Status of laminar grating manufacturing via lithography at HZB

In 2009 Carl Zeiss stopped the manufacture of precision gratings. All users of precision gratings were very concerned about this decision, since they all need such gratings for their experiments. One of the institutes of the HZB, the Institute for Nanometer Optics and Technology (INT), has extensive experience in micro fabrication (technology group). In spring 2010, HZB decided to take over the old C. Zeiss grating fabrication and build up its own technology center for grating fabrication. Using governmental support, HZB has installed all necessary equipment and processes to fabricate high quality gratings for the synchrotron radiation community.     

A Monte Carlo study of the primary absorbed energy redistribution in X-ray lithography

The minimum feature size producible by LIGA X-ray lithography is fundamentally limited by the redistribution of primary doses via photoelectrons and the influence of the resulting dose distribution on resist development. Secondary radiation from mask and substrate are well known as source for pattern distortion in deep X-ray lithography. Numerical simulations by means of Monte Carlo simulations using PENELOPE (Salvat et al. in PENELOPE-2008: a code system for Monte Carlo simulation of electron and photon transport. http://www.nea.fr/html/dbprog/penelope-2008.pdf, 2008) are applied to quantify these additional dose values in the resist/substrate interface and the irradiated/shadowed interface. A significant reduction of the additional dose by secondary radiation from the plating base is not observed for Au and Ti layers thicker than 10 nm. The influence of polarized or unpolarized X-rays might be neglected for structure dimensions larger than a few 10 nm. As an example of critical dimension, simulations were used to predict the structure quality of grating structures with a period of 2.4 μm and duty cycle 0.5 in a resist layer of 300 μm.     

Resist evaluation for proton beam writing,Ni mold fabrication and nano-replication

Proton beam writing (PBW) is a new direct-write technique which has shown great potential to fabricate structures down to 20 nm level in resist material. Protons can be accelerated up to a high energy (3.5 MeV) at Centre for Ion Beam Applications. Because the mass of a proton is much larger than the mass of an electron (m_p:m_e = 1,800:1), the energy of the secondary electrons is very small compared with secondary electrons generated by electron beam lithography. Therefore, a proton will travel along a straight path into resist and secondary electrons will only expose the resist within several nanometers around the path of the proton. PBW is capable of fabricating structures with very straight, vertical and smooth sidewalls without proximity effect. This is very important when combining PBW with Ni electroplating and nanoimprinting as well as injection molding. High quality Ni molds with smooth and vertical side walls are critical in nanoimprint lithography and injection molding. In our experiments, several new resists including AR-P 3250, a mixture of AR-P 3250 and AR 300-12, and ma-N 2401 are tested with PBW for the production of high aspect ratio Ni molds and thermoplastic replication with these molds. High aspect ratio structures (up to 7) are fabricated at a width of 500 nm in Ni molds. The structures are transferred to plastic via nanoimprinting and injection molding.     

Arrays of high-aspect ratio microchannels for high-throughput isolation of circulating tumor cells (CTCs)

Microsystem-based technologies are providing new opportunities in the area of in vitro diagnostics due to their ability to provide process automation enabling point-of-care operation. As an example, microsystems used for the isolation and analysis of circulating tumor cells (CTCs) from complex, heterogeneous samples in an automated fashion with improved recoveries and selectivity are providing new opportunities for this important biomarker. Unfortunately, many of the existing microfluidic systems lack the throughput capabilities and/or are too expensive to manufacture to warrant their widespread use in clinical testing scenarios. Here, we describe a disposable, all-polymer, microfluidic system for the high-throughput (HT) isolation of CTCs directly from whole blood inputs. The device employs an array of high aspect ratio (HAR), parallel, sinusoidal microchannels (25 × 150 μm; W × D; AR = 6.0) with walls covalently decorated with anti-EpCAM antibodies to provide affinity-based isolation of CTCs. Channel width, which is similar to an average CTC diameter (10–20 μm), plays a critical role in maximizing the probability of cell/wall interactions and allows for achieving high CTC recovery. The extended channel depth allows for increased throughput at the optimized flow velocity (2 mm/s in a microchannel); maximizes cell recovery, and prevents clogging of the microfluidic channels during blood processing. Fluidic addressing of the microchannel array with a minimal device footprint is provided by large cross-sectional area feed and exit channels poised orthogonal to the network of the sinusoidal capillary channels (so-called Z-geometry). Computational modeling was used to confirm uniform addressing of the channels in the isolation bed. Devices with various numbers of parallel microchannels ranging from 50 to 320 have been successfully constructed. Cyclic olefin copolymer (COC) was chosen as the substrate material due to its superior properties during UV-activation of the HAR microchannels surfaces prior to antibody attachment. Operation of the HT-CTC device has been validated by isolation of CTCs directly from blood secured from patients with metastatic prostate cancer. High CTC sample purities (low number of contaminating white blood cells) allowed for direct lysis and molecular profiling of isolated CTCs.     

Replication of sub-100 nm structures using h- and s-PDMS composite stamps

Soft-UV-NIL as replication technique was used to replicate sub-100 nm structures. The aim of this work is the stamp production and the replication of structures with dimensions smaller than 100 nm in a simple manner. Composite stamps composed of two layers, a thin hard PDMS layer supported by a thick soft PDMS (s-PDMS) layer are compared to common s-PDMS stamps regarding the resolution by using a Siemens star (star burst pattern) as test structure. The master is fabricated by electron beam lithography in a 140 nm thick PMMA resist layer. The stamp is molded directly from the structured resist, without any additional anti sticking treatment. Therefore the resist thickness determines the aspect ratio, which is 1.5 at the resolution limit. The replication is done in a UV-curing cycloaliphatic epoxy material. The employed test structure provides good comparability, the resolution limit at a glance, and it integrates a smooth transition from micro- to nanostructures. Therefore it is a capable structure to characterize the UV-NIL.     

Fabrication of a high aspect ratio (HAR) micropillar filter for a magnetic bead-based immunoassay

A microfluidic chip has been realized for investigating immune cell (U937) activation with lipopolysaccharide (LPS) and subsequent pro-inflammatory cytokine (Interleukin-6, IL-6) detection (Ruffert et al. Proc. EMBL Conference Microfluidics 2012a, p 184; Proc. NanoBioTech Montreux, Poster Sessions B 2012b, pp 17–18). The microfluidic chip comprises two compartments: one compartment for the on-chip cell cultivation, differentiation, and stimulation, while the second one hosts superpara-magnetic beads (Ø 2.8 μm) conjugated to anti-IL-6 antibodies for capturing the LPS-induced IL-6. The two compartments are separated by a micropillar-based filter with a spacing of 2 μm. This filter allows the induced cytokines to infuse into the bead compartment (i.e. the magnetic immunoassay compartment), while preventing the magnetic beads and cells to cross over to the other compartment. To fulfill this requirement, a high aspect ratio pillar array was demonstrated as key element of this study and functionally characterized. The pore size of the filter is given by the lateral distance between the single pillars, which are fabricated by molding microfluidic structures in polydimethylsiloxane, using a master mold made of the expoy-based photoresist SU-8?. An aspect ratio of 5:1 could be achieved with SU-8? bars featuring the dimensions 10 µm × 2 μm (height × width).     

Fabrication of large area diffraction grating using LIGA process

X-ray imaging is a very important technology in the fields of medical, biological, inspection, material science, etc. However, it is not enough to get the clear X-ray imaging with low absorbance. We have produced a diffraction gratings for obtaining high resolution X-ray phase imaging, such as X-ray Talbot interferometer. In this X-ray Talbot interferometer, diffraction gratings were required to have a fine, high accuracy, high aspect ratio structure. Then, we succeeded to fabricate a high aspect ratio diffraction grating with a pitch of 8 μm and small area using a deep X-ray lithography technique. We discuss that the diffraction gratings having a narrow pitch and an large effective area to obtain imaging size of practical use in medical application. If the pitch of diffraction gratings were narrow, it is expected high resolution imaging for X-ray Talbot interferometer. We succeeded and fabricated the diffraction grating with pitch of 5.3 μm, Au height of 28 μm and an effective area of 60 × 60 mm².     

Simulation and fabrication of a branch-channel rhombic micromixer for low pressure drop and short mixing length

The planar micromixers merit easy integration with the microsystem but encounter the problems of high pressure drop and long mixing length for high mixing efficiency over 90 %. In this article, an advanced branched rhombic micromixer (BRM) have been designed and investigated by 3D numerical simulations and experiments. Polydimethylsiloxane (PDMS) molding process was used for chip fabrication of the experiment. The CFD-ACE⁺ software was applied for modeling simulations. Simulation results showed that this optimum geometry design of four-mixing-unit BRM with the branch position at 700 μm high and 100 μm wide can effectively improve the mixing efficiency over 95 % at Reynolds number (Re) 120 with a rather low pressure drop about 9,000 Pa and a short mixing length of 5.5 mm as well. The high mixing efficiency at low pressure drop is attributed to the greatly increased contact interface area and chaotic-convection vortices as well as the low flow resistance with branched channels. The mixing verification is performed by the flow visualization system via the popular rhodamine B dye (10 mM) added DI method for PDMS BRM chips.     

Fabrication of micro pore optics with smooth sidewall using X-ray lithography

Micro pore optics (MPO) as an X-ray imaging system is perfectly suited for the applications in space telescopes due to its light-weight and high-resolution properties. We report the fabrication of MPO samples by LIGA process focusing on its sidewall surface used as mirrors for X-ray reflection. An intermediate mask is fabricated and used to obtain the working mask in order to avoid the UV exposure to a very thick photo resist layer. Around 400 μm-thick nickel MPO plate is obtained with the aspect ratio of the square pore and sidewall of 8 and 32, respectively. The root mean square roughness of the sidewall surface is below 10 nm in a 5 × 5 μm² region. Some striations are found on the sidewall surface originating from the jagged edge of the chromium coating on the UV mask.     

Low cost method for hot embossing of microstructures on PMMA by SU-8 masters

Polymer based microfabrication technologies are used extremely in Bio-MEMS, especially in Microfluidic devices in recent years. In this paper, a novel method for fabrication of microstructures on a polymeric material using hot embossing lithography process is presented. The proposed method involves usage of low cost materials and procedure with respect to previous methods and can be processed in a short time. The master is made from SU-8 on an inexpensive glass substrate which is patterned by standard lithography. The embossing pressure can be increased in our master as the glass substrate used in this paper is more robust than Silicon. Master robustness and SU-8 to glass adhesion is optimized by some substrate pretreatments and SU-8 baking time and temperatures. Microchannels are replicated on a Polymethylmetacrylate (PMMA) stamp which is a plexiglass sheet with thickness of 1 mm. Significant embossing parameters including temperature, pressure and time are discussed and optimum values are determined. Microchannels are imprinted by depth of 50 μm and minimum width of 15 μm and aspect ratio more than 3. The microchannels are sealed by a PMMA cap using thermal annealing bonding.     

Fabrication of micro sloping structures of SU-8 by substrate penetration lithography

In this paper, three-dimensional (3D) micro sloping structures were fabricated by ordinary mask pattern and diffraction phenomenon. Especially, we fabricated the structures with SU-8 negative photoresist and substrate penetration lithography. In this method, exposure is performed arranging in order of a mask, a substrate and the SU-8 resist. There is a gap that is equal to the thickness of the substrate between resist and mask. In narrow slit of mask, resist is less exposed than usual because of Fraunhofer diffraction. The amount of exposure depends on slit width so that the height of SU-8 resist can be controlled. A 173 μm height of structure was obtained in the case of 27 μm width slit and 24.2 μm height of structure was obtained in the case of 7.4 μm width slit. By using this method, high aspect ratio 3D SU-8 structures with smooth sloping were fabricated in the length of 100–300 μm and in the height of 50–200 μm with rectangular triangle mask pattern. In the same way, there is influence of Fresnel diffraction on edge of aperture so that micro taper structures were fabricated. A lot of taper structures were fabricated by the method to make the surface repellency. The contact angle was achieved more than 160° in this study.     

Orthogonal and fine lithographic structures attained from the next generation proton beam writing facility

A second generation proton beam writing (PBW) system has been built at the Centre for Ion Beam Applications at the National University of Singapore for fabrication of high aspect ratio 3D nano lithographic structures. System improvements and a few lithographic structures obtained with this facility are presented in this paper. Through accurate alignment of the magnetic quadrupole lenses and the electrostatic scanning system, orthogonal beam scanning has been achieved. The earlier constrain of limited beam scan area has been overcome by adopting a combination of beam and stage scanning as well as stitching. With these improvements smallest ever Ni structure of 65 nm in width has been fabricated using nickel electroplating on a proton beam written PMMA sample in the second generation PBW facility. Using this improved PBW facility, we have also demonstrated the fabrication of fine lithographic patterns with 19 nm line width and 60 nm spacing in 100 nm thick negative high resolution hydrogen silsesquioxane resist. Future possible system improvements leading to finer resolution will be discussed briefly.     

Session-based security enhancement of RFID systems for emerging open-loop applications

Radio frequency identification (RFID) is an important technique used for automatic identification and data capture. In recent years, low-cost RFID tags have been used in many open-loop applications beyond supply chain management, such as the tagging of the medicine, clothes, and belongings after the point of sales. At the same time, with the development of semiconductor industry, handheld terminals and mobile phones are becoming RFID-enabled. Unauthorized mobile RFID readers could be abused by the malicious hackers or curious common people. Even for authorized RFID readers, the ownership of the reader can be transferred and the owners of the authorized mobile reader may not be always reliable. The authorization and authentication of the mobile RFID readers need to take stronger security measures to address the privacy or security issues that may arise in the emerging open-loop applications. In this paper, the security demands of RFID tags in emerging open-loop applications are summarized, and two example protocols for authorization, authentication and key establishment based on symmetric cryptography are presented. The proposed protocols adopt a timed-session-based authorization scheme, and all reader-to-tag operations are authorized by a trusted third party using a newly defined class of timed sessions. The output of the tags is randomized to prevent unauthorized tracking of the RFID tags. An instance of the protocol A is implemented in 0.13-μm CMOS technology, and the functions are verified by field programmable gate array. The baseband consumes 44.0 μW under 1.08 V voltage and 1.92 MHz frequency, and it has 25,067 gate equivalents. The proposed protocols can successfully resist most security threats toward open-loop RFID systems except physical attacks. The timing and scalability of the two protocols are discussed in detail.     

LIGA micro-openings for coherence characterization of X-rays

Infinitely thin opaque screens serving for diaphragms as defined in the visible-light optics are not feasible for operation with X-ray beams due to their high penetrability. Micro-openings of predicted sidewall shape in a gold layer up to 140 μm thick which would provide low transparency, are proposed. The proposed micro-openings were made using the LIGA technique and tested successfully at photon energies of up to 25 keV. The micro-openings can be used as targets for coherence X-ray pattern or, if long interference tails are avoided by means of the advanced sidewall shape, as X-ray beam collimators.     

Large tuning ratio high aspect ratio variable capacitors using leveraged bending

Variable capacitors are a key component in Radio Frequency Micro Electro-Mechanical Systems (RF MEMS). They comprise fixed and flexible electrodes. Deformation, or actuation, of the flexible electrode changes the capacitance of the capacitor. This way, electrical properties of high frequency circuits can be modified. Traditionally, variable capacitors are based on a planar layout architecture, while a newer, vertical-wall, quasi three-dimensional approach theoretically enables increased device performance. Such devices depend on high aspect ratios, i.e. relatively high micro structures with very thin walls and gaps. A few vertical-wall variable capacitors made of nickel or gold have been fabricated to date, using deep X-ray lithography and subsequent electroplating (Achenbach et al. 2006; Klymyshyn et al. 2007, 2010) as the fabrication approach. They feature, amongst others, excellent quality factors of Q ≤ 95 at 5.6 GHz with 50 Ω reactance, but suffer from a very limited tuning range of the capacitance value (tuning ratio of, e.g., 1.38:1). The devices presented here exploit the same architecture and materials selection, resulting in similar, excellent Q-factors, but feature a different electrode layout approach, referred to as leveraged-bending. This layout is based on pulling a flexible electrode sideways, towards a fixed electrode, increasing the capacitance when actuating the variable capacitor. The leveraged bending approach theoretically enables infinitely high tuning ratios for components with perfect structure accuracy. To date, a significantly increased tuning ratio of 1.9:1 has been demonstrated. Limiting factors are an electrically non-ideal layout geometry chosen as a compromise to increase the fabrication yield, and structure deviations of ~1.6 μm from CAD layout to the electroplated component. Electrostatic actuation requires voltages between 0 and 72 V for capacitance values on the order of C = 0.3 pF at device dimensions of about 1.5 mm overall length, 5–10 μm gap and wall widths, and 100 μm metal height. Device performance measured with a vector network analyzer is in 97 % agreement with simulation results based on two-dimensional electrostatic-structural coupling (ANSYS Multiphysics) and three-dimensional electromagnetic field simulations (Ansoft HFSS). These simulations also indicate that an optimized gap geometry will allow to reduce the actuation voltage required by up to 40 %.     

Fabrication of high precision X-ray mask for X-ray grating of X-ray Talbot interferometer

X-ray imaging is used in many applications such as medical diagnosis and non-destructive inspection, and has become an essential technologies in these areas. In one image technique, X-ray phase information is obtained using X-ray Talbot interferometer, for which X-ray diffraction gratings are required; however, the manufacture of fine, highly accurate, and high aspect ratio gratings is very difficult. X-ray lithography could be used to fabricate structures with high precision since it uses highly directive syncrotron radiation. Therefore, we decided to fabricate X-ray gratings using X-ray lithography technique. The accuracy of the fabricated structure depends largely on the accuracy of the X-ray mask used. In our research, we combined deep silicon dry etching technology with ultraviolet lithography in order to fabricate untapered and high precision X-ray masks containing rectangular patterns. We succeeded in fabricating an X-ray mask with a pitch of 5.3 μm. The thickness of the Au absorber was about 5 μm, and the effective area was 60  × 60 mm², which is a sufficient size for phase tomography imaging. We demonstrated the utility of the Si dry etching process for making high precision X-ray masks.     

X-ray zone plates with 25 aspect ratio using a 2-μm-thick ultrananocrystalline diamond mold

Hard X-ray phase zone plates are focusing optics used for X-ray microscopes at synchrotron radiation facilities. The resolution is determined by the outer-most zone width (OZW) and modern lithographic techniques are capable of patterning OZW less than 100 nm. Efficiency of a phase zone plate will peak when the zones have a thickness that provides a π-phase shift to the X-rays. Thus, a hard X-ray zone plate with ideal efficiency and sub-100-nm resolution requires fabricating high-aspect-ratio, dense-packed structures in materials suitable for exposure to synchrotron radiation. The fabrication method implemented involves an electroforming mold process where a top resist layer is lithographically patterned and used for pattern transfer into a bottom layer which acts as the electroform mold. The resulting mold is filled with Au by electroplating, and afterwards the mold is not removed but remains in place for mechanical support. Ultrananocrystalline diamond (UNCD) was used as the mold layer. UNCD is deposited by hot-filament chemical vapor deposition with well-controlled stress and thickness up to 2 μm. The top resist layer is hydrogen silsesquioxane, which is a high-contrast electron beam lithography resist and resistant to the oxygen reactive ion etching required for UNCD pattern transfer. Using this fabrication method, we successfully produced zone plates with OZW down to 80 nm and an aspect ratio up to 25 for a thickness of 2 μm. The efficiency of several fabricated zone plates were measured, demonstrating their functionality.     

A novel three-dimensional microfluidic platform for on chip multicellular tumor spheroid formation and culture

The formation of three-dimensional (3D) multicellular cell spheroids such as microspheres and embryoid bodies has recently gained much attention as a useful cell culture technique, but few studies have investigated the suitability of glass for spheroids formation and culture. In this work, we present a novel three-dimensional microfluidic device made of poly(dimethylsiloxane) (PDMS) and glass for the easy and rapid synthesis and culture of tumor spheroid. The cell culture unit is composed of an array of microwells on the bottom of a glass plate, bigger microwells and elastomeric microchannels on the top of a PDMS plate. Cell suspension can be easily introduced into the cell culture unit and exchange with the external liquid environment by the microfluidic channels. A single tumor spheroid can be formed and cultured in each glass cell culture chamber, the surface of which was modified with poly(vinyl alcohol) to render it to be resistant to cell adhesion. As the cell culture medium could be replaced, spheroids of the human breast cancer (MCF-7) cells were cultured on the chip for 3 days, reaching the diameters of about 150 μm. Furthermore, the MCF-7 cells were successfully cultured on the chip in 2D and 3D culture modes. Results have shown that glass is well suitable for multicellular tumor spheroids culture. The established platform provides a convenient and rapid method for tumor spheroid culture, which is also adaptable for anticancer drug screening and fundamental biomedical research in cell biology.     

A dual-axis MEMS capacitive inertial sensor with high-density proof mass

This paper reports a novel dual-axis microelectromechanical systems (MEMS) capacitive inertial sensor that utilizes multi-layered electroplated gold. All the MEMS structures are made by gold electroplating that is used as a post complementary metal-oxide semiconductor (CMOS) process. Due to the high density of gold, the Brownian noise on the proof mass becomes lower than those made of other materials such as silicon in the same size. The single gold proof mass works as a dual-axis sensing electrode by utilizing both out-of-plane (Z axis) and in-plane (X axis) motions; the proof mass has been designed to be 660 μm × 660 μm in area with the thickness of 12 μm, and the actual Brownian noise in the proof mass has been measured to be 1.2 \({\upmu}{\text{G/}}\sqrt {\text{Hz}}\) (in Z axis) and 0.29 \({\upmu}{\text{G/}}\sqrt {\text{Hz}}\) (in X axis) at room temperature, where 1 G = 9.8 m/s². The miniaturized dual-axis MEMS accelerometer can be implemented in integrated CMOS-MEMS accelerometers to detect a broad range of acceleration with sub-1G resolution on a single sensor chip.