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Recent progress in the functionalization of atomic force microscope ...

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2236 Zhou et al.: <strong>Recent</strong> <strong>progress</strong> <strong>in</strong> <strong>the</strong> <strong>functionalization</strong> <strong>of</strong> AFM probes 2236FIG. 4. a Probe hav<strong>in</strong>g a sharp end, formed by dry etch<strong>in</strong>g <strong>the</strong> siliconnitride cantilever us<strong>in</strong>g a mask that extends only part <strong>of</strong> <strong>the</strong> way to <strong>the</strong> top<strong>of</strong> <strong>the</strong> pyramidal AFM tip. The sensor wire runs around <strong>the</strong> edge <strong>of</strong> <strong>the</strong>released probe, and is self-aligned to <strong>the</strong> edge s<strong>in</strong>ce excess metal disappearswhen <strong>the</strong> probe is released. b Thermocouple us<strong>in</strong>g double self-alignmentso that <strong>the</strong> size <strong>of</strong> <strong>the</strong> junction is limited by <strong>the</strong> hole beh<strong>in</strong>d <strong>the</strong> apex <strong>of</strong> <strong>the</strong>tip and <strong>the</strong> junction is self-aligned to <strong>the</strong> end <strong>of</strong> <strong>the</strong> tip as before. The probeis shown before <strong>the</strong> silicon substrate has been removed by a f<strong>in</strong>al wet etchprocess. c Double self-aligned <strong>the</strong>rmal resistor probe fabricated us<strong>in</strong>g <strong>the</strong>same method as <strong>the</strong> <strong>the</strong>rmocouple <strong>in</strong> b. The probe is shown after release.vantages. First, <strong>the</strong>y must be made <strong>in</strong>dividually, which istime consum<strong>in</strong>g and results <strong>in</strong> lack <strong>of</strong> reproducibility betweenprobes. Second, if a fiber is to be pulled <strong>in</strong> such a waythat <strong>the</strong> aperture is small, it is hard to prevent <strong>the</strong> taper angleat <strong>the</strong> end <strong>of</strong> <strong>the</strong> fiber from be<strong>in</strong>g ra<strong>the</strong>r shallow. The effect<strong>of</strong> this is that such probes lose a significant amount <strong>of</strong> <strong>the</strong>light <strong>in</strong> <strong>the</strong> cut<strong>of</strong>f metallic optical wave guide lead<strong>in</strong>g up to<strong>the</strong> aperture, as well as suffer<strong>in</strong>g <strong>the</strong> large losses associatedwith <strong>the</strong> aperture itself. F<strong>in</strong>ally, <strong>the</strong> fiber is ra<strong>the</strong>r stiff alongits length, so that <strong>force</strong> regulation must be accomplished by<strong>the</strong> use <strong>of</strong> shear-<strong>force</strong> regulation ra<strong>the</strong>r than by measurement<strong>of</strong> <strong>the</strong> deflection <strong>of</strong> a cantilever, which is more reliable. Thisobjection has been overcome to some extent by <strong>the</strong> use <strong>of</strong> abent fiber probe.More recently SNOM probes based on <strong>the</strong> use <strong>of</strong> micromach<strong>in</strong>edAFM probes have been realized. 20,21 EBL probe<strong>functionalization</strong> technology is well suited to <strong>the</strong> production<strong>of</strong> such probes. The process which has been adopted to date<strong>in</strong>volves <strong>the</strong> def<strong>in</strong>ition <strong>of</strong> a simple physical hole at <strong>the</strong> apex<strong>of</strong> <strong>the</strong> AFM probe by use <strong>of</strong> dry etch<strong>in</strong>g. 22 After release <strong>the</strong>entire probe, <strong>in</strong>clud<strong>in</strong>g <strong>the</strong> aperture, is coated with alum<strong>in</strong>umus<strong>in</strong>g a vacuum evaporator. Previous attempts to fabricatesuch probes us<strong>in</strong>g a palladium layer <strong>in</strong> which an aperturewas def<strong>in</strong>ed before release 5 were unsuccessful due to stresses<strong>in</strong> <strong>the</strong> ra<strong>the</strong>r thick Pd layer which were necessary for adequatescreen<strong>in</strong>g. A particular problem with this technique,however, is that <strong>the</strong> etch<strong>in</strong>g <strong>of</strong> a small hole through a siliconnitride layer that is thick enough to act as an adequate AFMprobe is difficult. For this reason, <strong>the</strong> silicon nitride around<strong>the</strong> tip is first th<strong>in</strong>ned from approximately 500 nm <strong>in</strong> thicknessto some 200 nm before aperture def<strong>in</strong>ition <strong>the</strong> ovalshape is approx 50 m across around <strong>the</strong> pyramid <strong>in</strong> Fig.J. Vac. Sci. Technol. A, Vol. 17, No. 4, Jul/Aug 1999


2237 Zhou et al.: <strong>Recent</strong> <strong>progress</strong> <strong>in</strong> <strong>the</strong> <strong>functionalization</strong> <strong>of</strong> AFM probes 2237FIG. 5. a Overview <strong>of</strong> a SNOM probe with a large aperture. The cantilever shape has been extended around <strong>the</strong> base <strong>of</strong> <strong>the</strong> pyramid to form a shield aga<strong>in</strong>stscattered light. The silicon nitride over <strong>the</strong> pyramidal tip has been th<strong>in</strong>ned to enable <strong>the</strong> aperture which is narrow to be etched all <strong>the</strong> way through. b Apex<strong>of</strong> a pyramid show<strong>in</strong>g a 150 nm diam SNOM aperure. c Effect <strong>of</strong> metallization granularity on <strong>the</strong> aperture shape. The aperture is seen to be rough on <strong>the</strong>scale <strong>of</strong> <strong>the</strong> gra<strong>in</strong> size, approximately 50 nm. Note <strong>the</strong> smooth shape <strong>of</strong> <strong>the</strong> underly<strong>in</strong>g silicon nitride substrate. d Somewhat smoo<strong>the</strong>r aperture pr<strong>of</strong>ileresult<strong>in</strong>g from <strong>the</strong> use <strong>of</strong> a cladd<strong>in</strong>g metal conta<strong>in</strong><strong>in</strong>g 5% w/w <strong>of</strong> copper.5a. S<strong>in</strong>ce light scatter<strong>in</strong>g around <strong>the</strong> probe was also foundto be troublesome, <strong>the</strong> cantilever has been extended for somedistance to form a screen around <strong>the</strong> probe. Such probes havebeen successfully scanned without <strong>force</strong> feedback for extendedperiods. Due to <strong>the</strong>ir low vertical stiffness and <strong>the</strong>large size <strong>of</strong> <strong>the</strong> probe apex region <strong>the</strong> local <strong>force</strong> on any part<strong>of</strong> <strong>the</strong> probe is low. Wear on <strong>the</strong> probe or on <strong>the</strong> substrateusually GaAs has <strong>the</strong>refore been found to be reduced to acompletely <strong>in</strong>significant level regardless <strong>of</strong> <strong>the</strong> external <strong>force</strong>applied to <strong>the</strong> probe. This significantly simplifies operation<strong>of</strong> <strong>the</strong> SNOM <strong>microscope</strong>, s<strong>in</strong>ce deflection measurement systemsgenerally based on bright optical sources such as diodelasers are not required. Due to <strong>the</strong> lack <strong>of</strong> any cut<strong>of</strong>f region<strong>in</strong> front <strong>of</strong> <strong>the</strong> probe aperture itself, measurements <strong>of</strong> totallight throughput for a 150 nm aperture Fig. 5b <strong>in</strong> red light633 nm <strong>of</strong> approximately one part <strong>in</strong> 10 3 has been rout<strong>in</strong>elyobta<strong>in</strong>ed. It should be noted that <strong>the</strong>se throughputs were obta<strong>in</strong>ed<strong>in</strong> a simple confocal transmission system hav<strong>in</strong>g illum<strong>in</strong>ationand collection optics operat<strong>in</strong>g at approximate numericalapertures NAs <strong>of</strong> 0.2–0.3. The SNOM probe itselfis capable <strong>of</strong> accommodat<strong>in</strong>g an illum<strong>in</strong>at<strong>in</strong>g beam <strong>of</strong> 0.55NA, which would lead to approximate quadrupl<strong>in</strong>g <strong>of</strong> <strong>the</strong>illum<strong>in</strong>at<strong>in</strong>g <strong>in</strong>tensity at <strong>the</strong> aperture.The limitation on resolution <strong>of</strong> <strong>the</strong> probes is def<strong>in</strong>ed by<strong>the</strong> granularity <strong>of</strong> <strong>the</strong> coat<strong>in</strong>g metal 99.999% pure alum<strong>in</strong>um.As may be seen from Fig. 5c, <strong>the</strong> aperture is roughJVST A - Vacuum, Surfaces, and Films


2238 Zhou et al.: <strong>Recent</strong> <strong>progress</strong> <strong>in</strong> <strong>the</strong> <strong>functionalization</strong> <strong>of</strong> AFM probes 2238FIG. 6. a 100 nm junction bismuth Hall probe magnetometer fabricated on a silicon tip. Leads to <strong>the</strong> junction are made <strong>of</strong> gold to reduce access resistanceand to allow bond<strong>in</strong>g. b Junction size <strong>of</strong> a Hall probe fabricated as a lithographic test. The junction size is estimated to be 50 nm. c Completeelectromagnetic Hall probe consist<strong>in</strong>g <strong>of</strong> a s<strong>in</strong>gle-turn electromagnetic coil at <strong>the</strong> apex <strong>of</strong> an AFM probe. d Close-up view <strong>of</strong> <strong>the</strong> probe shown <strong>in</strong> c. Thes<strong>in</strong>gle-turn coil consists <strong>of</strong> an approximately 50 nm wide wire which reaches a maximum diameter <strong>of</strong> approximately 250 nm. The wires lead<strong>in</strong>g to <strong>the</strong> coilare written as close toge<strong>the</strong>r as possible approx 100 nm spac<strong>in</strong>g center to center to m<strong>in</strong>imize stray magnetic fields.on <strong>the</strong> scale <strong>of</strong> <strong>the</strong> metal gra<strong>in</strong> size 50–70 nm, even though<strong>the</strong> nitride aperture is far better def<strong>in</strong>ed than that. <strong>Recent</strong>experiments us<strong>in</strong>g an alloy (Al 0.95 Cu 0.05 ) hav<strong>in</strong>g similar opticalproperties to those <strong>of</strong> pure alum<strong>in</strong>um are promis<strong>in</strong>gFig. 5d.C. Magnetic sensorsThe use <strong>of</strong> silicon cantilevers allows <strong>the</strong> operation <strong>of</strong>functionalized probes <strong>in</strong> <strong>the</strong> attractive regime. Examples <strong>of</strong>two such probes are shown <strong>in</strong> Fig. 6. Figure 6a shows aHall-bar probe, fabricated from bismuth, situated at <strong>the</strong> apex<strong>of</strong> a silicon attractive-mode probe. Such probes are expectedto have advantages over <strong>the</strong> more commonly used Hallprobes, which are fabricated on flat, solid substrates, s<strong>in</strong>ce<strong>the</strong> former have better access and are also able to operate <strong>in</strong>a controlled fashion <strong>in</strong> close proximity to <strong>the</strong> specimen us<strong>in</strong>g<strong>force</strong> feedback. Functional Hall probe sensors have been fabricateddown to a 100 nm junction size Fig. 6a, and litho-J. Vac. Sci. Technol. A, Vol. 17, No. 4, Jul/Aug 1999

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