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Neutron scattering studies of hard metals

Time: Fri 2022-01-28 10.00

Location: Kollegiesalen 7, Brinellvägen 8

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Language: English

Subject area: Materials Science and Engineering

Doctoral student: Ahmet Bahadir Yildiz , Egenskaper, Advanced Materials Characterization

Opponent: Dr. Daniele Mari, École Polytechnique Fédérale de Lausanne (EPFL), Switzerland

Supervisor: Prof. Peter Hedström, Egenskaper; Prof. Annika Borgenstam, Strukturer; Prof. Joakim Odqvist, Strukturer

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Since their discovery about 100 years ago, tools made of hard metals have been the enablers of development in various areas: from drilling subway lines for more sustainable cities to the machining of complex next-generation airplane engine parts for reduced CO2 emissions. An increase in properties of hard metals thus leads to efficient operations with shorter lead-time, less environmental footprint, and reduced cost. To tailor the as-sintered hard metal structure with desired properties and develop reliable modelling tools, it is critical to have statistically representative experimental data acquired in conditions mimicking the real processes for hard metals. However, to date, nano- and microstructural investigations of hard metals and related systems have been mainly focused on the lab-scale techniques, limiting the bulk-scale in-situ investigations. 

This thesis focuses on neutron scattering techniques and demonstrates how the utilization of small angle neutron scattering (SANS) techniques and neutron diffraction (ND) in a complementary manner with lab-scale techniques and computational tools can enhance the mechanistic understanding during processing of hard metals and related systems. Some of the presented information within the thesis is unique to neutron scattering experiments.

SANS experiments are used for the quantification of nano- and microstructural features including Co-rich binder pocket size, WC grain size, and size and volume fraction of (V,W)Cx interfacial layers. The quantitative data enables us to draw conclusions regarding the mechanism of grain coarsening inhibition in V-doped hard metals at different V additions. The findings indicate that the grain coarsening inhibition in V-doped hard metals originates from reduced WC/Co interface mobility and total driving force for coarsening. The complex nature of structural evolution at sintering temperatures is further investigated by in-situ SANS up to 1500 oC. Our results show that the size and volume fraction of interfacial layers strongly depend on the presence of bulk (V,W)Cx precipitates and V activity in the binder phase.

In-situ ND experiments during aging of (Ti,Zr)C-based systems provide time-resolved insights into the kinetics and structural evolution during phase separation at 1600 oC for 10 h. The results reveal that the decomposition of (Ti,Zr)C into TiC- and ZrC-rich phases can be significantly retarded by minor HfC or NbC additions. During decomposition, in line with the nucleation and growth process, no change is observed in the lattice parameter of ZrC-rich phase. In contrast, the lattice parameter of TiC-rich phase reduces with decomposition, resulting from TiC enrichment, i.e. it reaches equilibrium composition in the course of time. Furthermore, a novel multi-principal element carbide system (Ti,Zr,Hf,W)C with exceptional hardness is designed. Although the system has a miscibility gap, only minor decomposition is observed after 100 h aging at 1350 oC, where the formation of (Ti,W)C- and (Zr,Hf)C-rich decomposition products and WC precipitates occur. Such hindered decomposition enables the carbide system to preserve its high hardness.

In summary, by using neutron scattering techniques, this thesis contributes to a better understanding of nano- and microstructural evolution in hard metals and related systems during their processing at elevated temperatures. The thesis and appended papers also guide readers regarding the planning, e.g. sample preparation and sample environment selection, and data analysis of neutron scattering experiments. The thesis can thus serve as a starting point for the more widespread utilization of neutron scattering techniques by the hard metal industry.