Study of mechanical response in embossing of ceramic green substrate by micro-indentation

Micro-indentation test with a micro flat-end cone indenter was employed to simulate micro embossing process and investigate the thermo-mechanical response of ceramic green substrates. The laminated low temperature co-fired ceramic green tapes were used as the testing material ; the correlations of indentation depth versus applied force and applied stress at the temperatures of 25 degrees C and 75degrees C were studied. The results showed that permanent indentation cavities could be formed at temperatures ranging from 25 degrees C to 75 degrees C, and the depth of cavities created was applied force, temperature and dwell time dependent. Creep occurred and made a larger contribution to the plastic deformation at elevated temperatures and high peak loads. There was instantaneous recovery during the unloading and retarded recovery in the first day after indentation. There was no significant pile-up due to material flow observed under compression at the temperature up to 75 degrees C. The plastic deformation was the main cause for formation of cavity on the ceramic green substrate under compression. The results can be used as a guideline for embossing ceramic green substrates.Comment: Submitted on behalf of EDA Publishing Association (http://irevues.inist.fr/handle/2042/16838

Large Area Roller Embossing of Multilayered Ceramic Green Composites

In this paper, we will report our achievements in developing large area patterning of multilayered ceramic green composites using roller embossing. The aim of our research is to pattern large area ceramic green composites using a modified roller laminating apparatus, which is compatible with screen printing machines, for integration of embossing and screen printing. The instrumentation of our roller embossing apparatus, as shown in Figure1, consists of roller 1 and rollers 2. Roller 1 is heated up to the desired embossing temperature ; roller 2 is, however, kept at room temperature. The mould is a nickel template manufactured by plating nickel-based micro patterns (height : 50 $\mu$m) on a nickel film (thickness : 70 $\mu$m) ; the substrate for the roller embossing is a multilayered Heraeus Heralock HL 2000 ceramic green composite. Comparing with the conventional simultaneous embossing, the advantages of roller embossing include : (1) low embossing force ; (2) easiness of demoulding ; (3) localized area in contact with heater ; and etc. We have demonstrated the capability of large area roller embossing with a panel size of 150mmx 150mm on the mentioned substrate. We have explored and confirmed the impact of parameters (feed speed, temperature of roller and applied pressure) to the pattern quality of roller embossing. Furthermore, under the optimized process parameters, we characterized the variations of pattern dimension over the panel area, and calculated a scaling factor in order to make the panel compatible with other processes. Figure 2 shows the embossed patterns on a 150mmx 150mm green ceramic panel.Comment: Submitted on behalf of EDA Publishing Association (http://irevues.inist.fr/handle/2042/16838

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

Fabrication of Micro Pillar Arrays Via Aerosol Jet Printing

Direct write printing is one of the evolving technologies that can be used to fabricate 3D structures such as ceramic micro-pillars. Direct write printing processes can print high resolution structures in the micron or sub-micron range. These structures find their applications in 3D Micro-Electro Mechanical Systems (MEMS), ultra-sound and thermal imaging, heat exchangers and solid oxide fuel cells. The present research is focused on fabrication of vertical ceramic micro-pillars using the Aerosol Jet direct write printing process for enhancing the aspect ratio of the pillars. Aerosol Jet printing offers flexibility with respect to ink compositions as compared with fabrication techniques such as lithography or ink-jet printing. This study includes an investigation of ink compositions to formulate a printable Yttria Stabilized Zirconia (YSZ) ink. YSZ ceramic is chosen due to its wide range of applications. The effect of solid loading fraction on the viscosity of ink is also studied. The study identifies significant printing process parameters and their relationships to the process output for printing high aspect ratio YSZ micro-pillars. An experimental approach is followed where the diameter and height of pillars are the response variables of interest. A screening experiment with fractional factorial model is conducted in order to obtain the levels of process parameters that resulted in pillars with diameters as small as 50 µm and heights up to 1000 µm. After finding suitable process parameter levels, experiments were conducted to identify the minimum distance between consecutive pillars. Once the minimum possible distance was identified, 4x4 pillar arrays were printed on YSZ substrate and sintered in order to achieve sufficient pillar strength. Pillars with average diameters as small as 50 µm and heights up to 1000µm were achieved through this process

Novel patterning technology for the LTCC based packaging of an optical encoder

Powder blasting technology is proposed in this thesis as a new structuring tool for Low Temperature Co-fired Ceramic (LTCC). The process, consisting of mechanical abrasion through high speed particles, is mostly used on brittle material but was successfully adapted for the patterning of microstructures onto the fragile green tape substrate, through the manufacturing of novel stencil masks. These masks are based on high resolution patterned nickel sheet produced using UV-LIGA process or laser cutting coated with a thin layer of photopolymer which prevents efficiently the metal sheet deformations under particles bombardment. The magnetic properties of the metal allowed magnetic clamping to be used to maintain the mask down onto the substrate. The etching rate of the metal was shown to be low enough at a pressure of 50 psi (344kPa) at a distance nozzle-substrate (N-S) of 20mm and 50mm so that the mask could be re-used several times and ensured good pattern transfer quality from the mask to the substrate. The process was systematically characterised on DuPont 951 P2 (~165μm thick) green tapes. The erosion of the green tape ceramic was then characterised with the micro-patterned electroplated masks. It showed that the powder blasted structures had U shape walls and verticality of the walls closed to 90o can be obtained with increasing the number of passes. The structures have smooth edges and do not have any melting parts. Smoother structures were obtained with distance nozzle-substrate of 50mm favouring lower under etching of about 15-20μm at the expense of a three times increase in process duration. Vias as small as 62μm in entry diameter and 20μm exit diameter were produced along with beams 25μm top width and 54μm bottom width were produced. Following the green tape characterisation, a LTCC package for an optical encoder featuring 16 layers with the glass cavity was manufactured. 45x45mm nickel masks coated with LF55gn flexopolymer were produced featuring stacking pins, fiducials, cavities and circular apertures ranging from 100μm to 400μm diameters for interconnections. Each mask was powder blasted at 50 psi for a flow rate of about 0.1g/s, a distance N-S of 20mm and a speed of 5mm/s. The optical encoder was successfully attached on the package and tested

DIRECT PATTERNING OF NATURE-INSPIRED SURFACES FOR BIOINTERFACIAL APPLICATIONS

There are three major challenges for the design of patterned surfaces for biointerfacial applications: (i) durability of antibacterial/antifouling mechanisms, (ii) mechanical durability, and (iii) lifetime of the master mold for mass production of patterned surfaces. In this dissertation, we describe our contribution for the development of each of these challenges. The bioinspired surface, Sharklet AFTM, has been shown to reduce bacterial attachment via a biocide-free structure-property relationship effectively. Unfortunately, the effectiveness of polymer-based sharkskin surfaces is challenged over the long term by both eventual bacteria accumulation and a lack of mechanical durability. To address these common modes of failure, hard, multifunctional, antifouling, and antibacterial shark-skin patterned surfaces were fabricated via a solvent-assisted imprint patterning technique. A UV-crosslinkable adhesive material was loaded with titanium dioxide (TiO2)nanoparticles (NPs) from which shark skin microstructures were imprinted on a polyethylene terephthalate substrate. Furthermore, hard, multifunctional, antifouling, and antibacterial shark skin patterned surfaces were fabricated using inks comprised of zirconium dioxide (ZrO2) NPs and TiO2 NPs. The ZrO2 NPs provide an extremely hard and durable matrix in the final structure, while the TiO2 NPs provide active antibacterial functionality in the presence of UV light via photooxidation. The dynamic water contact angle, mechanical, antibacterial, and antifouling characteristics of the shark skin patterned surfaces were investigated as a function of TiO2 content. We then demonstrated the multifunctional shark skin system’s suitability for use as an antifouling biosensor. Lastly, we described the design of a durable, hard master mold for pattern transfer. The lifetime of many of the current molds is limited by a lack of mechanical durability as well as cost. In this study, ZrO2 NPs were imprinted on a variety of substrates using a solvent-assisted patterning technique and subsequently annealed to increase the mechanical durability of the mold. Polymer replications were demonstrated using the hard ZrO2 mold with thermal and UV nanoimprinting lithography techniques, and injection molding. After up to 115,000 injection molding cycles, there was no delamination or breakage in the ZrO2 mold. The high hardness and durability, as demonstrated through the many replication cycles, suggests that the ZrO2 mold has excellent potential for use in the mass production of patterned polymer replicas. We also explored the nanopatterning of stainless steel using the ZrO2 mold. The solution-processability and simple patterning technique of ZrO2 NPs enable large-area and cost-effective fabrication of the hard molds which can be used for the variety of nano and micro-replication technologies

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)

Overview of Materials for Microfluidic Applications

For each material dedicated to microfluidic applications, inherent microfabrication and specific physico‐chemical properties are key concerns and play a dominating role in further microfluidic operability. From the first generation of inorganic glass, silicon and ceramics microfluidic devices materials, to diversely competitive polymers alternatives such as soft and rigid thermoset and thermoplastics materials, to finally various paper, biodegradable and hydrogel materials; this chapter will review their advantages and drawbacks regarding their microfabrication perspectives at both research and industrial scale. The chapter will also address, the evolution of the materials used for fabricating microfluidic chips, and will discuss the application‐oriented pros and cons regarding especially their critical strategies and properties for devices assembly and biocompatibility, as well their potential for downstream biochemical surface modification are presented

Effect of micro-patterning on bacterial adhesion on polyethylene terephthalate surface.

Bacterial adhesion on surfaces commonly used in medicine and food industry could lead to infections and illnesses. Topographically patterned surfaces recently have shown to be a promising alternative to chemical antibacterial methods, which might release cytotoxin and promote antibiotic resistance. In this study, we fabricated micro-patterned polyethylene terephthalate surfaces, and quantitatively explored the amount and localization of Escherichia coli MG1655 cells attached on a series of defined topographies. The adhesion was conducted in static conditions and under a weak flow, in both physiological buffer and nutritious solutions. The results showed that in the presence of weak shear force, live bacteria could still maintain sensing ability in nutritious culture, but not in buffer solution. The finely textured surface, which could inhibit bacterial adhesion in the early stage of attachment, reversed its effect to enhance the adhesion after 24 h incubation, indicating that microbial cells seemed to be able to sense the disadvantageous condition and eventually overcome it. In terms of adhesion localization, bacteria exhibited preferential adhesion onto the edges of topographic features. The patterned substrates that have the most even (homogeneous) bacterial localization on topographic features retained the least attachment after 24 h exposure.Financial support from China Scholarship Council and Unilever Corporate Research is acknowledged.This is the accepted manuscript. The final version is available from Sage at http://jba.sagepub.com/content/early/2014/12/16/0885328214563998.refs