An investigation of thin amorphous carbon-based sputtered coatings for MEMS and micro-engineering applications

The work presented in this thesis describes an investigation into the production and properties of thin amorphous C films, with and without Cr doping, as a low wear / friction coating applicable to MEMS and other micro- and nano-engineering applications. Firstly, an assessment was made of the available testing techniques. Secondly, the optimised test methods were applied to a series of sputtered films of thickness 10 - 2000 nm in order to: (i) investigate the effect of thickness on the properties of coatingslcoating process (ii) investigate fundamental tribology at the nano-scale and (iii) provide a starting point for nanotribological coating optimisation at ultra low thickness. The use of XPS was investigated for the determination of Sp3/Sp2 carbon bonding. Under C 1s peak analysis, significant errors were identified and this was attributed to the absence of sufficient instrument resolution to guide the component peak structure (even with a high resolution instrument). A simple peak width analysis and correlation work with C KLL D value confirmed the errors. The use of XPS for Sp3/Sp2 was therefore limited to initial tentative estimations. Nanoindentation was shown to provide consistent hardness and reduced modulus results with depth (to < 7nm) when replicate data was suitably statistically processed. No significant pile-up or cracking of the films was identified under nanoindentation. Nanowear experimentation by multiple nanoscratching provided some useful information, however the conditions of test were very different to those expect for MEMS and micro- / nano-engineering systems. A novel 'sample oscillated nanoindentation' system was developed for testing nanowear under more relevant conditions. The films were produced in an industrial production coating line. In order to maximise the available information and to take account of uncontrolled process variation a statistical design of experiment procedure was used to investigate the effect of four key process control parameters. Cr doping was the most significant control parameter at all thicknesses tested and produced a softening effect and thus increased nanowear. Substrate bias voltage was also a significant parameter and produced hardening and a wear reducing effect at all thicknesses tested. The use of a Cr adhesion layer produced beneficial results at 150 nm thickness, but was ineffective at 50 nm. Argon flow to the coating chamber produced a complex effect. All effects reduced significantly with reducing film thickness. Classic fretting wear was produced at low amplitude under nanowear testing. Reciprocating sliding was produced at higher amplitude which generated three body abrasive wear and this was generally consistent with the Archard model. Specific wear rates were very low (typically 10-16 - 10-18 m3N-1m-1). Wear rates reduced exponentially with reduced film thickness and below (approx.) 20 nm, thickness was identified as the most important control of wear.

The behaviour of polymer quenchants

The internationally accepted Wolfson Heat Treatment Centre Engineering Group test was used to evaluate the cooling characteristics of the most popular commercial polymer quenchants: polyalkylene glycols, polyvinylpyrrolidones and polyacrylates. Prototype solutions containing poly(ethyloxazoline) were also examined. Each class of polymer was capable of providing a wide range of cooling rates depending on the product formulation, concentration, temperature, agitation, ageing and contamination. Cooling rates for synthetic quenchants were generally intermediate between those of water and oil. Control techniques, drag-out losses and response to quenching in terms of hardness and residual stress for a plain carbon steel, were also considered. A laboratory scale method for providing a controllable level of forced convection was developed. Test reproducibility was improved by positioning the preheated Wolfson probe 25mm above the geometric centre of a 25mm diameter orifice through which the quenchant was pumped at a velocity of 0.5m/s. On examination, all polymer quenchants were found to operate by the same fundamental mechanism associated with their viscosity and ability to form an insulating polymer-rich-film. The nature of this film, which formed at the vapour/liquid interface during boiling, was dependent on the polymer's solubility characteristics. High molecular weight polymers and high concentration solutions produced thicker, more stable insulating films. Agitation produced thinner more uniform films. Higher molecular weight polymers were more susceptible to degradation, and increased cooling rates, with usage. Polyvinylpyrrolidones can be cross-linked resulting in erratic performance, whilst the anionic character of polyacrylates can lead to control problems. Volatile contaminants tend to decrease the rate of cooling and salts to increase it. Drag-out increases upon raising the molecular weight of the polymer and its solution viscosity. Kinematic viscosity measurements are more effective than refractometer readings for concentration control, although a quench test is the most satisfactory process control method.

Automation, rationalisation and concentration : a case study in the British chemical industry

This thesis is based upon a case study of the adoption of digital, electronic, microprocessor-based control systems by Albright & Wilson Limited - a UK chemical producer. It offers an explanation of the company's changing technology policy between 1978 and 1981, by examining its past development, internal features and industrial environment. Part One of the thesis gives an industry-level analysis which relates the development of process control technology to changes in the economic requirements of production . The rapid diffusion of microcomputers and other microelectronic equipment in the chemical industry is found to be a response to general need to raise the efficiency of all processes, imposed by the economic recession following 1973. Part Two examines the impaot of these technical and eoonomic ohanges upon Albright & Wilson Limited. The company's slowness in adopting new control technology is explained by its long history in which trends are identified whlich produced theconservatism of the 1970s. By contrast, a study of Tenneco Incorporated, a much more successful adoptor of automating technology, is offered with an analysis of the new technology policy of adoption of such equipment which it imposed upon Albright & Wilson, following the latter's takeover by Tenneco in 1978. Some indications of the consequences by this new policy of widespread adoptions of microprocessor-based control equipment are derived from a study of the first Albright & Wilson plant to use such equipment. The thesis concludes that companies which fail to adopt rapidly the new control technology may not survive in the recessionary environment, the long- established British companies may lack the flexibility to make such necessary changes and that multi-national companies may have an important role jn the planned transfer and adoption of new production technology through their subsidiaries in the UK.

Current understanding of the mechanisms for clearance of apoptotic cells-a fine balance

Apoptosis is an important cell death mechanism by which multicellular organisms remove unwanted cells. It culminates in a rapid, controlled removal of cell corpses by neighboring or recruited viable cells. Whilst many of the molecular mechanisms that mediate corpse clearance are components of the innate immune system, clearance of apoptotic cells is an anti-inflammatory process. Control of cell death is dependent on competing pro-apoptotic and anti-apoptotic signals. Evidence now suggests a similar balance of competing signals is central to the effective removal of cells, through so called 'eat me' and 'don't eat me' signals. Competing signals are also important for the controlled recruitment of phagocytes to sites of cell death. Consequently recruitment of phagocytes to and from sites of cell death can underlie the resolution or inappropriate propagation of cell death and inflammation. This article highlights our understanding of mechanisms mediating clearance of dying cells and discusses those mechanisms controlling phagocyte migration and how inappropriate control may promote important pathologies. © the authors, publisher and licensee libertas academica limited.

High-throughput manufacturing of size-tuned liposomes by a new microfluidics method using enhanced statistical tools for characterization

Microfluidics has recently emerged as a new method of manufacturing liposomes, which allows for reproducible mixing in miliseconds on the nanoliter scale. Here we investigate microfluidics-based manufacturing of liposomes. The aim of these studies was to assess the parameters in a microfluidic process by varying the total flow rate (TFR) and the flow rate ratio (FRR) of the solvent and aqueous phases. Design of experiment and multivariate data analysis were used for increased process understanding and development of predictive and correlative models. High FRR lead to the bottom-up synthesis of liposomes, with a strong correlation with vesicle size, demonstrating the ability to in-process control liposomes size; the resulting liposome size correlated with the FRR in the microfluidics process, with liposomes of 50 nm being reproducibly manufactured. Furthermore, we demonstrate the potential of a high throughput manufacturing of liposomes using microfluidics with a four-fold increase in the volumetric flow rate, maintaining liposome characteristics. The efficacy of these liposomes was demonstrated in transfection studies and was modelled using predictive modeling. Mathematical modelling identified FRR as the key variable in the microfluidic process, with the highest impact on liposome size, polydispersity and transfection efficiency. This study demonstrates microfluidics as a robust and high-throughput method for the scalable and highly reproducible manufacture of size-controlled liposomes. Furthermore, the application of statistically based process control increases understanding and allows for the generation of a design-space for controlled particle characteristics.

A high sensitivity long period grating Mach-Zehnder refractometer

A refractive index sensing system has been demonstrated, which is based upon an in-line fibre long period grating Mach-Zehnder interferometer with a heterodyne interrogation technique. This sensing system has comparable accuracy to laboratory-based techniques used in industry such as high performance liquid chromatography and UV spectroscopy. The advantage of this system is that measurements can be made in-situ for applications in continuous process control. Compared to other refractive index sensing schemes using LPGs, this approach has two main advantages. Firstly, the system relies on a simple optical interrogation system and therefore has the real potential for being low cost, and secondly, so far as we are aware it provides the highest refractive index resolution reported for any fibre LPG device.

Experiences on dynamic simulation software in chemical engineering education

Commercial process simulators are increasing interest in the chemical engineer education. In this paper, the use of commercial dynamic simulation software, D-SPICE® and K-Spice®, for three different chemical engineering courses is described and discussed. The courses cover the following topics: basic chemical engineering, operability and safety analysis and process control. User experiences from both teachers and students are presented. The benefits of dynamic simulation as an additional teaching tool are discussed and summarized. The experiences confirm that commercial dynamic simulators provide realistic training and can be successfully integrated into undergraduate and graduate teaching, laboratory courses and research. © 2012 The Institution of Chemical Engineers.

Direct observation of morphological development during the spin-coating of polystyrene-poly(methyl methacrylate) polymer blends

We present results of the direct observation, in real-space, of the phase separation of high molecular weight polystyrene and poly(methyl methacrylate) from ortho-xylene using our newly developed technique of high speed stroboscopic interference microscopy. Taking a fixed concentration (3 wt % in o-xylene) at a fixed composition (1:4 by weight) and by varying the rotational rate during the spin-coating process, we are able to observe the formation of a range of phase separated bicontinuous morphologies of differing length-scales. Importantly, we are able to show that the mechanism by which the final phase separated structure is formed is through domain coarsening when rich in solvent, before vitrification occurs and fixes the phase separated structure. The ability to directly observe morphological development offers a route toward controlling the length-scale of the final morphology through process control and in situ feedback, from a single stock solution. © 2013 Wiley Periodicals, Inc.

The effects of material variations in high value manufacturing industries

It has never been easy for manufacturing companies to understand their confidence level in terms of how accurate and to what degree of flexibility parts can be made. This brings uncertainty in finding the most suitable manufacturing method as well as in controlling their product and process verification systems. The aim of this research is to develop a system for capturing the company’s knowledge and expertise and then reflect it into an MRP (Manufacturing Resource Planning) system. A key activity here is measuring manufacturing and machining capabilities to a reasonable confidence level. For this purpose an in-line control measurement system is introduced to the company. Using SPC (Statistical Process Control) not only helps to predict the trend in manufacturing of parts but also minimises the human error in measurement. Gauge R&R (Repeatability and Reproducibility) study identifies problems in measurement systems. Measurement is like any other process in terms of variability. Reducing this variation via an automated machine probing system helps to avoid defects in future products.Developments in aerospace, nuclear, oil and gas industries demand materials with high performance and high temperature resistance under corrosive and oxidising environments. Superalloys were developed in the latter half of the 20th century as high strength materials for such purposes. For the same characteristics superalloys are considered as difficult-to-cut alloys when it comes to formation and machining. Furthermore due to the sensitivity of superalloy applications, in many cases they should be manufactured with tight tolerances. In addition superalloys, specifically Nickel based, have unique features such as low thermal conductivity due to having a high amount of Nickel in their material composition. This causes a high surface temperature on the work-piece at the machining stage which leads to deformation in the final product.Like every process, the material variations have a significant impact on machining quality. The main cause of variations can originate from chemical composition and mechanical hardness. The non-uniform distribution of metal elements is a major source of variation in metallurgical structures. Different heat treatment standards are designed for processing the material to the desired hardness levels based on application. In order to take corrective actions, a study on the material aspects of superalloys has been conducted. In this study samples from different batches of material have been analysed. This involved material preparation for microscopy analysis, and the effect of chemical compositions on hardness (before and after heat treatment). Some of the results are discussed and presented in this paper.

A dynamic feature information model for integrated manufacturing planning and optimization

This paper presents a new, dynamic feature representation method for high value parts consisting of complex and intersecting features. The method first extracts features from the CAD model of a complex part. Then the dynamic status of each feature is established between various operations to be carried out during the whole manufacturing process. Each manufacturing and verification operation can be planned and optimized using the real conditions of a feature, thus enhancing accuracy, traceability and process control. The dynamic feature representation is complementary to the design models used as underlining basis in current CAD/CAM and decision support systems. © 2012 CIRP.

Nanotechnology and microfluidics:formulation design and on-chip manufacture of nanoparticles

Nanoparticles offer an ideal platform for the delivery of small molecule drugs, subunit vaccines and genetic constructs. Besides the necessity of a homogenous size distribution, defined loading efficiencies and reasonable production and development costs, one of the major bottlenecks in translating nanoparticles into clinical application is the need for rapid, robust and reproducible development techniques. Within this thesis, microfluidic methods were investigated for the manufacturing, drug or protein loading and purification of pharmaceutically relevant nanoparticles. Initially, methods to prepare small liposomes were evaluated and compared to a microfluidics-directed nanoprecipitation method. To support the implementation of statistical process control, design of experiment models aided the process robustness and validation for the methods investigated and gave an initial overview of the size ranges obtainable in each method whilst evaluating advantages and disadvantages of each method. The lab-on-a-chip system resulted in a high-throughput vesicle manufacturing, enabling a rapid process and a high degree of process control. To further investigate this method, cationic low transition temperature lipids, cationic bola-amphiphiles with delocalized charge centers, neutral lipids and polymers were used in the microfluidics-directed nanoprecipitation method to formulate vesicles. Whereas the total flow rate (TFR) and the ratio of solvent to aqueous stream (flow rate ratio, FRR) was shown to be influential for controlling the vesicle size in high transition temperature lipids, the factor FRR was found the most influential factor controlling the size of vesicles consisting of low transition temperature lipids and polymer-based nanoparticles. The biological activity of the resulting constructs was confirmed by an invitro transfection of pDNA constructs using cationic nanoprecipitated vesicles. Design of experiments and multivariate data analysis revealed the mathematical relationship and significance of the factors TFR and FRR in the microfluidics process to the liposome size, polydispersity and transfection efficiency. Multivariate tools were used to cluster and predict specific in-vivo immune responses dependent on key liposome adjuvant characteristics upon delivery a tuberculosis antigen in a vaccine candidate. The addition of a low solubility model drug (propofol) in the nanoprecipitation method resulted in a significantly higher solubilisation of the drug within the liposomal bilayer, compared to the control method. The microfluidics method underwent scale-up work by increasing the channel diameter and parallelisation of the mixers in a planar way, resulting in an overall 40-fold increase in throughput. Furthermore, microfluidic tools were developed based on a microfluidics-directed tangential flow filtration, which allowed for a continuous manufacturing, purification and concentration of liposomal drug products.

Development of surface flaw thresholds for pre-cured fiber reinforced polymer and groove size tolerance for near surface mounted fiber reinforced polymer retrofit systems

Since the introduction of fiber reinforced polymers (FRP) for the repair and retrofit of concrete structures in the 1980’s, considerable research has been devoted to the feasibility of their application and predictive modeling of their performance. However, the effects of flaws present in the constitutive components and the practices in substrate preparation and treatment have not yet been thoroughly studied. This research aims at investigating the effect of surface preparation and treatment for the pre-cured FRP systems and the groove size tolerance for near surface mounted (NSM) FRP systems; and to set thresholds for guaranteed system performance. This study was conducted as part of the National Cooperative Highway Research Program (NCHRP) Project 10-59B to develop construction specifications and process control manual for repair and retrofit of concrete structures using bonded FRP systems. The research included both analytical and experimental components. The experimental program for the pre-cured FRP systems consisted of a total of twenty-four (24) reinforced concrete (RC) T-beams with various surface preparation parameters and surface flaws, including roughness, flatness, voids and cracks (cuts). For the NSM FRP systems, a total of twelve (12) additional RC T-beams were tested with different grooves sizes for FRP bars and strips. The analytical program included developing an elaborate nonlinear finite element model using the general purpose software ANSYS. The bond interface between FRP and concrete was modeled by a series of nonlinear springs. The model was validated against test data from the present study as well as those available from the literature. The model was subsequently used to extend the experimental range of parameters for surface flatness in pre-cured FRP systems and for groove size study in the NSM FRP systems. Test results, confirmed by further analyses, indicated that contrary to the general belief in the industry, the impact of surface roughness on the global performance of pre-cured FRP systems was negligible. The study also verified that threshold limits set for wet lay-up FRP systems can be extended to pre-cured systems. The study showed that larger surface voids and cracks (cuts) can adversely impact both the strength and ductility of pre-cured FRP systems. On the other hand, frequency (or spacing) of surface cracks (cuts) may only affect system ductility rather than its strength. Finally, within the range studied, groove size tolerance of ±1/8 in. does not appear to have an adverse effect on the performance of NSM FRP systems.

Modelação e análise de um sistema flexível de produção

A modelação dos sistemas industriais apresenta para as organizações uma vantagem estratégica no domínio do estudo dos seus processos produtivos. Através da modelação será possível aumentar o conhecimento sobre os sistemas podendo permitir, quando possível, melhorias na gestão e planeamento da produção. Este conhecimento poderá permitir também um aumento da eficiência dos processos produtivos, através da melhoria ou eliminação das principais perdas detetadas no processo. Este trabalho tem como principal objetivo o desenvolvimento e validação de uma ferramenta de modelação, previsão e análise para sistemas produtivos industriais, tendo em vista o aumento do conhecimento sobre estes. Para a execução e desenvolvimento deste trabalho, foram utilizadas e desenvolvidas várias ferramentas, conceitos, metodologias e fundamentos teóricos conhecidos da bibliografia, como OEE (Overall Equipment Effectiveness), RdP (Redes de Petri), Séries Temporais, Kmeans, ou SPC (Statistical Process Control). A ferramenta de modelação, previsão e análise desenvolvida e descrita neste trabalho, mostrou-se capaz de auxiliar na deteção e interpretação das causas que influenciam os resultados do sistema produtivo e originam perdas, demonstrando as vantagens esperadas. Estes resultados foram baseados em dados reais de um sistema produtivo.

Guideline-based decision support has a small, non-sustained effect on transthoracic echocardiography ordering frequency.

BACKGROUND: Guidance for appropriate utilisation of transthoracic echocardiograms (TTEs) can be incorporated into ordering prompts, potentially affecting the number of requests. METHODS: We incorporated data from the 2011 Appropriate Use Criteria for Echocardiography, the 2010 National Institute for Clinical Excellence Guideline on Chronic Heart Failure, and American College of Cardiology Choosing Wisely list on TTE use for dyspnoea, oedema and valvular disease into electronic ordering systems at Durham Veterans Affairs Medical Center. Our primary outcome was TTE orders per month. Secondary outcomes included rates of outpatient TTE ordering per 100 visits and frequency of brain natriuretic peptide (BNP) ordering prior to TTE. Outcomes were measured for 20 months before and 12 months after the intervention. RESULTS: The number of TTEs ordered did not decrease (338±32 TTEs/month prior vs 320±33 afterwards, p=0.12). Rates of outpatient TTE ordering decreased minimally post intervention (2.28 per 100 primary care/cardiology visits prior vs 1.99 afterwards, p<0.01). Effects on TTE ordering and ordering rate significantly interacted with time from intervention (p<0.02 for both), as the small initial effects waned after 6 months. The percentage of TTE orders with preceding BNP increased (36.5% prior vs 42.2% after for inpatients, p=0.01; 10.8% prior vs 14.5% after for outpatients, p<0.01). CONCLUSIONS: Ordering prompts for TTEs initially minimally reduced the number of TTEs ordered and increased BNP measurement at a single institution, but the effect on TTEs ordered was likely insignificant from a utilisation standpoint and decayed over time.

Sensemaking, safety, and situated communities in (con)temporary networks

This paper discusses the difficulties involved in managing knowledge-intensive, multinational, multiorganisational, and multifunctional project networks. The study is based on a 2-year quasi-ethnography of one such network engaged in the design and development of a complex new process control system for an existing pharmaceutical plant in Ireland. The case describes how, drawing upon the organisational heritage of the corporations involved and the logic implicit within their global partnership arrangements, the project was initially structured in an aspatial manner that underestimated the complexity of the development process and the social relations required to support it. Following dissatisfaction with initial progress, a number of critical management interventions were made, which appeared to contribute to a recasting of the network ontology that facilitated the cultivation and protection of more appropriate communicative spaces. The case emphasises the need to move away from rationalistic assumptions about communication processes within projects of this nature, towards a richer conceptualisation of such enterprises as involving collective sensemaking activities within and between situated ‘communities’ of actors. Contrary to much contemporary writing, the paper argues that space and location are of crucial importance to our understanding of network forms of organising.