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Thixoforming : Semi-solid Metal Processing

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8.5 Developing Al 2O 3 PECVD Coatings for <strong>Thixoforming</strong> Mouldsj269<br />

g-Al2O3 and t-ZrO2, worked well in the forming experiments. A suitable interlayer<br />

concept was developed to provide good adhesion in order to support the oxidic PVD<br />

top layer. The combination of oxide coatings with a TiAlN interlayer showed good<br />

results after SEM and EDS evaluation. A comparison between uncoated and coated<br />

dies confirmed the stability of the oxide coating system and its potential for<br />

technological application in the semi-<strong>solid</strong> forming process.<br />

8.5<br />

Developing Al2O3 PECVD Coatings for <strong>Thixoforming</strong> Moulds<br />

Alumina (Al2O3) coatings are known to exhibit advantageous mechanical properties<br />

and also chemical inertness and oxidation resistance at high temperatures [39]. Thin<br />

alumina films act as diffusion barriers for Ni, Al, Ti and Ta even at 1100 C during<br />

annealing for 100 h [40] and it has been shown that this material is a suitable<br />

candidate for coatings used in wear and hot gas protection applications [41, 42].<br />

Therefore, in this work, we investigated alumina coatings for protecting die surfaces<br />

during the semi-<strong>solid</strong> processing of steel [43]. Despite the availability of tooling<br />

concepts for the semi-<strong>solid</strong> processing of Al-based alloys [44], the increase in the tool<br />

lifetime is an almost unaddressed challenge for the semi-<strong>solid</strong> processing of steel [43].<br />

The degradation of the die is enabled through the interaction between the die and the<br />

casting alloy at temperatures >1300 C [45] and may result in the formation of<br />

intermetallic phases, chemical reaction products, thermal fatigue cracking and wear<br />

by erosion and corrosion [46, 47]. Alumina, exhibiting the previously discussed<br />

properties, is therefore a promising candidate to fulfil the requirements of semi-<strong>solid</strong><br />

processing of steel. Alumina as a polymorphous material exists in several modifications<br />

(a-, k-, g-, d-, q-Al2O3). The alumina polymorphs presenting the highest<br />

protective performances are the thermodynamically stable a-alumina and the<br />

metastable k-alumina. Various deposition techniques including CVD [42] and<br />

PECVD methods have also been employed to synthesize alumina coatings at<br />

relatively low temperatures. Lin et al. reported the growth of amorphous alumina<br />

for deposition temperatures ranging between 200 and 600 C [48], while T€aschner<br />

et al. reported a mixture of a- and g-alumina and even phase pure a-alumina, utilizing<br />

an unipolar pulsed DC plasma at a substrate temperature of 650 C [49].<br />

Although the reduction of the deposition temperature allowed by these latter<br />

methods is significant, it is not sufficient for coatings on steel since tempering of steel<br />

tools occurs at approximately 550 C [50]. The only published studies reporting<br />

deposition of a-alumina at temperatures permitting deposition on steel tools are<br />

based on homoepitaxial [51] and localized epitaxial [52] growth on chromium<br />

templates. However, the reported deposition rates (1 nm min 1 ) of both of these<br />

processes are not compatible with the requirements of the die coating industry. The<br />

major aim of our work within the SFB 289 project was to design a process to perform<br />

the deposition of a-alumina at substrate temperatures allowing deposition on steel<br />

dies, namely at 550 C. To achieve that goal, a bipolar DC PECVD method has been<br />

developed. The systematic study of the relationship between the process conditions

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