Development of high aspect ratio X-ray parabolic compound refractive lens at Indus-2 using X-ray lithography

A synchrotron beamline dedicated to soft and deep X-ray lithography is operational on Indus-2 synchrotron source and is being used for high aspect ratio microfabrication. This X-ray lithography facility provides the access to X-ray mask fabrication, X-ray exposures and development of micro-nano structures. We report the development of planar parabolic refractive X-ray lenses in SU-8 for energy range 8–20 keV using this facility. The focussing properties of X-ray lenses were studied with synchrotron radiation in the X-ray energy range 8–20 keV on the moderate emittance machine Indus-2. A focal spot of 11 μm at 15.9 keV is obtained with a gain of 18.     

Deep X-ray lithography at ELETTRA using a central beam-stop to enhance adhesion

 In the deep X-ray lithography process adhesion of resist structures on metallic coated substrate is strongly correlated with the spectral distribution of the radiation. At ELETTRA the bending magnet radiation spectrum extends up to 20 keV which can severely increase the secondary radiation process from the metal coated resist substrate, especially when the deep lithography process is used for mask replication involving lower resist and absorber thicknesses. To reduce the proportion of high energy photons in the radiation spectrum the central part of the beam is blocked by a beam-stop acting as a low energy band-pass filter. The results of the first expositions at ELETTRA using different size beam-stops are presented and discussed. Received: 10 August 2001/Accepted: 24 September 2001     

Fabrication of X-ray imaging zone plates by e-beam and X-ray lithography

X-ray imaging and microscopy techniques have been developed in worldwide due to their capabilities of large penetration power and high spatial resolution. Fresnel zone plates is considered to be one of the most convenient optic devices for X-ray imaging and microscopy system. The zone plates with aspect ratio of 7 and 13 have been fabricated by e-beam lithography combined with X-ray lithography in this paper. Firstly, the X-ray lithography mask of zone plates with outermost zone width of 100 nm was fabricated by e-beam lithography and gold electroplating techniques. Secondly, the zone plates with gold profile thickness of 700 and 1,300 nm were replicated by X-ray lithography and gold electroplating techniques. X-ray imaging and microscopy techniques were introduced to characterize the high-aspect-ratio zone plates’ inner structures. At the X-ray energy of 7.5 keV, the first-order focusing efficiency of zone plates with gold profile thickness of 700 nm is about 8.63%.     

Polytetrafluoroethylene processing characteristics using high-energy X-ray

Polytetrafluoroethylene (PTFE) microstructures’ processing characteristics using X-ray photo dcomposition and desorption are studied in the highest energy region (2 keV to >12 keV). While the exposed surface states are seen melting and boiling from the remaining bubble structure of the irradiated surface, basic photochemistry of PTFE is also same as previous reports and high-aspect ratio structures are successfully formed. We developed new Ni stencil electroformed stencil masks and successfully fabricated first and practical example of PTFE micro fluidic parts. The characteristics of fabricated micro fluidic parts, a PTFE fluid filter for vertical fluid flow operation which works as passive valve, agreed with the calculated results. This suggests that the accuracy of patterning is adequate to apply this technique to fabricate microfluidic parts and other various microparts.     

Synchrotron laboratory for micro and nano devices: facility concept and design

SyLMAND, the Synchrotron Laboratory for Micro and Nano Devices at the Canadian Light Source, is a new deep X-ray lithography facility focusing on spectral and beam power adjustability and large exposable area formats. We present the concept of the bend magnet beamline and its main components. A double disk intensity chopper offers the unique capability of continuous average beam power reduction to a range between 261?W and approximately 0.1?W without affecting the spectrum. Continuous spectral tuning between 1?C2?keV and >15?keV photon energy is achieved using a double mirror system and low atomic number pre-filters. The radiation fan is more than 150?mm wide, allowing for full 6?? wafer exposure under vacuum conditions. We furthermore describe the vacuum window concept that was required as a result of the large exposure area and broad spectral tunability.     

Fabrication of high aspect ratio comb-drive actuator using deep X-ray lithography at Indus-2

We report microfabrication of high aspect ratio comb-drive using deep X-ray lithography at Indus-2 synchrotron radiation source. Analysis shows that the comb-drive actuator of aspect ratio 32 will produce nearly 2.5 μm displacement when 100 V DC is applied. The displacement increases as the gap between the comb finger decreases. For fabrication of comb-drive, polyimide–gold X-ray mask using UV lithography is made for the first time in India. To pattern on an 800 μm thick X-ray photoresist (PMMA) exposures are performed using our deep X-ray lithography beamline (BL-07) at Indus-2. Metallization on the selective regions of the developed X-ray photoresist with comb-drive pattern was carried out by RF sputtering. Following this the comb-drive actuator of PMMA was fabricated by one-step X-ray lithography. The comb-drive can also be used as a sensor, energy harvester, resonator and filter.     

Application of photo-etching of polytetrafluoroethylene induced by high energy synchrotron radiation to LIGA

Polytetrafluoroethylene (PTFE) microstructures’ processing characteristics using X-ray photo decomposition and desorption are studied in the highest energy region (2–12 keV). While the exposed surface states are seen melting and boiling from the remaining bubble structure of the irradiated surface, basic photochemistry of PTFE is also same as previous reports. Surface modification of PTFE from hydrophobic to hydrophilic was investigated in order to bond PTFE sheets to a brass substrate. Then, we have a successfully fabricated Ni microstructure by LIGA process using PTFE photo-etching using high energy X-ray. Proposed LIGA using SR-photo-etching of PTFE can simplify the total process, and it can ensure that dimensional errors remain small due to swelling in developer and electroplating bath.     

Micropatterning PEDOT:PSS layers

PEDOT:PSS is a conductive polymer that is used as electrodes in organic electronic devices, but also in neuronal probes and implantable devices. This material can also be used for building deformable electrodes in soft substrates for several sensing applications. However, this material being sensitive to several chemicals and moisture it is difficult to pattern microstructures using standard lithography techniques. This paper will review and show some techniques developed for patterning PEDOT:PSS thin films using both soft lithography, such as microcontact printing and shadow masking, and conventional lithography techniques. In addition of this review we present a new lithography technique using silicon nitride protection layer and an analysis and comparison of ICP RIE dry plasma etch rates of PEDOT:PSS with different gases.     

Lithography with high depth of focus by an ion projection system

Ion projection lithography is developed to generate structures with minimum feature sizes in the 100-nm range with a high pixel transfer rate. The high depth of focus (DOF) resulting from the telecentric beam path concept is also noteworthy. A silicon wafer exhibiting 200-μm-deep cavities, which are fabricated by anisotropic etching, is patterned with a grating of 0.6 μm periodicity running with identical spacings from the bottom to the top. SiO₂ serves as an inorganic ion sensitive resist. Exposed to 73 keV helium ions, SiO₂ shows an enhanced etching rate in hydrofluoric acid, the structure developing agent. The patterning techniques considered are promising for the fabrication of two-dimensional reflecting mirrors or sensoric elements distributed on spherical surfaces     

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     

Fabrication and performance of 2-D compound X-ray refractive lenses

Due to the weak refraction of X-rays in matter, a focusing or deflection of X-ray using conventional refractive optics was not feasible. However, since compound X-ray refractive lens (CXRL) with consecutive holes array was proposed, it becomes currently a noticeable issue in X-ray optics. In this paper, we report on fabrication and performance test of two types of PMMA (polymethyl methacrylate) CXRLs. Firstly, one dimensional refractive X-ray lenses of parabolic and circular shape is fabricated by LIGA process. Based on the results, we conduct a fabrication of 2-D CXRLs. Here we suggest a LIGA-self align method which doesn’t need a special align equipment and is simpler method than conventional one. Through performance tests, we show experimentally that CXRLs are novel optical components for the hard X-ray range of about 8 keV and that they have possibilities to apply the X-ray optics for micro-focusing, imaging, and lithography.     

Resist-less patterning on SiO2 by combination of X-ray exposure and vapor HF etching

We succeeded in a resist-less patterning of SiO₂/Si substrates by a combination of X-ray exposure and vapor hydrogen fluoride (HF) etching. A 2 μm thick SiO₂ layer was formed on a Si substrate by employing a thermal oxidation process. An X-ray mask consisted of a 1 μm thick Ta absorber on a 2 μm thick Si₃N₄ membrane mounted on a 1 mm thick Si frame, and a honeycomb pattern where 640 nm diameter circle dots arranged in the corners of a hexagon with a pitch of 960 nm was processed. X-ray exposure experiments were carried out on a beamline BL-4 with a peak photon energy of 2 keV at the TERAS synchrotron radiation (SR) facility. When a dose energy was 750 mAh, the transfer of the patterns was confirmed, although irradiations with different dose energy were also conducted. Moreover, heating temperatures and total etching times of SiO₂/Si substrates in vapor HF etching were changed, and the shapes of etched patterns were observed by scanning electron microscope. It was learnt that an appropriate etching time existed between 30 and 60 min. Moreover, we observed discoloration of irradiated area by SR; and this seemed to be caused by changes in the etching rate of SiO₂/Si substrates that led to the development of resist-less patterning technique.     

Surface roughness control by energy shift in deep X-ray lithography

 Previous studies show that the surface roughness of the sidewall generated by deep X-ray lithography (DXL) is a function of the photon energy of X-rays. Present study demonstrates and reveals the ideas of controlling surface roughness by tuning irradiation photon energy on the sidewall using the developing temperature. The ideas are resulted from two observations (1) X-rays of higher energy induce photoelectrons of higher energy in the resist and the corresponding scattering distance is nearly a square function of electron energy [1], and (2) high-energy X-rays are expected to induce more surface roughness and this effect has been observed by different laboratory [2]. Received: 10 August 2001/Accepted: 24 September 2001 Major part of this work was carried out in Hsinchu. This paper was presented at the Fourth International Workshop on High Aspect Ratio Microstructure Technology HARMST 2001 in June 2001.     

High-aspect-ratio microstructures fabricated by X-ray lithography of polymethylsilsesquioxane-based spin-on glass thick films

 In this paper, a process for 200 μm high-aspect-ratio micro-optical (HARM) structures fabricated by deep X-ray lithography (DXRL) of polymethylislesuioane-based spin-on glass (SOG) thick films is presented. The SOG material used in the whole procedures is polymethylsilsesquioxane (GR650), which is a kind of sol-gel derived material and can be cured at a reasonable low temperature (75 °C). A technique to cast thick GR650 films was established in the overall process. After consolidation, the GR650 thick films were machined to reach 200 μm uniformly. Then, as negative resists, the GR650 thick films were patterned directly by DXRL. X-ray irradiated regions can be selectively retained with high structural resolution by development in an organic solvent, such as methanol. Parameter screening was done to find minimum and maximum doses needed for patterning/cross-linking, to vary development time, and to explore different film thickness. The whole process is a novel of technique to create HARM structures based on SOG materials without using molds. This technique can be extended to considerably larger structural heights. Surface and bulk compositions of the irradiated films were measured by XPS and Fourier transform infrared spectroscopy. Surface quality by roughness testing system (WYKO RST) was investigated to fabricate the microstructure with a high-accuracy surface. Received: 31 October 2001/Accepted: 23 January 2002 This work was partially supported by NSF/LEQSF (2001-04)-RII-02 grant “Micro/Nanodevices for Physical, Chemical and biological Sensors”.     

CMOS X-rays detector array based on scintillating light guides

This paper describes a pixel imaging array consisting in 400 μm×400 μm photodiodes fabricated in CMOS technology. An array of scintillating CsI:Tl crystals is placed above the photodiodes. These crystals are encapsulated in aluminum walls, forming a light path that guides the visible light produced by the scintillating crystal into the photodiodes. In this way, the X-ray energy is first converted into visible light which is then detected by the photodiode at the end of each light guide. The scintillator is 800 μm thick, absorbing almost all 20 keV X-ray photons. Usually, the spatial resolution of the scintillating X-ray detectors is identical to the scintillator thickness. By using the light guides, the scintillator thickness can be increased without decreasing the spatial resolution. The increase of the scintillator thickness is desirable in order to increase the X-rays absorption efficiency. Tests carried out on the system show very promising results near 20 keV.     

Shape deviations in masks for optical structures produced by electron beam lithography

E-beam lithography is a well-known technology used in the structuring of resist for mask fabrication. In the LIGA process E-beam lithography is used to fabricate the first X-ray mask. Due to the high precision of X-ray lithography patterning errors and defects are transformed into the several hundred micrometers thick resist structures. The side walls of these high-aspect-ratio structures are often used as optical mirrors, for which very good surface properties are essential. Deviations in the shape of the side walls even far below the wavelength of the used light lead to spurious strayed or misguided light. For grating microspectrometers the requirements are particularly stringent. The width of the grating teeth does not only have to be precise, but also the grating teeth have to be positioned accurately along the entire grating width. Using LIGA microspectrometers as an example, deviations in masks and LIGA-structured side walls were studied and subsequent correlations made with the corresponding e-beam writing pattern.     

Rapid prototyping system with sub-micrometer resolution for microfluidic applications

We report on a maskless lithography rapid prototyping system for fabrication of microfluidic circuits with sub-micrometer resolution in standard i-line photoresists. The micropatterning system uses the laser direct imaging technique with a focused ultraviolet laser beam and an acousto-optic deflector to steer the beam in two dimensions. The use of an acousto-optic deflector results in high patterning speeds due to absence of moving parts and achieves sub-micrometer beam positioning precision on the photoresist surface. Patterns up to 100 cm² with well defined edges and wall smoothness on the nanometer scale can be obtained. Direct illumination of the photoresist omits high-resolution masks and alignment with the photoresist sample, in turn making the lithography process more time- and cost-effective as well as flexible, with user control throughout the process. The system provides an efficient alternative to existing photolithography techniques and is especially suitable for rapid prototyping and laboratory use.     

Fabrication of HARM structures by deep-X-ray lithography using graphite mask technology

The cost-effective fabrication process for high-aspect-ratio microstructures using X-rays depends largely on the availability and quality of X-ray masks. The fabrication of X-ray masks using commercially available graphite sheet stock, as a mask membrane is one approach that is designed to reduce cost and turnaround time. Rigid graphite offers unique properties, such as moderate X-ray transmission, fairly low cost, electrical conductivity, and the ability to be used with either subtractive or additive processes [1, 2]. This paper will demonstrate the potential of a cost-effective, rapid prototyping of high-aspect-ratio microstructures (HARMs) using graphite masks. The graphite wafer accommodates both the intermediate mask and the working mask. In order to allow a direct comparison of the graphite mask quality with other X-ray masks, the primary pattern was derived from a Ti X-ray mask using soft X-ray lithography (XRL). Received: 7 July 1999 / Accepted: 29 September 1999     

Consumption-related development in microelectroforming

 High-aspect ratio microelectroforming is one of the most challenging techniques in MEMS microfabrication. This is particularly true with plating metal into the very tall micropatterned polymer molds made by X-ray lithography for primary or secondary metal structures or metal mold inserts within the framework of the LIGA process. Among various problems are: (1) the time consumption in plating very tall parts or using microelectroplating as a replication technique; (2) the cost of material, in particular in the formation of very high-aspect-ratio absorber structures for X-ray masks in the deep and ultra-deep X-ray lithography step. Received: 7 July 2000/Accepted: 23 August 2000