[논문]Sintering of Si3N4 with Y2O3 and Al2O3 added by coprecipitation

Kim, J.-S.; Schubert, H.; Petzow, G.

doi:10.1016/0955-2219(89)90026-5

[해외논문] Sintering of Si3N4 with Y2O3 and Al2O3 added by coprecipitation

Journal of the European Ceramic Society, v.5 no.5, 1989년, pp.311 - 319

Kim, J.-S. , Schubert, H. , Petzow, G.

Abstract ▼ AI-Helper

The aim of this work was to improve the chemical and geometrical homogeneity of Si3N4 powder by applying wet chemical preparation routes for the dispersion of sintering additives in Si3N4. The conventional Y2O3-Al2O3 additive system with 3:5 molar ratio (YAG) has been chosen as a standard composition. The amount added was 5, 10 and 15 mole%, respectively. Three routes have been comparably tested: precipitation of hydroxides from nitrates with ammonia onto the Si3N4 surfaces, precipitation in the absence of Si3N4 followed by mechanical mixing with Si3N4, and mechanical mixing of oxides with Si3N4 in an attrition mill.The calcination of the powders was found to be a critical preparation step due to the risk of picking-up of additional oxygen, which results in the Si2N2O formation and slows down the densification. For calcination at 900oC under N2, the sintering behavior of the precipitated powder was favorable and 2.7% higher final density could be achieved for identical sintering parameters.

Abstract

Das Ziel dieser Arbeit war die Verbesserung der chemischen und geometrischen Homogenitat von Si3N4-Pulvern durch die Anwendung von naszchemischen Verfahren zur Verteilung der Sinteradditive im Si3N4-Pulver.Als Additive wurde das konventionelle Y2O3-Al2O3-System mit einem molaren Verhaltnis von 3:5 (YAG) gewahlt. Es wurden 5, 10 und 15 mol-% beigegeben und 3 verschiedene Verfahrenswege im Vergleich getestet: Die direkte Prazipitation der Hydroxide aus Nitratverbindungen in Ammoniak auf die Siliziumnitridoberflachen, die separate Fallung der Hydroxide, gefolgt von einem mechanischen Mischen von Additiv und Si3N4 und die mechanische Mischung der Oxide mit Si3N4 in einem Attritor.Die Kalzination der Pulver war ein kritischer Schritt in dem Herstellungsprozesz, weil die Gefahr der Sauerstoffaufnahme bestind, die zur Bildung von Si2N2O fuhre und die Verdichtung verringert. Wenn die Kalzination in Stickstoff bei 900oC durchgefuhrt wurde, war das Sinterverhalten der prazipitierten Pulver gut und es konnte unter den gleichen Sinterbedingungen eine um 2.7% hohere Enddichte erreicht werden.

Abstract

Le but de cette etude etait d'ameliorer l'homogeneite chimique et geometrique d'une poudre de Si3N4 en dispersant les additifs de frittage synthetises par voie chimique en solution. L'additif classique du systeme Y2O3-Al2O3 de rapport molaire 3:5 (YAG) a ete choisi. Les quantites ajoutees etaient de 5, 10 et 15% molaires. Trois voies ont ete comparees: precipitation des hydroxydes a partir des nitrates dans l'ammoniaque sur la surface du Si3N4, precipitation en l'absence de Si3N4 suivie d'un melange mecanique et homogeneisation des oxydes et du Si3N4 dans un broyeur par attrition. Nous avons constate que la calcination des poudres etait une etape critique en raison du risque d'oxydation qui entrine la formation de Si2N2O et ralentit la densification. La poudre precipitee calcinee a 900oC sous azote atteint, dans des conditions de frittage identiques, une densite superieure de 2.7% a celle des autres poudres.

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[해외논문] Sintering of Si3N4 with Y2O3 and Al2O3 added by coprecipitation

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