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Deposition and characterization of single and multilayered boron carbide and boron carbonitride thin films by different sputtering configurations

Abstract : Over the last 30 years there has been a great deal of interest in the research of hard and wear resistant coatings. There exist ceramic thin films for industrial applications such as cutting tools, automobile and machine part including TiN, TiAlN, TiC, SiC, WC as examples. However, increasing technological and industrial demands request thin films with more advanced properties. For this purpose, B-C-N ternary system with its superhard phases is of great interest during last ten years. Boron carbide (B4C) with its high hardness and modulus besides other relevant properties is one of the most prominent candidates. Furthermore, boron carbonitride (BCN) thin films are attracting due to the combination of different properties as a result of that of different phases such as diamond, cubic boron nitride (c-BN) and hexagonal boron nitride (h-BN). A thorough literature study shows that these two materials have not been yet investigated in details in the thin film form. Boron carbide is one of the least studied materials by atomistic deposition techniques such as sputtering and the least studied compound in the B-C-N ternary diagram. On the other hand, almost all the efforts were given by different researchers to deposit cubic boron nitride. Very little only could be found focusing on the effect of nitrogen incorporation into boron carbide structure and on the different phases that could be obtained. The aim of this thesis study is first to investigate the effect of different sputter deposition parameters on the properties of boron carbide thin films and to establish a relation between deposition parameters, growth morphologies of boron carbide films and mechanical and wear properties. Second, to study the effect of nitrogen incorporation into boron carbide structure and to grow optimized hard and tough BCN thin films with an improved wear resistance. In this work, single and multilayered boron carbide and boron carbonitride thin films were deposited by several sputtering configurations. Three types of well-adherent and homogenous boron carbide films were deposited by conventional direct current (DC) magnetron sputtering, plasma-enhanced DC magnetron sputtering, and radio frequency (RF) sputtering. Boron carbonitride thin films deposited by reactive DC magnetron sputtering with addition of nitrogen to the processing gas were also studied. Functionally-graded multilayered designs were used to grow thicker boron carbide and boron carbonitride films. An "in-house" produced direct current compatible boron carbide target and a commercial boron carbide target were used for the deposition of thin films. The effect of deposition parameters on film properties were studied by using various characterization techniques. Elemental composition of the films was measured by electron probe microanalysis (EPMA). Field–emission gun scanning electron microscope (FE-SEM) was used to investigate the microstructure and the morphology of the films. Elemental depth profiles of the coatings were obtained using a secondary ion mass spectrometer (SIMS). Nanomechanical properties were determined by nanoindentation. Tribological properties of the coatings were studied using "pin–on–disc" testing. Chemical bonding was investigated by Fourier transform infrared spectroscopy (FTIR). Nanostructure and crystallinity of the films were evaluated by transmission electron microscopy (TEM) observation. Results demonstrated that boron carbide films are promising candidates for wear resistance and hardness related applications. With a controlled change of process parameters, different microstructures, thus films with different properties were obtained. With N incorporation into boron carbide structure, optimized hard and better wear-resistant films were achieved. This showed that application ranges may be further expanded. Additionally, it was found that functionally-graded multilayered approach is an adequate solution to prevent film delamination and intrinsic stress related problems of hard and wear-resistant films. Thicker boron carbide and boron carbonitride films for several industrial applications could therefore be deposited easily with a proper design for the different underlayers.
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Submitted on : Monday, February 1, 2010 - 8:00:00 AM
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Tolga Tavsanoglu. Deposition and characterization of single and multilayered boron carbide and boron carbonitride thin films by different sputtering configurations. Engineering Sciences [physics]. École Nationale Supérieure des Mines de Paris, 2009. English. ⟨NNT : 2009ENMP1641⟩. ⟨pastel-00005772⟩

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