Quasi-3D microstructure fabrication technique utilizing hard X-ray lithography of synchrotron radiation

 Quasi-three-dimensional (3D) microstructure fabrication technique utilizing hard X-ray lithography (HXL) has been developed. In this technique, as the intensity distribution of the X-rays is controlled by a newly developed bending mirror, the exposure residual depth of polymethyl methacrylate (PMMA) resist is controlled over the exposed area. The maximum difference of depths was approximately 50 μm over the large area more than 60 mm (horizontal) × 5 mm (vertical). We also investigated the effects of controlling the beam intensity distribution for exposure changing X-ray mask absorber shapes and angle on the obtained quasi-3D resist pattern shapes. As the results, Quasi-3D PMMA patterns with inclined shape sidewall and graded depths were successfully fabricated. We believe this technique greatly expands applications of LIGA process. Received: 10 August 2001/Accepted: 24 September 2001 This paper was presented at the Fourth International Workshop on High Aspect Ratio Microstructure Technology HARMST 2001 in June 2001.     

Geometrical strengthening and tip-sharpening of a microneedle array fabricated by X-ray lithography

A novel fabrication method for LIGA (from the German “Lithographie”, “Galvanik”, and “Abformung”) microneedles with through holes is presented. Such microneedles are in demand by most bio-medical MEMS applications and in some fluidic MEMS applications. We propose a technique that combines conventional deep X-ray lithography, plane-pattern to cross-section transfer (PCT) process, and alignment X-ray lithography. The technique provides precise hole alignment with ± 3 μm tolerance. Finite-element simulations on various hole locations were performed to determine the optimum position. We previously fabricated a microneedle with a 100-μm base and a 300-μm height by a right-triangular mask. The resultant microneedle had a very sharp tip but was excessively steep, and thus resulted in a very low strength. Improved strength and tip sharpness was consequently achieved by changing the mask-pattern from a triangular pattern to a polygonal mask and changing the dimensions of the microneedle to have a 300-μm base with various heights between 350 and 800 μm. Using the proposed technique, we could produce a total of 100 hollow microneedles on a 5 × 5 mm² chip. Moreover, we successfully fabricated sharpened microneedles that were stronger than that we have fabricated so far. The molding process or electroplating and the cost list of the LIGA microneedle will also be included.     

Fabrication of microneedle array using LIGA and hot embossing process

We demonstrate a novel fabrication technology of the microneedle array applied to painless drug delivery and minimal invasive blood extraction. The fabrication technology consists of a vertical deep X-ray exposure and a successive inclined deep X-ray exposure with a deep X-ray mask whose pattern has a hollow triangular array. The vertical exposure makes triangular column array with a needle conduit. With the successive inclined exposure, the column array shapes into the microneedle array without deep X-ray mask alignment. Changing the inclined angle and the gap between the mask and PMMA (PolyMethylMetaAcrylic) substrate, different types of microneedle array are fabricated in 750–1000 m shafts length, 15^o–20^o tapered tips angle, and 190–300 m bases area. The masks are designed to 400–600 m triangles length, 70–100 m conduits diameter, 25–60EA/5 mm² arrays density, and various tip shapes such as triangular, rounded, or arrow-like features. In the medical application, the fabricated PMMA microneedle array fulfills the structural requirements such as three-dimensional sharp tapered tip, HAR (High-Aspect-Ratio) shafts, small invasive surface area, and out-of-plane structure. In the skin test, the microneedle array penetrates back of the hand skin with minimum pain and without tip break and blood is drawn after puncturing the skin. Hot embossing process and mold fabrication process are also investigated with silicon and PDMS mold. The processed tetrahedral PMMA structures are fabricated into the microneedle array by the additional deep X-ray exposure. With these processes, the microneedle array can be utilized as the mold base for electroplating process.The author thanks the staff in 9 C LIGA beamline, Pohang Light Source (PLS), Korea for their assistance on the fabrication process.     

Structure quality in deep X-ray lithography applying commercial polyimide-based masks

The structure quality of deep X-ray lithography components strongly depends on the quality of the applied X-ray mask. In this article we compare the results obtained with two different mask types. Sophisticated working masks generated by e-beam lithography, soft X-ray lithography and electroplating of gold absorbers on a titanium mask membrane have been fabricated at the Institute for Microstructure Technology, Research Center, Karlsruhe (FZK/IMT), Germany. Prototype masks generated by e-beam lithography, optical lithography and electroplating of gold absorbers on a polyimide mask membrane have been fabricated by Optnics Precision, Japan, with the aim to offer commercially available low cost masks. Both mask types were applied to pattern PMMA resist layers of 300–750 μm thickness at the 2.5 GeV electron storage ring ANKA, Germany, using comparable process parameters. FZK/IMT masks provide microstructures with significantly better structure quality. The layout area, however, is currently limited to 12 cm², and the Ti mask membrane tends to lead to a slight resist surface attack, such as rounding of the resist edges. Optnics masks provide microstructures with reduced structure quality due to sidewall striations (sidewall roughness up to 2 μm) and thermal distortions (of up to 3–5 μm) which limit the potential scope of applications. They could nevertheless potentially be applied as low quality, low cost X-ray masks. High resolution and high accuracy applications, however, require more sophisticated but also more expensive masks, like the Ti-masks from FZK/IMT.     

Inexpensive, quickly producable X-ray mask for LIGA

 The capability to produce X-ray masks inexpensively and rapidly is expected to greatly enhance the commercial appeal of the LIGA process. This paper presents a process to fabricate X-ray masks both inexpensively (under $1000) and rapidly (within a few days). The process involves one UV lithography step and eliminates the need for an intermediate X-ray mask. The X-ray mask produced by this process consists of a 125 μm thick graphite membrane that supports a gold-on-nickel absorber pattern. The thickness of the absorber structures is great enough to supply sufficient contrast even when radiation sources with high characteristic photon energies up to 40 keV are utilized and/or when deep exposures are desired. The mask fabrication process is initiated by spin coating 30–50 μm of SU-8 directly on a graphite membrane. The SU-8 is then patterned using a UV mask. Gold-on-nickel absorber structures are electroplated directly onto the SU-8 covered graphite. Once the remaining SU-8 is removed, attaching the graphite membrane to a frame completes the mask. To test the performance of the mask, a nickel mold insert was fabricated. A sheet of PMMA 500 μm in thickness was bonded to a nickel substrate, then exposed to X-rays through the mask, and developed. Electroplating nickel into the patterned PMMA sheet produced a mold insert. SEM pictures taken of the SU-8, the X-ray mask, and the mold insert are shown. This method of rapidly producing an inexpensive X-ray mask for LIGA resulted in a mold insert with smooth, vertical sidewalls whose dimensions were within two micrometers of the UV mask dimensions. Received: 12 December 1998/Accepted: 2 February 1999     

Large area, cost effective X-ray masks for high energy photons

The cost effectiveness of the deep X-ray lithography and electrodeposition process, LIGA, depends directly on the throughput of the process. The use of high energy photons allows the exposure of stacked photoresist and results in high throughput. High energy X-ray exposures require a different mask than low energy X-ray exposures. The high energy mask allows a large area exposure but requires a thicker X-ray absorber. The cost of generating high energy X-ray masks can be drastically reduced by using a thick optical photoresist process rather than an X-ray exposure process. The cost can be further reduced by using alternatives to the typical X-ray absorber, gold. High atomic weight (high Z) materials are ideal absorbers. Lead has been demonstrated as being a useable alternative as an X-ray absorber. Received: 7 July 1999 / Accepted: 1 September 1999     

The fabrication of LIGA mask using photolithography and synchrotron radiation lithography

 The fabrication of LIGA mask is a very important step in LIGA process. Usually an intermediate mask with gold absorber pattern of 2 μm thickness is fabricated firstly using gold electroplating for absorber pattern in the resist structure written by Electron Beam (e-Beam), then the LIGA mask can be copied from the intermediate mask using synchrotron radiation lithography and gold electroplating. Recently, we use photolithography (instead of e-beam) to make the primary structure, and produce the intermediate mask with gold absorber pattern of 1.5 μm thickness produced by etching gold film with 1.5 μm thickness under the photoresist structure using Ar⁺. The LIGA mask with absorber pattern of 13 μm thickness is copied from the intermediate mask using synchrotron radiation lithography and gold electroplating. Received: 30 October 1995/Accepted: 9 December 1995     

Application of 3D gray mask for the fabrication of curved SU-8 structures

This paper proposes a novel technology to fabricate 3D structures such as curved structures on SU-8 resist by 3D gray mask combined with glycerol compensation technique. 3D Gray mask is designed and fabricated by patterning and reflowing AZ4620 resist on standard quartz or glass mask plate. Through exposure dose control, curved shapes with different curvatures have been successfully fabricated with smooth structure surface. Simple calculations on the prediction of the shapes and sizes of the exposed 3-D structures have also been carried out, and the results show a close relationship between the calculations and the experiments. Compared to traditional gray mask technologies, this method provides a simple and cost effective way to fabricate curved structures with reasonable surface smoothness, which may be suitable for optical or micro fluidic applications.Based on the following paper presented at the HARMST 2003 Conference: K. Y. Hung and F. G. Tseng, Application of Shadow Mask and Polarized Inclined-Exposure for Curved SU-8 Structures on Inclined Surface, Proc. of 5th High Aspect Ratio Micro-Structure Technology Conference, June 15–17, 2003, Monterey, California USA.This work was supported by the National Science Council of Taiwan, ROC under the grant NSC 89–2323-B-007–005.     

Fabrication of monolithic multilevel high-aspect-ratio ferromagnetic devices

This paper describes a process to fabricate monolithic multilevel high-aspect-ratio microstructures (HARMs) for ferromagnetic devices built on silicon wafers using aligned X-ray lithography in conjunction with electrodeposition. Two X-ray masks were fabricated, each consisting of gold (Au) absorber structures on a transparent polyimide membrane. One mask was used to print a polymethyl methacrylate (PMMA) resist layer. Then, a second PMMA layer was applied to the same wafer, and the second mask was used to pattern it. Transparent alignment windows in the second mask, combined with a piezoelectrically controlled X-ray aligner, allowed for high alignment accuracy between the two print patterns over large areas (>4 inch in diameter). Au circuits were electroplated into first PMMA layer from a sulfite-based electrolyte, and nickel-iron (NiFe) ferromagnetic HARMs were formed in second PMMA resist from a sulfate-based bath. The deposition resulted in well-defined NiFe structures with aspect-ratios up to 67:1 as well as smooth sidewalls and top surfaces. Chemical composition measurements with energy X-ray dispersive spectroscopy (EDS) and wavelength X-ray dispersive spectroscopy (WDS) showed that Fe content increased during the electrodeposition process. To electrically isolate the NiFe posts and Au circuits, both wet chemical etching and sputter etching were explored to remove the exposed seed layer, and the latter approach completely removed the seed layers without damaging the electroplated features.     

Silicon IC compatible LIGA mask-fabrication process

 This paper describes a technique for fabricating a LIGA mask that offers good compatibility with the silicon IC process. X-ray exposure can be eliminated from the LIGA mask-fabrication process, so that LIGA masks can be fabricated with existing silicon IC process equipment. A gold absorber pattern, 2 μm wide and 10 μm thick, has been successfully fabricated by combining a three-layer resist-patterning process with the electroplating process. Improvements in both the mask structure and fabrication process alleviate the problems of dust in a cleanroom and contamination in the etching chamber. Received: 25 August 1997/Accepted: 23 September 1997     

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.     

Fabrication of electrostatic MEMS microactuator based on X-ray lithography with Pb-based X-ray mask and dry-film-transfer-to-PCB process

Lithographie Galvanoformung Abformung (LIGA) is a promising approach for fabrication of high aspect ratio 3D microactuator for dual-stage slider in hard disk drive. However, this approach involves practically challenging X-ray lithography and structural transfer processes. In this work, electrostatic MEMS actuator is developed based on a LIGA approach with cost-effective X-ray lithography and dry-film-transfer-to-PCB process. X-ray lithography is performed with X-ray mask based on lift-off sputtered Pb film on mylar substrate and photoresist application using casting-polishing method. High quality and high aspect ratio SU8 microstructures with inverted microactuator pattern have been achieved with the interdigit spacing of ~5 μm, vertical sidewall and a high aspect ratio of 29 by X-ray lithography using the low-cost Pb based X-ray mask. A new dry-film-transfer-to-PCB is employed by using low-cost dry film photoresist to transfer electroplated nickel from surface-treated chromium-coated glass substrate to printed circuit board (PCB) substrate. The dry film is subsequently released everywhere except anchor contacts of the electrostatic actuator structure. The fabricated actuator exhibits good actuation performance with high displacement at moderate operating voltage and suitably high resonance frequency. Therefore, the proposed fabrication process is a promising alternative to realize low-cost MEMS microactuator for industrial applications.     

Equations of exposure time and X-ray mask absorber thickness in the LIGA process

 The LIGA X-ray exposure step was modeled into three inequalities from exposure requirements. From these inequalities, equations for the minimum and maximum exposure times required for a good quality microstructure were obtained. An equation for the thickness of an X-ray mask absorber was also obtained from the exposure requirement of threshold dose deposition. A power function of photon energy, approximating the attenuation length of the representative LIGA resist, PMMA, and the mean photon energy of the X-rays incident upon an X-ray mask absorber were applied to the above mentioned equations. Consequently, the trends of the minimum and maximum exposure times with respect to mean photon energy of X-rays and thickness of PMMA were examined and an equation for the maximum exposable thickness of PMMA was obtained. The trends of the necessary thickness of a gold X-ray mask absorber with respect to photon energy of the X-rays and PMMA thickness ratio were also examined. The simplicity of the derived equations has clarified the X-ray exposure phenomenon and the interplay of exposure times, the attenuation coefficient and the thickness of an X-ray mask absorber, the attenuation coefficient and the thickness of a resist, and synchrotron radiation power density. Received: 22 November 1999/Accepted: 27 January 2000     

Optimization of laser writer-based UV lithography with high magnification optics to pattern X-ray lithography mask templates

Deep X-ray lithography is a preferred fabrication approach for those micro devices that depend on smooth and vertical sidewalls of comparatively deep structures rather than extreme lateral resolution. The structure quality obtained depends on, and is limited by, the quality of the X-ray mask applied. A critical component of the mask is its absorber patterns. They get fabricated by electroplating into voids of a polymer template. These templates must usually be at least 3 μm deep and exhibit smooth and vertical sidewalls with a lateral resolution of micrometers and possibly below. Primary patterning of the templates is very demanding. Best results are obtained when dedicated electron beam writers with acceleration voltages of 100 kV and above are applied. This, however, limits access to patterning infrastructure and substantially drives delivery timeline and cost, making mask absorber template patterning a bottleneck of the entire process sequence. We propose, evaluate and optimize an alternative absorber patterning approach based on direct laser writing. An ultraviolet laser with 355 nm wavelength and 250 mW beam power by Heidelberg Instruments is applied to expose 2.9 μm thick, chemically amplified, high contrast, negative tone resist mrx-5. Exposure parameters analyzed include the dose and focal settings. Experiments are carried out on bare silicon wafers as well as on chrome-gold and on titanium oxide plating bases. For all cases, results with and without an additional antireflective coating of 200 nm AZ BAR-Li are studied. Aspects of the resist template structure quality analyzed include the sidewall verticality and its smoothness and defects, resist adhesion to the substrate, minimum feature size and structure accuracy, as well as irregularities due to stitching of partial layouts. In an optimized process, a dose of 14 mW on oxidized titanium and BAR-Li was used. We were able to demonstrate 1.5 μm minimum feature size of isolated structures and structural details of about 1 μm. The sidewalls are vertical and exhibit a roughness of dozens of nanometers. When an antireflective coating is used, chamfers are observed at the resist bottom. The structure accuracy occasionally deviates from the original layout by 200–300 nm, particularly at stitching singularities or towards the end of resist walls. The described absorber template patterning process delivers a resolution that much extends beyond previous UV patterning approaches. The structure accuracy, however, is inferior to electron beam written samples. Given the cost and timeline benefit, results of the study will allow users to identify which primary patterning approach is best suited for their micro devices.

     

Single-step UV diffraction lithography to define a hydrophobic SU-8 interconnected hoodoo structure

Micro-hoodoo (inverse trapezoidal) structures fabricated by silicon etching, soft-lithography, or photolithography have attracted great interest due to their improved hydrophobicity and self-cleaning properties. We present here a simple single-step UV diffraction lithography technique for fabricating micro-hoodoo structures with or without adjustable interconnecting bridges using a negative SU-8 photoresist. The theoretical calculations and the fabrication results revealed that the sizes and sidewall profiles of the micro-hoodoo structures and interconnecting bridges could be precisely controlled by the fabrication conditions, including the pattern-to-pattern spacing, exposure dose, and gap between the mask and the SU-8 surfaces. The theoretical calculations were conducted using an integrated model based on a Fresnel diffraction model for estimating the hoodoo size and an exponent decay model for estimating the sidewall profile. The integrated model agreed well with the fabricated hoodoo sizes and sidewall profiles, and the model provided an explanation for the structural instabilities observed during formation of the interconnecting bridges between hoodoos. The interconnecting bridges made the hydrophobic hoodoo structures sticky toward water, with a water contact angle hysteresis of up to 86.6°. The directional bridge interconnections produced directionally sticky hydrophobic surfaces that successfully mimicked function in butterfly wings to enable directional water removal.     

A Micro corona motor fabricated by a SU-8 built-on X-ray mask

A micro corona motor was fabricated using a membraneless built-on X-ray mask. Sharp stator electrodes of this motor ionize air molecules and ionized charges transfer onto the rotor surface, resulting in rotating rotor motions by Coulomb forces. For good performance, the stators electrodes should be wide (axial) and have sharp tips. Therefore, X-ray lithography was adopted for precise, high aspect ratio characteristics. To avoid the fabrication difficulty of a membrane X-ray mask, a built-on X-ray mask (conformal mask) technique was employed with negative toned SU-8 photoresist. SU-8 features X-ray fabrication compatibility, X-ray transparency and a large range of thickness. This technique may be suitable for fast fabrication of prototypes or very tall structures, which can be largely affected by printing gaps. For the X-ray built-on mask, 20 m SU-8 was patterned and 8 m gold absorber was electroplated on top of the 300 m PMMA resist. Tests showed good quality pattern transfer from the SU-8 pattern and smooth sidewalls.The authors would like to thank the National Science Foundation, Grant DMI-0115527, Manufacturing Machines and Equipment Program, Division of Design, Manufacture, and Industrial Innovation, and Atoz CompuNet Ltd. for support for this work. We also acknowledge partial support from Center for Nano and Molecular Science and Technology and Welch foundation in The University of Texas at Austin.     

Fabrication of X-rays mask with carbon membrane for diffraction gratings

We have produced diffraction gratings for obtaining high resolution X-ray phase imaging, such as X-ray Talbot interferometer. These diffraction gratings were required to have a fine, high accuracy, high aspect ratio structure. Therefore, we decided to use the X-rays lithography technique that used synchrotron radiation of the directivity for a manufacture process. The accuracy of the completed structure depends largely on the accuracy of the X-ray mask. In our group, a resin material is conventionally used for the membrane of large X-ray masks. However, X-ray masks comprising a resin membrane have the disadvantage that, after several cycles of X-ray exposure, they crease and sag due to X-ray-derived heat. As a substitute for the conventional resin membrane, we experimentally fabricated a new X-ray mask using a carbon wafer membrane. The newly fabricated X-ray mask was subjected to X-ray exposure experiment. We succeeded in making the structure body which was almost shape. And the experimental results verified that the new mask did not deteriorate even when used repeatedly, demonstrating that it was highly durable.     

Fabrication method with high-density,high-height microneedle using microindentation method for drug delivery system

We have developed a microneedle formation method that has high needle height and density by forming indentations on a metal plate using a micro-machined silicon microneedle, called the “microindentation method.” When a silicon microneedle is used as an indenter that is stamped onto a metal plate and the formed indentation has the same shape as the Si microneedle formed by plastic deformation of metal plate, it is possible to fabricate a microneedle mold arranged in an array by repeating indentation formation while changing the position using a single silicon microneedle. In this research, we developed an indentation apparatus that repeatedly forms indentations on lead plates to successfully fabricate a high-density microneedle array that has the height of the silicon microneedle as the indenter.

     

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.     

Influence of mask substrate materials on resist sidewall roughness in deep X-ray lithography

Absorption of X-rays in deep X-ray lithography masks can significantly increase exposure time, harden the X-ray spectrum and lead to heating and distortion of the mask. To reduce the impact of such absorption, we have evaluated low atomic mass (low-z) materials that allow the utilization of thick substrates (>100 μm) for reliable mask fabrication. Various forms of graphite, vitreous carbon (VC), boron nitride and beryllium were chosen for testing. Transmission tests were conducted to evaluate resulting surface roughness in the X-ray resist sidewalls. We found that VC, beryllium and pyrolytic graphite all have minimal effect on the resist sidewall surface roughness; however, graphite and boron nitride both significantly increase the roughness to about 300 nm RMS. We could show that this increase in surface roughness is directly related to the crystal structure of these materials. From the tests conducted, VC proves a promising mask substrate, superior to the more expensive and hazardous beryllium that is commonly used for thick high precision masks. VC has been successfully employed as a mask substrate and corresponding resist structures are introduced.