Fast plasma sintering deposition of nano-structured silicon carbide coatings

Fast plasma sintering deposition of SiC nano-structured coatings was achieved using a specially designed non-transferred dc plasma torch operated at reduced pressure. Employing the Taguchi method, the deposition parameters were optimized and verified. With the optimized combination of deposition parameters, homogeneous SiC coatings were deposited on relatively large area substrates of Φ50 mm and 50×50 mm with a deposition rate as high as 20 μm/min. Ablation test showed that such coatings can be used as oxidation resistance coatings in high temperature oxidizing environment.

Thermophoretic control of building units in the plasma-assisted deposition of nanostructured carbon films

The role of the plasma-grown nanoparticles in the plasma-enhanced chemical vapor deposition (PECVD) of the nanostructured carbon-based films was investigated. The samples were grown in the low-pressure rf plasmas of CH 4+H2+Ar gas mixtures. The enhanced deposition of the building units from the gas phase was found to support the formation of polymorphous nanostructured carbon films. The results reveal the crucial role played by the thermophoretic force in controlling the deposition of the plasma-grown fine particles.

High-rate, room temperature plasma-enhanced deposition of aluminum-doped zinc oxide nanofilms for solar cell applications

A custom-designed inductively coupled plasma (ICP)-assisted radio-frequency magnetron sputtering deposition system has been employed to synthesize aluminium-doped zinc oxide (ZnO:Al) nanofilms on glass substrates at room temperature. The effects of film thickness and ZnO target (partially covered by Al chips) power on the structural, electrical and optical properties of the ZnO:Al nanofilms are studied. A high growth rate (∼41 nm/min), low electrical sheet resistance (as low as 30 Ω/□) and high optical transparency (>80%) over the visible spectrum has been achieved at a film thickness of ∼615 nm and ZnO target power of 150 W. The synthesis of ZnO:Al nanofilms at room temperature and with high growth rates is attributed to the unique features of the ICP-assisted radio-frequency magnetron sputtering deposition approach. The results are relevant to the development of photovoltaic thin-film solar cells and flat panel displays.

RF plasma sputtering deposition of hydroxyapatite bioceramics : synthesis, performance, and biocompatibility

Hydroxyapatite (HA) coatings have numerous applications in orthopedics and dentistry, owing to their excellent ability to promote stronger implant fixation and faster bone tissue ingrowth and remodeling. Thermal plasma spray and other plasma-assisted techniques have recently been used to synthesize various calcium phosphate-based bioceramics. Despite notable recent achievements in the desired stoichiometry, phase composition, mechanical, structural, and bio-compatible properties, it is rather difficult to combine all of the above features in a single coating. For example, many existing plasma-sprayed HA coatings fall short in meeting the requirements of grain size and crystallinity, and as such are subject to enhanced resorption in body fluid. On the other hand, relatively poor interfacial bonding and stability is an obstacle to the application of the HA coatings in high load bearing Ti6Al4V knee joint implants. Here, we report on an alternative: a plasma-assisted, concurrent, sputtering deposition technique for high performance biocompatible HA coatings on Ti6Al4V implant alloy. The plasma-assisted RF magnetron co-sputtering deposition method allows one to simultaneously achieve most of the desired attributes of the biomimetic material and overcome the aforementioned problems. This article details the film synthesis process specifications, extensive analytical characterization of the material's properties, mechanical testing, simulated body fluid assessments, biocompatibility and cytocompatibility of the HA-coated Ti6Al4V orthopedic alloy. The means of optimization of the plasma and deposition process parameters to achieve the desired attributes and performance of the HA coating, as well as future challenges in clinical applications are also discussed.

Reactive species in RF plasma sputtering deposition of nanocrystalline calcium phosphate bio-active films

Optical emission of reactive plasma species during the synthesis of functionally graded calcium phosphate-based bioactive films has been investigated. The coatings have been deposited on Ti-6Al-4V orthopedic alloy by co-sputtering of hydroxyapatite (HA) and titanium targets in reactive plasmas of Ar + H2O gas mixtures. The species, responsible for the Ca-P-Ti film growth have been non-intrusively monitored in situ by a high-resolution optical emission spectroscopy (OES). It is revealed that the optical emission originating from CaO species dominates throughout the deposition process. The intensities of CaO, PO and CaPO species are strongly affected by variations of the operating pressure, applied RF power, and DC substrate bias. The optical emission intensity (OEI) of reaction species can efficiently be controlled by addition of H2O reactant.

Spark plasma sintering of novel ZrB2-SiC-TiSi2 composites with better mechanical properties

We report here the development of ultrafine grained ZrB2-SiC composites using TiSi2 as the sintering aid and spark plasma sintering (SPS) as the processing technique. It was observed that the presence of TiSi2 improved the sinterability of the composites, such that near theoretical densification (99.9%) could be achieved for ZrB2-18 wt.% SiC-5 wt.% TiSi2 composites after SPS at 1600 degrees C for 10 min at 50 MPa. Use of innovative multi stage sintering (MSS) route, which involved holding the samples at lower (intermediate) temperatures for some time before holding at the final temperature, while keeping the net holding time to 10 min, allowed attainment of full densification of ZrB2-18 wt.% SiC-2.5 wt.% TiSi2 at a still lower final temperature of 1500 degrees C at 30 MPa. TEM observations, which revealed the presence of anisotropic ZrB2 grains with faceted grain boundaries and TiSi2 at the intergranular regions, suggested the occurrence of liquid phase sintering in the presence of TiSi2. No additional phase was detected in XRD as well as TEM, which confirmed the absence of any sintering reaction. The as developed composites possessed an excellent combination of Vickers hardness and indentation toughness, both of which increased with increase in TiSi2 content, such that the ZrBi2-18 wt.% SiC-5 wt.% TiSi2 (SPS processed at 1600 degrees C) possessed hardness of similar to 20 GPa and indentation toughness of similar to 5 MPa m(1/2). The use of MSS SPS at 1500 degrees C for ZrBi2-18 wt.% SiC-2.5 wt.% TiSi2 composite resulted in improvement in hardness of up to similar to 27 GPa and attainment of high flexural strength of similar to 455 MPa. (C) 2011 Elsevier B.V. All rights reserved.

On the densification mechanisms and properties of Cu-Pb and Cu-Pb-TiB2 nanocomposites densified using spark plasma sintering

The present paper is aimed to understand the sub-processes triggered by rapid heating during spark plasma sintering as well as to assess the extent to which densification and properties of metallic materials can be enhanced using such superfast consolidation process. Using nanocrystalline Cu-Pb as a model system, the influence of Pb as well as TiB2 addition on the densification mechanisms and properties are discussed. Importantly, a high hardness of 2 GPa is achieved in Cu-based nanocomposites. (C) 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Spark plasma sintering may lead to phase instability and inferior mechanical properties: A case study with TiB2

In contrast to the widely reported beneficial aspects of spark plasma sintering in developing materials with better properties, we report here two interesting aspects recorded with difficult-to-sinter titanium diboride: (a) in situ formation of second phase (TiB) and (b) inferior hardness (by similar to 30%) and elastic modulus (by similar to 20%) for spark plasma sintered TiB2, with respect to hot pressed TiB2. The formation of TiB is discussed with reference to the enhanced reaction kinetics in the presence of pulsed electric field. (C) 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Direct Characterizing of Densification Mechanisms during Spark Plasma Sintering

Spark plasma sintering (SPS) is a convenient and rapid means of producing dense ceramic compacts. However, the mechanisms responsible for rapid densification have not been identified satisfactorily, with different studies using an indirect approach yielding varied values for the densification parameters. This study involved SPS in high purity nanocrystalline alumina with temperatures ranging from 1173 to 1423K and stresses from 25 to 100MPa. A direct approach, with analyses at a constant density, revealed a stress exponent of similar to 1 and an inverse grain size dependence of similar to 3, consistent with Coble creep process. Whereas the direct approach gives a stress exponent of similar to 1, the indirect approach used previously gives stress exponents ranging from similar to 2.2 to 3.5 with the same data, thereby revealing potentially spurious values of the densification parameters from conventional indirect approaches to characterizing densification. The rapid densification during SPS is related to the finer grain sizes retained with the rapid heating rates and the imposed stress that enhances the driving force for densification.

Influence of yttria and zirconia additions on spark plasma sintering of alumina composites

The mechanisms of densification and creep were examined during spark plasma sintering (SPS) of alumina doped with a low and high level of zirconia or yttria, over a temperature range of 1173-1573 K and stresses between 25 and 100 MPa. Large additions of yttria led clearly to in situ reactions during SPS and the formation of a yttrium-aluminum garnet phase. Dopants generally lead to a reduction in the densification rate, with substantial reductions noted in samples with similar to 5.5 vol% second phase. In contrast to a stress exponent of n similar to 1 for pure alumina, the doped aluminas displayed n similar to 2 corresponding to an interface-controlled diffusion process. The higher activation energies in the composites are consistent with previous data on creep and changes in the interfacial energies. The results reveal a compensation effect, such that an increase in the activation energy is accompanied by a corresponding increase in the pre-exponential term for diffusion.

Spark plasma sintering of TiNi nano-powders for biological application

Nano-sized TiNi powder with an average size of 50nm was consolidated using spark plasma sintering (SPS) at 800 °C for 5min. A layer of anatase TiO 2 coating was formed on the sintered TiNi by chemical reaction with a hydrogen peroxide (H2O2) solution at 60 °C followed by heat treatment at 400 °C to enhance the bioactivity of the metal surface. Cell culture using osteoblast cells and a biomimetic test in simulated body fluid proved the biocompatibility of the chemically treated SPS TiNi. © IOP Publishing Ltd.

Mechanical behaviour of AISiC nano composites produced by Ball Milling and Spark Plasma Sintering

Neste trabalho foram produzidos nanocompósitos de AlSiC misturando alumínio puro com nano partículas de SiC com diâmetro de 45 – 55 nm, usando, de forma sequencial, a técnica da metalurgia do pó e a compactação por “ Spark Plasma Sintering”. O compósito obtido apresentava grãos com 100 nm de diâmetro, encontrandose as partículas de SiC localizadas, principalmente, nas fronteiras de grão. O nanocompósito sob a forma de provetes cilíndricos foi submetido a testes de compressão uniaxial e a testes de nanoindentação para analisar a influência das nanopartículas de SiC, da fração volúmica de ácido esteárico e do tempo de moagem, nas propriedades mecânicas do material. Para efeitos de comparação, utilizouse o comportamento mecânico do Al puro processado em condições similares e da liga de alumínio AA1050O. A tensão limite de elasticidade do nanocompósito com 1% Vol./Vol. de SiC é dez vezes superior à do AA1050. O refinamento de grão à escala nano constitui o principal mecanismo de aumento de resistência mecânica. Na realidade, o Al nanocristalino sem reforço de partículas de SiC, apresenta uma tensão limite de elasticidade sete vezes superior à da liga AA1050O. A adição de 0,5 % Vol./Vol. e de 1 % Vol./Vol. de SiC conduzem, respetivamente, ao aumento da tensão limite de elasticidade em 47 % e 50%. O aumento do tempo de moagem e a adição de ácido esteárico ao pó durante a moagem conduzem apenas a um pequeno aumento da tensão de escoamento. A dureza do material medida através de testes de nanoindentação confirmaram os dados anteriores. A estabilidade das microestruturas do alumínio puro e do nanocompósito AlSiC, foi testada através de recozimento de restauração realizado às temperaturas de 150 °C e 250 °C durante 2 horas. Aparentemente, o tratamento térmico não influenciou as propriedades mecânicas dos materiais, excepto do nanocompósito com 1 % Vol./Vol. de SiC restaurado à temperatura de 250 °C, para o qual se observou uma redução da tensão limite de elasticidade na ordem dos 13 %. No alumínio nanocristalino, a tensão de escoamento é controlada pelo efeito de HallPetch. As partículas de SiC, são segregadas pelas fronteiras do grão e não contribuem para o aumento de resistência mecânica segundo o mecanismo de Orowan. Alternativamente, as nanopartículas de SiC constituem um reforço das fronteiras do grão, impedindo o seu escorregamento e estabilizando a nanoestrutura. Deste modo, as propriedades mecânicas do alumínio nanocristalino e do nanocompósito de AlSiC poderão estar relacionadas com a facilidade ou dificuldade do escorregamento das fronteiras de grão, embora não seja apresentada prova explícita deste mecanismo à temperatura ambiente.