Análisis de los programas

Electron-beam lithography was used to create any critical feature in the device masks because of its superior resolution and easily modified masks as compared to pho- tolithography. An electron-beam resist, Zeon ZEP520A, was used as the mask be- cause of its increased dry-etch selectivity as compared with standard PMMA. After an approximately 7 second N2 blast, the ZEP was spin-coated at 5000 rpm for 120

sec, resulting in a ∼350 nm thick film. The ZEP was then oven-baked for 20 minutes at 180◦C. A Hitachi S4300 cold-cathode field emission scanning electron microscope (SEM) was employed to raster expose the electron-beam resist, with the aid of Oliver Dial’s Bewitch software. This was accomplished by intercepting the X-Y scanning coil voltage sources and replacing it with our own voltage sources provided by a 1 MHz Digital to Analog PCI card inside a standard desktop computer. An acceler- ating voltage of 15 kV and working distance of 6 mm was always used. The beam current was dynamically adjusted to maintain a constant dose during the beam write by monitoring the beam current (∼ 1–2 nA) at the objective aperture. This relied on first measuring the beam current on the sample mount (∼ 5–35 pA) utilizing a Faraday cup and then assuming a linear relationship between the current impinging on the objective aperture and the sample mount. Because the S4300 uses a cold- cathode electron source, the tip had to be flashed every 48 hours to prevent residual ion adsorption. It was empirically determined that cold-cathode’s current stability was maximized by “flashing” the tip the night before the beam write. This allowed the tip to slowly accrue a uniform monolayer of material during the night without high voltages. A magnification of 500×, corresponding to a calibrated field of view

of 180 μm on a side, was predominantly used to write microdisks of 2.5− 40 μm radii because it was empirically found that high scanning coil voltages (>9 V) and high voltage slew rates caused raster roughness on the silicon microresonators. The physical orientation of repeated device exposure was done along the axis parallel to the “tip” of the SEM in order to fix the working distance during the beam write. In addition, the electron beam’s direction of rastering had to be aligned to the direction of travel of the X-Y stages.1

The achievable resolution and the exposure times were determined by the con- straints of the lithography tool and the resist beam used. The beam current on the sample was typically set to IB 35 pA by opening the condenser lens to a value

of 7−8. Because the scanning coils could not be reliably driven faster than ∼ 250 kHz, the rastering speed was kept at S 100−150 kHz. 350 nm thick ZEP prop- erly exposes between 37 to 39 μC/cm2 for open areas and convex features such as microdisks. However, because of the subsequent reflow, the ZEP was always overex- posed to 45μC/cm2 _{in order to remove nanoscopic traces of leftover resist that could}

have resulted in uneven resist wetting of the disk periphery. This additionally pro- vided a better averaging of the beam current over the devices resulting in smoother features. Typical single field of view patterns were Apat 4500 μm2. With these

values in hand, the physical grid resolution and pattern exposure time were found through simple dimensional analysis to be

δ= IB dose·S ≈25 nm (3.1a) tpat = dose·Apat IB ≈60 sec/pattern. (3.1b)

Although the Hitachi S4300 has a beam spot size of approximately 0.5 nm on a side, proximity effects limit the achievable resolution such that δ≈25 nm is sufficient to provide a smooth circular pattern. Typically, 10−20 patterns were written per beam write, making the total beam write time on the order of 20 minutes. This resulted in beam current variations of a couple percent from pattern to pattern. After exposure,

1_{for the sample orientation used, this corresponded to a stage rotation of 5.3−5.7 and a raster rotation of 17 on}

5 μm

(b)

beam write line

before reflow

fusing after reflow

Figure 3.3: (a) 100×magnification optical microscope image of electron-beam resist after develop. Shown is a region where electron beam rests for a short period and then tracked to the left of the image resulting in a very narrow gap in the ZEP resist. (b) Optical microscope image of the same region taken at same magnification after reflowing the resist at 160◦C for 5 minutes.

the sample was immediately transported to a fume hood for developing. The develop chemistry was 3 minutes in Zeon ZED-N50 developer, followed by a 10 second rinse in Zeon ZMD-D (or ZMD-B) solution and a final N2 dry.

After close inspection of the mask under 100×magnification in the Nikon optical microscope, the wafer was then subjected to a post-lithography bake. By suitable choice of temperature and duration, this bake can significantly reduce imperfections in the electron-beam resist pattern. Temperatures too low do not result in resist reflow, while temperatures too high can cause significant loss of resist to sublimation. A temperature high enough to allow the resist to reflow must be reached and maintained for the imperfections in the resist pattern to be reduced. The appropriate duration and temperature for the resist prepared as described above was empirically determined to be 5 minutes at 160◦C. The experimental standard that was used in order to measure resist reflow used a fortuitiously narrow gap in electron-beam resist, as seen in Figure 3.3(a). The gap in the resist is caused by the slow stage translation in between patterns with the electron beam still being fired at the sample. The result is a sub-micron gap in the electron-beam resist that extends near but not affecting the

10 μm

Figure 3.4: (a) 100×magnification optical microscope image of electron-beam resist after develop and reflow at 160◦C for 5 minutes. Shown is a 10 μm radius microdisk etch pattern.

device patterns. Five minutes at 160◦C was determined to be the minimum time and temperature that was necessary to allow this resist gap to fuse together (as shown in Fig. 3.3(b)) when the stage was translating at a linear rate (assuming IB ∼ 30–35

pA). After the reflow process, the roughness in the patterns was greatly reduced, and the sidewall angle was reduced from 90◦ to approximately 45◦.

Figure 3.4 shows an optical image of a typical electron-resist mask after reflow, where no discernible imperfections could be observed at visible wavelengths. While increasing the minimum radii of curvatures that were possible, the reflow process created nearly surface-tension limited patterns in a fashion similar to that used to create silica microspheres [29] or microtoroids [31]. The contact angle that the resist makes with the surface is a function of the materials used, the size of the microdisks, and the amount of remaining solvent in the resist. It was found empirically that the latter had the most drastic effect on the reflow. It was for this reason that the whole lithography process, from spin-coating through resist reflow, was treated as if the polymeric resists were continuously evaporating. Strict serial lithography

4 8 4 8

100 nm 100 nm

Figure 3.5: SEM micrograph of a 5 μm radii microdisk after mask reflow and low bias voltage ICP/RIE etching. (a) The optimized etch using 12.0 sccm each of C₄F₈and SF₆. (b) An unoptimized etch using 14.5 sccm C₄F₈and 12.0 sccm SF₆, resulting in heavy polymerization on the sidewalls.

processing of samples and a careful choreography of transfer times was utilized to ensure reproducible reflow results.