Elaboration and Characterization of Mullite Refractory Products from Moroccan Andalusite
Enrichment of schist mined in Morocco resulted in an extract essentially made of andalusite, quartz and muscovite, which was investigated with the aim to synthesize mullite refractory materials. X-ray diffraction analysis was used to assess phase transformations upon heating at different temperatures. Mullite formation starts as early as 1200℃ and seems almost total at 1450℃. This process correlates with a weak shrinkage (3.5% at 1450℃) and the formation of an important glass phase. Green compacts obtained by unidirectional pressing the extract powder were heated under air in the temperature range 1200℃ - 1600℃. Chemical and mechanical properties of these materials were investigated and correlated with their microstructure.
Copper sludge from printed circuit board production/recycling for ceramic materials: a quantitative analysis of copper transformation and immobilization.
The fast development of electronic industries and stringent requirement of recycling waste electronics have produced a large amount of metal-containing waste sludge. This study developed a waste-to-resource strategy to beneficially use such metal-containing sludge from the production and recycling processes of printed circuit board (PCBs). To observe the metal incorporation mechanisms and phase transformation processes, mixtures of copper industrial waste sludge and kaolinite-based materials (kaolinite and mullite) were fired between 650 and 1250 °C for 3 h. The different copper-hosting phases were identified by powder X-ray diffraction (XRD) in the sintered products, and CuAl2O4 was found to be the predominant hosting phase throughout the reactions, regardless of the strong reduction potential of copper expected at high temperatures. The experimental results indicated that CuAl2O4 was generated more easily and in larger quantities at low-temperature processing when using the kaolinite precursor. Maximum copper transformations reached 86% and 97% for kaolinite and mullite systems, respectively, when sintering at 1000 °C. To monitor the stabilization effect after thermal process, prolonged leaching tests were carried out using acetic acid with an initial pH value of 2.9 to leach the sintered products for 20 days. The results demonstrated the decrease of copper leachability with the formation of CuAl2O4, despite different sintering behavior in kaolinite and mullite systems. This study clearly indicates spinel formation as the most crucial metal stabilization mechanism when sintering copper sludge with aluminosilicate materials, and suggests a promising and reliable technique for reusing metal-containing sludge as ceramic materials.
Submicron polymer structures with X-ray lithography and hot embossing
This article describes the process chain for replication of submicron structures with varying aspect ratios (AR) up to 6 in polymethylmethacrylate (PMMA) by hot embossing to show the capability of the entire LIGA process to fabricate structures with these dimensions. Therefore a 4.7 μm thick layer of MicroChem 950k PMMA A11 resist was spin-coated on a 2.3 μm Ti/TiOx membrane. It was patterned with X-ray lithography at the electron storage ring ANKA (2.5 GeV and λc ≈ 0.4 nm) at a dose of 4 kJ/cm3 using a Si3N4 membrane mask with 2 μm thick gold-absorbers. The samples were developed in GG/BDG and resulted in AR of 6–14. Subsequent nickel plating at 52°C resulted in a 200 μm thick nickel tool of 100 mm diameter, which was used to replicate slit-nozzles and columns in PMMA. Closely packed submicron cavities with AR 6 in the nickel shim were filled to 60% during hot embossing.