COMUNICAÇÃO TÉCNICA _____________________________________________________________________________________________________________________________________________________ _________________________________________________ Nº 170936 Lead-free glass frit for automotive application Cátia Fredericci H. Fellegara A.P. Abreu A.L. Molisani H.N. Yoshimura Trabalho apresentado no Brazilian Symposium on Glass and Related Materials, 9., Curitiba, 2012. Slide da apresentação. A série “Comunicação Técnica” compreende trabalhos elaborados por técnicos do IPT, apresentados em eventos, publicados em revistas especializadas ou quando seu conteúdo apresentar relevância pública. ___________________________________________________________________________________________________ Instituto de Pesquisas Tecnológicas do Estado de São Paulo S/A - IPT Av. Prof. Almeida Prado, 532 | Cidade Universitária ou Caixa Postal 0141 | CEP 01064-970 São Paulo | SP | Brasil | CEP 05508-901 Tel 11 3767 4374/4000 | Fax 11 3767-4099 www.ipt.br Lead-free glass frit for automotive application Fredericci, (1) C. , (2) H. , (3) Abreu Molisani, (1) A.L. (4) Yoshimura,H.N. Fellegara A.P. , (1) Instituto de Pesquisas Tecnológicas do Estado de São Paulo - IPT (2) Ticon – Tintas Condutivas Ltda (3) Raw Materials (4) Universidade Federal do ABC (UFABC) [email protected] 1 ABSTRACT In the light of recent health and environmental restrictions and concerns, the use of PbO and CdO is largely avoided whenever possible. Several frits that fuse at low temperature and present low toxicity, containing Bi2O3, SiO2, and B2O3 have been developed as lead-free frits for automotive application. Many studies have been published about lead free glass frit; however, few publications have been made regarding the refractory used to melt them. In this work it was analyzed the glass formation in the system Bi2O3-SiO2-B2O3-TiO2 melted in electrocast mullite and electrocast alumina-zirconia-silica (AZS) refractory. The glass was melted at 1250oC/5h and quenched in water. The resulting frit was analyzed by X ray diffraction (XRD), X ray fluorescence (XRF) and differential thermal analyses. The refractories were cut and their cross sections were analyzed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The results of XRD shown that the frit was vitreous and presents glass transition temperature and crystallizes at about 480oC and 615oC, respectively. The electrocast AZS refractory was more adequate than the electrocast mullite for melting the glass studied. Figure 2. (a) and (b) SEM micrographs of the interface glass-mullite refractory, (c) and (d) EDS spectra of the points listed in (b). 2 MATERIALS AND METHODS - The commercial refractories indicated in Table 1 were cut using a diamond saw to approximately 50x50x73 mm3. -Cylindrical holes were made in the central region with dimensions of 25 mm diameter by 50 mm deep. -The glass composition listed in Table 1 was put on the crucible, was heated at 1250 oC for 5 h and quenched in water. -The resulting frit was analyzed by X ray fluorescence (XRF). -The refractories were cut and their cross sections were analyzed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). Table 1. Refractory materials used for melting the glass. Figure 3. (a) SEM micrograph of the interface glass-AZS refractory, (b), (c), (d), (e), (f) , (g) EDS spectra of the points listed in (a). 3.2 X Ray Fluorescence Spectroscopy Table 2. Nominal glass composition (wt%) Table 2. Glass composition (wt%) after melting in AZS refractory. 3 RESULTS 4 CONCLUSION 3.1 Microstructural Analysis The best refractory tested for melting the bismuth based glass was the AZS. The composition of the glass after melting showed a little contamination of ZrO2 and Al2O3, but did not compromise the properties of the frit. It is a potential lead free material to be used in formulation of enamels for the formation of black band on rear windows of cars. glass refractory Figure 1. Photographs of refractories after melting the glass at 1250 oC/5h. KNOWLEDGMENTS C. Fredericci thanks CNPq for funding (P. 313242/2009-7).