Optimization of fluidic microchannel manufacturing processes in low temperature co-fired ceramic substrates

The processing of starch powder and polymer based sacrificial layer for fabrication of microfluidic structures in low temperature co-fired ceramics (LTCC) is described in the paper. Sacrificial volume material (SVM) was placed into the channel of LTCC sheets to avoid sagging by supporting embedded, three-dimensional structures such as channels, cavities during firing. Sagging of laminated structures is a common problem in the processing of the LTCC. A series of experiments were carried out for different lamination schemes which affect the quality of LTCC sheets. Samples were tested by an acoustic microscope to reveal the internal inhomogeneities and delaminations. As a consequence of burnout, the increased fraction of evolving gases from SVM requires an adequate adaptation of the firing process to provide a residue-free burnout without damaging the structure. Using thermal analysis the intensity of the evaporating gases was determined during co-firing. Based on these results, the modification of the heating p rofile could be done. It is proposed that the fabrication of embedded structures in a multi-layer LTCC platform could be achieved by controlling SVM burnout with a modified heating profile. Using this approach, fabrication of embedded channels in LTCC substrate is demonstrated

Structuration of the low temperature co-fired ceramics (LTCC) using novel sacrificial graphite paste with PVA–propylene glycol–glycerol–water vehicle

A novel formulation for thick-film graphite sacrificial pastes is studied in this paper. It is composed of coarse graphite powder (grain size: 25 μm), dispersed in a vehicle consisting of polyvinyl alcohol (PVA) dissolved in a propylene glycol (PG)–glycerol (G)–water mix, which is not aggressive to thin LTCC sheets. The presented sacrificial paste has been successfully applied for fabrication of thin (<50 μm) membranes and microchannels in low temperature co-fired ceramics (LTCC) substrate. The properties of the graphite-based paste have been examined using thermo-gravimetric analysis (TGA), differential thermo-gravimetric (DTG) and differential thermal analysis (DTA). The obtained membranes and microchannels have been investigated using scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and optical profile measurements gauge

Diode laser modules based on laser-machined, multi-layer ceramic substrates with integrated water cooling and micro-optics

This thesis presents a study on the use of low temperature co-fired ceramic (LTCC) material as a new platform for the packaging of multiple broad area single emitter diode lasers. This will address the recent trend in the laser industry of combining multiple laser diodes in a common package to reach the beam brightness and power required for pumping fibre lasers and for direct-diode industrial applications, such as welding, cutting, and etching. Packages based on multiple single emitters offer advantages over those derived from monolithic diode bars such as higher brightness, negligible thermal crosstalk between neighbouring emitters and protection against cascading failed emitters. In addition, insulated sub-mounted laser diodes based on telecommunication standards are preferred to diode bars and stacks because of the degree of assembly automation, and improved lifetime. At present, lasers are packaged on Cu or CuW platforms, whose high thermal conductivities allow an efficient passive cooling. However, as the number of emitters per package increases and improvements in the laser technology enable higher output power, the passive cooling will become insufficient. To overcome this problem, a LTCC platform capable of actively removing the heat generated by the lasers through impingement jet cooling was developed. It was provided with an internal water manifold capable to impinge water at 0.15 lmin-1 flow rate on the back surface of each laser with a variation of less than 2 °C in the temperature between the diodes. The thermal impedance of 2.7°C/W obtained allows the LTCC structure to cool the latest commercial broad area single emitter diode lasers which deliver up to 13 W of optical power. Commonly, the emitters are placed in a “staircase” formation to stack the emitters in the fast-axis, maintaining the brightness of the diode lasers. However, due to technical difficulties of machining the LTCC structure with a staircase-shaped face, a novel out-plane beam shaping method was proposed to obtain an elegant and compact free space combination of the laser beam on board using inexpensive optics. A compact arrangement was obtained using aligned folding mirrors, which stacked the beams on top of each other in the fast direction with the minimum dead space

Metallisation and structuring of low temperature Co-fired ceramic for micro and millimetre wave applications

The recent developments in Low Temperature Co-fired Ceramic (LTCC) as a substrate material enable it to be used in the micro and millimetre wave range providing low dissipation factors at high frequencies, good dielectric properties and a high degree of integration for further miniaturised devices. The most common metallisation method used in LTCC technology is screen printing with high cost noble metals such as silver and gold that are compatible with the high sintering temperatures (8500C). However, these techniques require high capital cost and maintenance cost. As the commercial world requires convenient and low cost process technologies for mass production, alternative metallisation methods should be considered. As a result, electroless copper plating of fired LTCC was mainly investigated in this research. The main goals of this project were to carry out electroless plating of fired LTCC with sufficient adhesion and to extend the process to metallise closed LTCC channel structures to manufacture Substrate Integrated Waveguide (SIW) components. The objectives were focused on electroless copper deposition on fired LTCC with improved adhesion. Electroless deposits on the Sn/Pd activated LTCC surface showed poor adhesion without any surface pre-treatments. Hence, chemical etching of fired LTCC was carried out using concentrated NaOH solution. NaOH pre-treatment of LTCC led to the formation of flake like structures on the LTCC surface. A number of surface and chemical analysis techniques and weight measurements were used to investigate the mechanism of the modification of the LTCC surface. The results showed that the flake like structures were dispersed in the LTCC material and a material model for the LTCC structure was proposed. SEM EDX elemental mapping showed that the flake like structure consisted of aluminium, calcium, boron and oxygen. Further experiments showed that both the concentration of NaOH and the immersion time affect the surface morphology and the roughness of fired LTCC. The measured Ra values were 0.6 m for untreated LTCC and 1.1 m for the LTCC sample treated with 4M NaOH for 270 minutes. Adhesion tests including peel test and scratch test were carried out to examine the adhesion strength of the deposited copper and both tests indicated that the NaOH pre-treatment led to an improvement, with the best results achieved for samples treated with 4M NaOH. A second aspect of the research focused on the selective metallisation of fired LTCC. Excimer laser machining was used to pattern a resist film laminated on the LTCC surface. This process also roughened the substrate and created channels that were characterised with respect to the laser operating parameters. After patterning the resist layer, samples were activated using Sn/Pd catalyst solution followed by the electroless copper deposition. Electroless copper was selectively deposited only on the patterned LTCC surface. Laser parameters clearly affected the copper plating rate. Even with a similar number of shots per area, the tracks machined with higher repetition rate showed relatively more machining depth as well as good plating conditions with low resistance values. The process was further implemented to realize a complete working circuit on fired LTCC. Passive components including a capacitor and an inductor were also fabricated on LTCC using the mask projection technique of the excimer laser system. This was successful for many designs, but when the separation between conductor lines dropped below 18 m, electroless copper started to deposit on the areas between them. Finally, a method to deposit copper films on the internal walls of closed channel structures was developed. The method was first demonstrated by flowing electroless copper solutions through silane treated glass capillaries. A thin layer (approx. 60 nm) of electroless copper was deposited only on the internal walls of the glass capillaries. The flow rate of the electroless copper solution had to be maintained at a low level as the copper deposits tended to wash away with higher flow rates. The structures were tested for transmission losses and showed low (<10dB) transmission losses in the terahertz region of the electromagnetic spectrum. The process was further applied to deposit electroless copper on the internal walls of the LTCC closed channel structures to manufacture a LTCC Substrate Integrated Waveguide (SIW)

Electrochemical Immunosensing of Cortisol in an Automated Microfluidic System Towards Point-of-Care Applications

This dissertation describes the development of a label-free, electrochemical immunosensing platform integrated into a low-cost microfluidic system for the sensitive, selective and accurate detection of cortisol, a steroid hormone co-related with many physiological disorders. Abnormal levels of cortisol is indicative of conditions such as Cushing’s syndrome, Addison’s disease, adrenal insufficiencies and more recently post-traumatic stress disorder (PTSD). Electrochemical detection of immuno-complex formation is utilized for the sensitive detection of Cortisol using Anti-Cortisol antibodies immobilized on sensing electrodes. Electrochemical detection techniques such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) have been utilized for the characterization and sensing of the label-free detection of Cortisol. The utilization of nanomaterial’s as the immobilizing matrix for Anti-cortisol antibodies that leads to improved sensor response has been explored. A hybrid nano-composite of Polyanaline-Ag/AgO film has been fabricated onto Au substrate using electrophoretic deposition for the preparation of electrochemical immunosening of cortisol. Using a conventional 3-electrode electrochemical cell, a linear sensing range of 1pM to 1µM at a sensitivity of 66µA/M and detection limit of 0.64pg/mL has been demonstrated for detection of cortisol. Alternately, a self-assembled monolayer (SAM) of dithiobis(succinimidylpropionte) (DTSP) has been fabricated for the modification of sensing electrode to immobilize with Anti-Cortisol antibodies. To increase the sensitivity at lower detection limit and to develop a point-of-care sensing platform, the DTSP-SAM has been fabricated on micromachined interdigitated microelectrodes (µIDE). Detection of cortisol is demonstrated at a sensitivity of 20.7µA/M and detection limit of 10pg/mL for a linear sensing range of 10pM to 200nM using the µIDE’s. A simple, low-cost microfluidic system is designed using low-temperature co-fired ceramics (LTCC) technology for the integration of the electrochemical cortisol immunosensor and automation of the immunoassay. For the first time, the non-specific adsorption of analyte on LTCC has been characterized for microfluidic applications. The design, fabrication technique and fluidic characterization of the immunoassay are presented. The DTSP-SAM based electrochemical immunosensor on µIDE is integrated into the LTCC microfluidic system and cortisol detection is achieved in the microfluidic system in a fully automated assay. The fully automated microfluidic immunosensor hold great promise for accurate, sensitive detection of cortisol in point-of-care applications

Fabrication and Characterization of Miniaturized Components Based on Extruded Ceramic-Filled Polymer Blends

The objective of this work is to develop an improved manufacturing process for microstructured ceramic components that is based on co-extrusion. Co-extrusion of structured feedrods holds promise for development of multi-layered, functionally graded and/or textured structures. However, it requires a polymer binder that is difficult to remove before structures can be sintered to full density. A two-step debinding is introduced to eliminate debinding defects that are commonly observed in thermal debinding (TD). Cracking is a major issue due to a lack of pore spaces for outgassing of pyrolysis products in traditional TD. In two-step debinding, a soluble binder is removed partially by solvent extraction (SE) which creates a porous network and allows gases to escape in subsequent TD of remaining binder components. The feasibility of solvent extraction (SE) is documented for the extrusion of solid ceramic rods and co-extrusion of tubes, where alumina powder was batched with polyethylene butyl acrylate (PEBA) as backbone polymer and polyethylene glycol (PEG) as water soluble binder. SE for specimens with varying PEBA:PEG ratios were tested in water at three different temperatures for various times. Experiments were also performed with different grades of PEBA and EVA to investigate the effect of thermoplastics on SE. The 1:1 mixture showed a PEG removal up to 80wt.% of the original PEG content after 6h extraction. After subsequent thermal debinding, rods and tubes were sintered successfully without defects, demonstrating the viability of the process. Scanning electron microscopy and optical analysis were performed to characterize the process. In order to illustrate potential applications, microfluidic devices were manufactured using extrusion followed by hot embossing. Ceramic microfabricated components have advantages over silicon, glass or polymer devices in terms of their ability to sustain high temperatures without compromising their functional capabilities. Flat tapes were extruded to create substrates, which were subsequently embossing micro patterns using a brass metal mold. To seal the microchanneled feature, a glass slide was attached to the chip by thermal bonding. Though a good bond was obtained, small portions were found where poor bonding was observed. To check leakage, colored water was forced to flow through the channel,and no leakage of water was found. A low temperature sintered ceramic material was fabricated as a potential alternative to the commercial low temperature co-fired ceramic (LTCC) tape. Overall, the study describes new possibilities for microstructure fabrication on ceramic based substrate and established the embossing process as a promising technique for fabrication

E-plane parallel coupled resonators for waveguide bandpass filter applications

High skirt selectivity and extended out-of-band rejection is a major challenge for the successful progress of in-line microwave filters. This thesis presents novel filter realizations with improved performance, compatible with the standard single thin all-metal insert in a split-block housing and therefore maintaining the low-cost fabrication characteristics. In addition, significant filter performance improvement is achieved. The synthesis procedure implemented for the filter concept consists of a few steps. Some preliminary steps are a rigorous characterization of a double-ridge coaxial waveguide, and the modelling of an equivalent circuit model for the parallel coupled ridge waveguide devised in the filter concept. From these elements, a full wave electromagnetic analysis shows that parallel-coupled asymmetric ridge waveguides produce strongly dispersive coupling which introduces a transmission zero. Later on this property is extended to parallel-coupled asymmetric ridge waveguide resonators, where it is demonstrated that it is possible to independently control the coupling coefficient and the frequency of the transmission zero. This allows the realization of pseudo-elliptic narrowband in-line bandpass filters in E-plane technology. A general synthesis procedure for high order filters is outlined and numerical and experimental results are presented for validation. The elements employed for the synthesis procedure of the bandpass prototypes are also applied to investigate structures suitable for different applications. In particular, stopband and dual stopband filters are presented with numerical and experimental results. Finally, the study of a microwave chemical/biochemical sensing device for the characterization and detection of cells in chemical substances and cells in solution in micro-litre volumes is also reported.Engineering and Physical Sciences Research Council(EPSRC

3D Structuration Techniques of LTCC for Microsystems Applications

This thesis aimed at developing new 3D structuration techniques for a relatively recent new ceramic technology called LTCC, which stands for Low Temperature, Co-fired Ceramic. It is a material originally developed for the microelectronic packaging industry; its chemical and thermal stabilities make it suitable to military-grade and automotive applications, such as car ignition systems and Wi-Fi antennae (GHz frequencies). In recent years however, the research in ceramic microsystems has seen a growing interest for microfluidics, packaging, MEMS and sensors. Positioned at the crossing of classical thick-film technology on alumina substrate and of high temperature ceramics, this new kind of easily structurable ceramic is filling the technological and dimensional gap between microsystems in Silicon and classical "macro microsystems", in the sense that we can now structure microdevices in the range from 150 mm to 150 mm. In effect, LTCC technology allows printing conductors and other inks from 30 mm to many mm, structuration from 150 mm to 150 mm, and suspended structures with gaps down to 30 mm thanks to sacrificial materials. Sensors and their packaging are now merged in what we can call "functional packaging". The contributions of this thesis lie both in the technological aspects we brought, and in the innovative microfluidic sensors and devices created using our developed methods. These realizations would not have been possible with the standard lamination and firing techniques used so far. Hence, we allow circumventing the problems related to microfluidics circuitry: for instance, the difficulty to control final fired dimensions, the burden to produce cavities or open structures and the associated delaminations of tapes, and the absence of "recipe" for the industrialization of fluidic devices. The achievements of the presented research can be summarized as follows: The control of final dimensions is mastered after having studied the influence of lamination parameters, proving they have a considerable impact. It is now possible to have a set of design rules for a given material, deviating from suppliers' recommendations for the manufacture of slender structures requiring reduced lamination. A new lamination method was set up, permitting the assembly of complex microfluidic circuits that would normally not sustain standard lamination. The method is based on partial pseudo-isostatic sub-laminations, with the help of a constrained rubber, subsequently consolidated together with a final standard uniaxial lamination. The conflict between well bonded tapes and acceptable output geometry is greatly attenuated. We achieved the formulation of a new class of Sacrificial Volume Materials (SVM) to allow the fabrication of open structures on LTCC and on standard alumina substrates; these are indeed screen-printable inks made by mixing together mineral compounds, a glassy phase and experimental organic binders. This is an appreciable improvement over the so-far existing SVMs for LTCC, limited to closed structures such as thin membranes. An innovative industrial-grade potentially low-cost diagnostics multisensor for the pneumatic industry was developed, allowing the measurement of compressed air pressure, flow and temperature. The device is entirely mounted by soldering onto an electro-fluidic platform, de facto making it a true electro-fluidic SMD component in itself. It comprises additionally its own integrated SMD electronics, and thanks to standard hybrid assembly techniques, gets rid of external wires and tubings – this prowess was never achieved before. This opens the way for in situ diagnostics of industrial systems through the use of low-cost integrated sensors that directly output conditioned signals. In addition to the abovementioned developments, we propose an extensive review of existing Sacrificial Volume Materials, and we present numerous applications of LTCC to sensors and microsystems, such as capacitive microforce sensors, a chemical microreactor and microthrusters. In conclusion, LTCC is a technology adapted to the industrial production of microfluidic sensors and devices: the fabrication steps are all industrializable, with an easy transition from prototyping to mass production. Nonetheless, the structuration of channels, cavities and membranes obey complex rules; it is for the moment not yet possible to choose with accuracy the right manufacturing parameters without testing. Consequently, thorough engineering and mastering of the know-how of the whole manufacturing process is still necessary to produce efficient LTCC electro-fluidic circuits, in contrast with older techniques such as classical thick-film technology on alumina substrates or PCBs in FR-4. Notwithstanding its lack of maturity, the still young LTCC technology is promising in both the microelectronics and microfluidics domains. Engineers have a better understanding of the structuration possibilities, of the implications of lamination, and of the most common problems; they have now all the tools in hand to create complex microfluidics circuits