (Range et al, 1969;Fernfindez Gonz~ilez et al, 1976;Jackson and Abdel-Kader, 1978;Theng et al, 1984;G~ibor et al, 1995). Hydrazine was also used to induce artificial disorder in kaolinite (Barrios et al, 1977).…”

Section: Introductionmentioning

confidence: 99%

Thermal Behavior of the Kaolinite-Hydrazine Intercalation Complex

Cruz

Franco

2000

Clays and clay miner.

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“…Nevertheless, this reflection is significantly broader than that of untreated dickite. Thus, the number of layers in the diffracting domains decreased as a consequence of the intercalation-desorption processes, which was noted by Barrios et al (1977) from a study of the K-H complex.…”

Section: Resultsmentioning

confidence: 66%

Thermal Decomposition of a Dickite-Hydrazine Intercalation Complex

Cruz

Franco

2000

Clays and clay miner.

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Abstract--The intercalation complex of a low-defect dickite from Tarifa, Spain, with hydrazine was studied by high-temperature X-ray diffraction (HTXRD), differential thermal analysis (DTA), and thermogravimetry (TG). The X-ray diffraction (XRD) pattern obtained at room temperature indicated that the intercalation of hydrazine and H20 into dickite caused an increase of the basal spacing from 7.08 to 10.24 A, which is slightly lower than the 10.4-A spacing commonly observed after intercalation into kaolinite. Heating between 25-50~ produced a structural rearrangement of the complex, which decreased the basal spacing from 10.24 to 9.4 A, and the resulting 9.4-A complex was stable between 50-90~ Heating between 90-300~ caused a gradual reduction in spacing, which occurred through a set of intermediate phases. These phases were interpreted to be interstratifications of intercalated and non-intercalated layers. These changes were also observed by DTA and TG. Two main endothermic reactions and two main stages of mass loss, respectively, were indicated in the DTA and the TG curves in the temperature range 25-200~ This behavior suggests that intercalated molecules, hydrazine and H20, occupied well-defined sites in the interlayer of the dickite. The intercalated molecules were lost in an ordered fashion as confirmed by the infrared analysis of the decomposition products; H~O was lost in the first stage and ammonia was identified in the second stage. Above 300~ complete removal of the intercalated molecules restored the basal spacing of the dickite. However, the basal reflections were broadened, the relative intensities were changed, and changes in the dehydroxylation temperature indicated that the intercalation-desorption process induced some stacking disorder in the dickite structure.

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“…It must be remembered that kaolinites may show disordered states. In this case a decrease in the intensity at ~ 3690 cm -1 has been observed compared with well-crystallized kaolinite (Barrios et al, 1977).…”

Section: Discussionmentioning

confidence: 68%

The use of RbCl disks for the infrared spectroscopy detection of hydrated and dehydrated halloysite in mixtures with kaolinite

Mendelovici

Sagarzazu²

1985

Clay miner.

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A simple IR spectroscopy method for detecting hydrated and dehydrated halloysite in artificial mixtures with kaolinite is described. The method is based on the exclusive ability of RbC1 among the alkali halides to form a complex with haUoysite but not with kaolinite. This complex absorbs at 3500 cm -1 when hydrated halloysite or admixed halloysite is examined in RbCI disks, the limit of detection being 15% in the kaolin admixture. Heating the clay powders or corresponding RbCI disks at 110~ affects the 3500 cm ~ frequency. The development of this absorption band together with a decrease in the intensity ratio of the 3690/3620 cm -~ frequencies is proportional to increasing amounts of halloysite in the kaolin admixtures. This method has an analytical applicability and is relatively rapid.When both kaolinite and halloysite are present in a sample, characterization and crystallinity measurements from X-ray diffraction (XRD) may be misleading (Keller & Haenni, 1978) and other investigative methods are desirable. Electron microscopy can distinguish between the platy morphology of kaolinite and tubular morphology of halloysite. In the present paper it is shown how infrared spectroscopy (IR) can be used to identify halloysite, in its hydrated or dehydrated forms, mixed with kaolinite in different proportions. In contrast to kaolinite, halloysite may form a complex with RbC1 under appropriate conditions, whereas neither of these clays interact with KBr. Thus, the unusual alkali halide RbC1 is used here as a matrix for the preparation of the disks for IR study. The development of the RbC1 complex with increasing concentrations of halloysite can be detected by IR spectroscopy, indicating an analytical potential for this simple and rapid method. EXPERIMENTALArtificial mixtures of halloysite (Ward's # 13) and kaolinite (Georgia, USA) in different weight proportions (5, 10, 15, 25, 35, 50, 75, 85 and 95% halloysite in kaolinite) were prepared by thoroughly mixing the corresponding amounts of clays. Each mixture was examined by IR absorption spectroscopy in the 4000-1500 cm -1 region with a Perkin Elmer model 567 grating spectrophotometer. Disks of 13 mm diameter were made in a die, after manual gentle mixing (to avoid grinding effects), using 0.1250 g previously dried fine RbC1 powder (Merck) plus 0.0008 g of dried (110~ or undried clay. Spectra of freshly prepared disks were recorded before and after heating the disks at 110~ A dry glove box was used for handling the powders or disks. If heated, they were subsequently cooled under 9 1985 The Mineralogical Society

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Qualitative and Quantitative Study of Stacking Faults in a Hydrazine Treated Kaolinite—Relationship with the Infrared Spectra

Cited by 62 publications

References 20 publications

Thermal Behavior of the Kaolinite-Hydrazine Intercalation Complex

Thermal Behavior of the Kaolinite-Hydrazine Intercalation Complex

Thermal Decomposition of a Dickite-Hydrazine Intercalation Complex

The use of RbCl disks for the infrared spectroscopy detection of hydrated and dehydrated halloysite in mixtures with kaolinite

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