Factors affecting frit solubility in glaze suspensions
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1 Factors affecting frit solubility in glaze suspensions Dr. Arnaldo Moreno Instituto de Tecnología Cerámica Asociación de Investigación de las Industrias Cerámicas Universitat Jaume I, Castellón, Spain
2 My talk today Frits and ceramic glazes Frit solubility Effect of glaze constituents on cation release Influence of process variables on lixiviation kinetics
3 Frits and ceramic glazes Background Frits are key constituents in all floor and wall tile glazes. About 4% of ceramic glazes just consist of frits (9 95% w/w) and kaolin (5 1% w/w). Ceramic glazes are applied as aqueous suspensions or slips, by different techniques. Minor amounts of deflocculant (sodium tripolyphosphate (TPP)) and binder (sodium carboxymethylcellulose (CMC)) are used to keep slip rheological behaviour steady.
4 Viscosidad (Pa s) Fuerza de cizalla (Pa) Viscosity (Pa s) Frits and ceramic glazes The problem Glaze rheological behaviour varies on aging 1 Viscosidad Fuerza ,1,1,1,1,1, Gradiente de velocidad (1/s).1, Shear rate (1/s) Flow curve on day of preparation Viscosity curve after 16 days aging
5 Frit solubility Things we knew Lixiviation occurs in glasses (Si-O -...K + ) Frit + H 2 O Si-OH Frit + OH - Sol + K + (Si-O -...R O-Si) Frit + H 2 O 2Si-OH Frit + 2OH - Sol + R +2 K Ca Zn Mg Crust H 2 O R +2 : Ca +2, Mg +2, Zn +2 Frit (Si-OH) Frit + H 2 O (Si-O - ) Sol. + H 3 O + Sol. (B-OH) Frit + H 2 O (B-O - ) Sol. + H 3 O + Sol.
6 Content (w/w %) Frit solubility Things we did Determination of frit cation release SiO 2 Al 2 O 3 B 2 O 3 CaO Na 2 O K 2 O Frit components ZnO PbO MgO ZrO 2
7 Frit solubility Things we did Determination of frit cation release Dry grinding of the frit at lab scale. Residue: 1% at 4µm mesh. Dispersion of the ground frit in 15 cm 3 distilled water. Standing time: 24h. Temperature: 7ºC. Determination of cations in solution by atomic absorption spectrophotometry and colorimetry.
8 Frit solubility Things we learned Determination of frit cation release Solids content (SC): 6% 3 3 Concentration (mol/l) Concentration (mol/l) 1 3 K K Ca Mg 1 Ca Zn Mg time (h) time (h)
9 Effect of glaze constituents on cation release Things we knew Cations in aqueous media can interact with glaze components Plastic solid particles Deflocculant (TPP) Binder (CMC) Flocculating action Reduction of effectiveness Salt formation/precipitation All interactions are dynamic, as solubilization is a continuous process
10 Effect of glaze constituents on cation release Things we did Adding.25% TPP to frit suspension SC=6% T=3ºC Calcium concentration (mol/l) TPP Water Magnesium concentration (mol/l) TPP Water Time (h) Time (h) TPP forms stable soluble complexes with Ca, Mg, and Zn.
11 Effect of glaze constituents on cation release Things we did Adding.25% TPP to frit suspension SC=6% T=3ºC Potassium concentration (mol/l) TPP 1 Water Time (h) Boron concentration (mol/l) TPP Water Time (h) TPP also enhances diffusion of ions that do not form complexes.
12 Effect of glaze constituents on cation release Things we did Adding.25% TPP to frit suspension SC=6% T=3ºC TPP ph Water Time (h) TPP Buffer effect ph increases ph hardly changes over time
13 Influence of process variables on lixiviation kinetics Things we changed Slip temperature Boron concentration (mol/l) ºC 5ºC 3ºC Time (h) Magnesium concentration (mol/l) ºC 5ºC 3ºC Time (h) TPP =.25% SC = 6%
14 Influence of process variables on lixiviation kinetics Things we changed Slip temperature 5 Zinc concentration (mol/l) ºC 5ºC 3ºC Time (h) TPP =.25% SC = 6%
15 Influence of process variables on lixiviation kinetics Things we changed Solids content (SC) SC (w/w %) SA/V (m 2 /m 3 ) x x x 1 6 Concentration (mol/l) 1 3 B K Ca Si Mg (SA/V) 1-6 (m 2 /m 3 ) T = 3ºC SA/V: particle surface area/solution volume
16 Influence of process variables on lixiviation kinetics Things we changed Frit particle size (milling time) Test Residue (4µm mesh) Calcium Magnesium Zinc Potassium Boron 1 1% %
17 Influence of process variables on lixiviation kinetics Things we changed Standing time Test Standing time Calcium Magnesium Zinc Potassium Boron 1 3 min h h days
18 In conclusion We now know that Frits in aqueous solutions release mainly magnesium, calcium, potassium, and boron. The presence of TPP enhances the release of these cations which, in some cases, form soluble complexes. Suspension temperature and solids content speed up the frit dissolution process. Slip standing time has a twofold effect on the lixiviation process, which increases the dissolution rate.
19 Many thanks for your attention Arnaldo Moreno, Senior Researcher Instituto de Tecnología Cerámica, Castellón, Spain,
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