In:
Journal of the American Ceramic Society, Wiley, Vol. 101, No. 2 ( 2018-02), p. 919-927
Abstract:
The main goal of this work was to verify whether a phase with composition K 2 CaSi 4 O 10 exists in the ternary system K 2 O‐CaO‐SiO 2 . Therefore, a series of solid‐state reactions of stoichiometric mixtures of K 2 CO 3 , CaCO 3 and SiO 2 was performed at 800 and 900?C which, indeed, resulted in the formation of this previously unknown potassium calcium silicate. More detailed characterizations of this compound were based on single‐crystal X‐ray diffraction experiments. Basic crystallographic data are as follows: triclinic symmetry, space group P‐1 , a = 7.0915(7) Å, b = 8.4211(9) Å, c = 10.2779(12) Å, α = 104.491(10)°, β = 100.570(9)°, γ = 113.738(9)°, V = 515.26(10) Å 3 , Z = 2. Structure solution was performed by direct methods. Subsequent refinement calculations using anisotropic displacement parameters for all atoms converged to a residual of R (| F |) = 0.0355 for 1889 independent reflections with I 〉 2σ( I ). From a structural point of view K 2 CaSi 4 O 10 belongs to the so‐called litidionite family of A′ AMS i 4 O 10 compounds for which several natural and synthetic representatives have been described in the literature. Actually, it is the first member where the A′‐ and A‐positions are exclusively occupied by K‐ions. Following the nomenclature for oxosilicates K 2 CaSi 4 O 10 can be allocated to the group of the tubular chain silicates. Fundamental building units are loop‐branched dreier double chains (running parallel to [100]) which can be described using the following structural formula: { lB , }[ 3 Si 8 O 20 ]. Ca‐ions are coordinated by 5 nearest oxygen neighbors in form of distorted trigonal bipyramids. By sharing a common edge two adjacent bipyramids are linked into [Ca 2 O 8 ]‐dimers providing linkage between consecutive tubes in the direction of the c ‐axis. Charge compensation is achieved by the incorporation of the larger potassium ions into cavities of the heteropolyhedral network. Powder X‐ray diffraction patterns of the bulk material of the synthesis products revealed that, additionally to K 2 CaSi 4 O 10 , the 800°C ‐sample contained K 8 CaSi 10 O 25 and at least one further, yet unknown crystalline phase. This unidentified so‐called 22‐Å compound was also present in the 900 °C‐specimen together with K 2 CaSi 4 O 10 and K 2 Ca 4 Si 8 O 21 . Our proof of existence of K 2 CaSi 4 O 10 is a further step towards a better understanding of the ternary system K 2 O‐CaO‐SiO 2 and provides a basis for identification and quantification of this compound in phase analysis. It corrects earlier phase‐analytical studies on this system which is of relevance for applied and technical mineralogy including different types of residual materials such as slags or ashes from biomass combustion. The results of our investigation show that even comparatively simple ternary oxide systems are not as well understood as expected.
Type of Medium:
Online Resource
ISSN:
0002-7820
,
1551-2916
DOI:
10.1111/jace.2018.101.issue-2
Language:
English
Publisher:
Wiley
Publication Date:
2018
detail.hit.zdb_id:
2008170-4
detail.hit.zdb_id:
219232-9
Permalink