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.     

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.     

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.     

Polyimide-based X-ray masks with advanced performance of pattern accuracy and thermal stability

Polyimide-based X-ray masks which are generated by optical lithography and electroplating of gold absorbers on a polyimide mask membrane gain attention as low cost masks. The organic membranes generally have problem of (1) pattern edge sharpness, (2) miniaturization of pattern and (3) thermal stability. To make the masks commodity in deep and accurate lithography area, Optnics Precision, Japan, has overcome the above difficulties and realized the masks with advanced performance of pattern accuracy and thermal stability by improving the making process and the material. Good results were obtained in the exposure experiment that used this mask. When this X-ray mask is combined with the electroforming technique and the material development technique that Optnics has, the application to various fields like an industrial field and medical field can be expected.     

New type X-ray mask fabricated using inductively coupled plasma deepetching

 The fabrication of X-ray masks is a critical and challenging process in LIGA technique. As inductively coupled plasma (ICP) deepetching appears to be the most suitable source for deep silicon etching, we fabricated a new type X-ray mask using this technique. In comparison with other types of X-ray masks, the mask we fabricated has the advantages of its low cost and its simple fabrication process. Desired microstructures have also been fabricated using this new type X-ray mask in LIGA technique. Received: 17 July 2000/Accepted: 4 September 2000     

Direct, high throughput LIGA for commercial applications: a progress report

Direct LIGA; LIGA without injection molding; has the potential to become a cost effective, high throughput form of LIGA. The process requires high energy photons; near 20,000 eV; which are best produced in facilities such as the X-ray ring at Brookhaven National Laboratory. The increased absorption lengths over lower energy photons eliminates the need for a membrane type X-ray mask. This in turn facilitates very large area X-ray masks fabricated from standard silicon wafers with 20 μm gold absorbers. The absorption length increase in PMMA to 2 cm is used to implement stacked PMMA exposures in which 1 mm thick PMMA layers are used to produce exposed PMMA sheets. These sheets are eventually solvent bonded to working substrates with plating bases. New high energy X-ray masks have been developed. Two exposure stations at Brookhaven are operational. The recently commissioned manufacturing exposure station which uses a 22 inch scanner which can expose four separate PMMA-mask combination is in the testing phase. Received: 7 July 1999/Accepted: 30 July 1999     

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.     

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     

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.     

Fabrication of high aspect ratio nano gratings using SR lithography

In this paper, the fabrication technique for high-aspect-ratio diffractive optical element (DOE) is introduced. The 500 nm-width and 1,000 nm-width line-and-space pattern has been successfully fabricated. It was fabricated by synchrotron radiation (SR) lithography for the application of nano gratings, and poly-methylmethacrylate (PMMA) was used as X-ray resist. The nanoscale grating with the aspect ratio of 4.4 and 2.2 was achieved. So far, there are a number of reported techniques for fabrication of DOEs yet the height of those gratings is not sufficient. Therefore, we have attempted to investigate the fabrication of high-aspect-ratio nano gratings by a high-resolution X-ray lithography using SR source at Ritsumeikan University, Japan. Nevertheless, the evaluation of various factors influencing the high-aspect-ratio structure fabricated by our recommended technique is discussed. So far the fabricating process, such as, proximity gap of exposure, the exposure dosage, and the development time have been optimized to fabricate the gratings.     

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     

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     

A new UV sensitive positive resist for X-ray masks manufacture

LIGA is a well-established process to fabricate metallic micro parts with high resolution, high precision and very low sidewall roughness by means of X-ray lithography and electroplating. The availability of a precise X-ray mask is a precondition for the final precision of the manufactured micro parts. Typical mask substrate materials, e.g. beryllium, carbon based foils, Si₃N₄ or SiC show different disadvantages such as low X-ray transparency or high toxicity or high prices or low conductivity or high thermal expansion or surface porosity causing X-ray scattering. For the fabrication of X-ray masks, PMMA with its unique features such as high aspect ratio patterns with high precision, exhibits low sensitivity and the layers preparation is not easy. SU-8, an epoxy-based UV and X-ray sensitive, chemically amplified, negative tone photoresist exhibits high aspect ratio patterns with vertical sidewalls. The difficult remove of the resist after the electroplating process significantly hinders the inspection of the fabricated X-ray mask. We present the use and suitability of an UV sensitive, chemically amplified, viscous, aqueous-alkaline developable, and easy removable positive tone photoresist, XP mr-P 15 AV, exhibiting high aspect ratio patterns with vertical sidewalls for the fabrication of X-ray masks by means of UV lithography on vitreous carbon substrates.     

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.     

Low cost transparent SU-8 membrane mask for deep X-ray lithography

Deep X-ray lithography masks require good transparency and mechanical resistance to the intense synchrotron X-ray beam, large active areas (cm)² and compatibility with the standard fabrication processes (optical lithography and gold electroforming). Moreover higher resolution can be achieved with low roughness flat membrane. Furthermore multiple aligned exposures require an optically transparent material. Diamond like Carbon membranes fulfill those requirements but have a prohibitive cost. Our approach consists in using an SU-8 epoxy resin layer as membrane material. In this communication the different steps of the fabrication process will be presented, as well as the results obtained using the mask for particular applications.     

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     

Mask design compensation for sloped sidewall structures fabricated by X-ray lithography

We have investigated and report in this paper the factors influencing the deformation caused by the dependence between the absorbed X-ray energy on the resist and the shape of the absorber on the X-ray mask. Based on the measurement of errors that occurred during the transferring process between the 2-D shape of mask pattern and the resulting wall of the fabricated 3-D structure, we have developed newly useful graphical data on the absorbed X-ray energy, dosage, and shape of a microstructure. As a result, it is being reported as a method for compensation for the deformed shape after the fabrication of a quadruplets-microneedle. We have considered a number of factors affecting the deformation and finally realized that the effect of a dose–depth nonlinear curve is the most possible cause. Without the compensation of the mask design, we could observe the deformed shapes of the sloped sidewall on the exposed structures. Polymethylmethacrylate microneedle structures fabricated by X-ray lithography with an additional plane-pattern to cross-section transfers technique are directly influenced by the absorber on the X-ray mask pattern. The sidewall of the microneedle was improved by changing the mask pattern from a double right-triangular pattern to a double semi-circular pattern, modeled by comparing the results from a mask-pattern and the actual structure.     

Manufacture of a micro-sized piezoelectric ceramic structure using a sacrificial polymer mold insert

There have been technical limitations to manufacture microstructures due to difficulty of demolding during replication process of high aspect ratio microstructure in mass production technologies. In the present study, the fabrication of a novel sacrificial micro mold insert and powder injection molding process using such a micro mold insert is proposed and developed. It utilizes a synchrotron radiation to fabricate the shape of polymer based sacrificial mold inserts and then these mold inserts were exposed at X-ray once more to adjust its solubility. This second X-ray exposure facilitates dissolving of mold inserts instead of demolding process which have difficulties like pattern collapses or defects in case of precise replication process. In this manner, severe problems of demolding process in conventional mass production technologies can be efficiently overcome. To verify the usefulness of the proposed technique, polymer based micro mold inserts with several tens of micrometer sized structure for piezoelectric sensor applications were fabricated using X-ray micromachining process radiated synchrotron. The solubility of mold inserts were optimized by the second X-ray exposure without an X-ray mask and then subsequent powder injection molding process was utilized with a piezoelectric based material. Finally, piezoelectric ceramics with micrometer-scale and high aspect ratio of 5 were successfully fabricated, verifying that the present sacrificial mold system is useful for the precise replication process such as the fabrication of microstructure with high aspect ratio or complicated structure.     

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.     

Fabrication of antiscatter grids and collimators for X-ray and gamma-ray imaging by lithography and electroforming

Creatv MicroTech has developed unique fabrication techniques to make high precision, high-aspect-ratio metal microstructures to custom specifications. A lithography based fabrication method permits precise fabrication of various microstructures. Collimators and antiscatter grids with continuous, smooth, thin, parallel or focused septa have been fabricated using deep X-ray and optical lithography, combined with metal electroforming. Microfabrication of high-aspect-ratio structures, especially of relatively large areas, presents many challenges: specialized mask design and X-ray mask fabrication; resist preparation, optimal exposure parameters, post-exposure processing, electroforming, polishing, and final assembly. Here, we present microstructures of various designs that we fabricated and describe the challenges that had to be overcome.