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Register a new userSelective etching of PDMS: etching as a negative tone resist
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Szabolcs Szilasi Dr
Publication date
2017
fields
Physics
and research's language is
English
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In this work authors present for the first time how to apply the additive-free, cured PDMS as a negative tone resist material, demonstrate the creation of PDMS microstructures and test the solvent resistivity of the created microstructures. The PDMS layers were 45 um and 100 um thick, the irradiations were done with a focused proton microbeam with various fluences. After irradiation, the samples were etched with sulfuric acid that removed the unirradiated PDMS completely but left those structures intact that received high enough fluences. The etching rate of the unirradiated PDMS was also determined. Those structures that received at least 7.5*10^15 ion*cm-2 fluence did not show any signs of degradation even after 19 hours of etching. As a demonstration, 45 um and 100 um tall, high aspect ratio, good quality, undistorted microstructures were created with smooth and vertical sidewalls. The created microstructures were immersed into numerous solvents and some acids to test their compatibility. It was found that the unirradiated PDMS cannot, while the irradiated PDMS microstructures can resist to chloroform, n-hexane, toluene and sulfuric acid. Hydrogen fluoride etches both the unirradiated and the irradiated PDMS.
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Although, poly(dimethylsiloxane) (PDMS) is a widely used material in numerous applications, such as micro- or nanofabrication, the method of its selective etching has not been known up to now. In this work authors present two methods of etching the pure, additive-free and cured PDMS as a positive resist material. To achieve the chemical modification of the polymer necessary for selective etching, energetic ions were used. We created 7 um and 45 um thick PDMS layers and patterned them by a focused proton microbeam with various, relatively large fluences. In this paper authors demonstrate that 30 wt% Potassium Hydroxide (KOH) or 30 wt% sodium hydroxide (NaOH) at 70 oC temperature etch proton irradiated PDMS selectively, and remove the chemically sufficiently modified areas. In case of KOH development, the maximum etching rate was approximately 3.5 um/minute and it occurs at about 7.5*10^15 ion*cm-2. In case of NaOH etching the maximum etching rate is slightly lower, 1.75 um/minute and can be found at the slightly higher fluence of 8.75*10^15 ion*cm-2. These results are of high importance since up to this time it has not been known how to develop the additive-free, cross-linked poly(dimethylsiloxane) in lithography as a positive tone resist material.
A chemical etching method was developed for (110) and (001) NdGaO3 single crystal substrates in order to obtain an atomically flat GaO2-x - terminated surface. Depending on the surface step density the substrates were etched in pH-controlled NH4F- or NH4Cl-based solutions, followed by an annealing step at temperatures of 800-1000oC, in air or in oxygen flow, in order to recrystallize the surface. Atomic Force Microscopy (AFM) and high-pressure Reflection High Energy Electron Diffraction (RHEED) were used to analyse the surface morphology of the samples after every treatment. Studies on the chemistry and characteristics of the terminating layer showed that the chemically etched NdGaO3 substrate surface has a GaO2-x termination and that the (110) and (001) NdGaO3 surfaces are characterized by a different free surface energy, which is lower for latter.
A digital etching method was proposed to achieve excellent control of etching depth. The digital etching characteristics of p+ Si and Si0.7Ge0.3 using the combinations of HNO3 oxidation and BOE oxide removal processes were studied. Experiments showed that oxidation saturates with time due to low activation energy. A physical model was presented to describe the wet oxidation process with nitric acid. The model was calibrated with experimental data and the oxidation saturation time, final oxide thickness, and selectivity between Si0.7Ge0.3 and p+ Si were obtained. The digital etch of laminated Si0.7Ge0.3/p+ Si was also investigated. The depth of the tunnels formed by etching SiGe layers between two Si layers was found in proportion to digital etching cycles. And oxidation would also saturate and the saturated relative etched amount per cycle (REPC) was 0.5 nm (4 monolayers). A corrected selectivity calculation formula was presented. The oxidation model was also calibrated with Si0.7Ge0.3/p+ Si stacks, and selectivity from model was the same with the corrected formula. The model can also be used to analyze process variations and repeatability. And it could act as a guidance for experiment design. Selectivity and repeatability should make a trade-off.
Despite the fact that the resolution of conventional contact/proximity lithography can reach feature sizes down to ~0.5-0.6 micrometers, the accurate control of the linewidth and uniformity becomes already very challenging for gratings with periods in the range of 1-2 {mu}m. This is particularly relevant for the exposure of large areas and wafers thinner than 300{mu}m. If the wafer or mask surface is not fully flat due to any kind of defects, such as bowing/warpage or remaining topography of the surface in case of overlay exposures, noticeable linewidth variations or complete failure of lithography step will occur. We utilized the newly developed Displacement Talbot lithography to pattern gratings with equal lines and spaces and periods in the range of 1.0 to 2.4 {mu}m. The exposures in this lithography process do not require contact between the mask and the wafer, which makes it essentially insensitive to surface planarity and enables exposures with very high linewidth uniformity on thin and even slightly deformed wafers. We demonstrated pattern transfer of such exposures into Si substrates by reactive ion etching using the Bosch process. An etching depth of 30 {mu}m or more for the whole range of periods was achieved, which corresponds to very high aspect ratios up to 60:1. The application of the fabricated gratings in phase contrast x-ray imaging is presented.
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