Conclusió de cada proposta

In order to investigate the combined effects of shear loading and electrical bias on N- UNCD and Pt, a method to shear contacts while applying a voltage for a period of time over a

selected region using C-AFM was developed. The test consists of repeatedly rastering a Pt- coated probe tip over a square surface region while tracking changes to conductivity scanned surface region while periodically evaluating the integrity of the probe tip. Fig. 2.14 shows a high level overview of the test steps.

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Figure 2.14: The AFM protocol used for evaluating changes to surface conductivity of N-UNCD and Pt exposed to load, shear, and electrical bias. Scans were performed at a new location for each probing scan and modification scan group. A total of i locations were scanned. Probing scans were performed before and after each modification scan to check electrical integrity of the probe tip. A total number of j modification scans are performed at each modification location.

Testing began with the insertion of the probe and sample into the AFM. The deflection sensitivity and the stiffness of the probe were initially overestimated to prevent unintended large loads from being applied during the engage process. A dAFM-based attractive-mode engage

Probe/sample inserted into AFM. Soft engage of tip and surface using dAFM. Cantilever stiffness and deflection sensitivity

determined.

System purge.

Move to new location.

False (out-of-contact) scan to minimize drift.

Evaluate baseline offset of probe.

Probing scan under voltage Vp.

Modification scan under voltage Vm. Repeat for j scans jth scan Repeat for i locations IV map.

process, like that described in section 2.6.1 was then used to bring the tip and surface into contact without heavily cycling or disturbing the electrical integrity of the tip. The deflection sensitivity of the probe was fit from the slope of the in-contact portion of a lightly-loaded FvD measurement. The probe was then disengaged and thermal calibration (see section 2.1.4) was performed to determine the stiffness of the probe.

Scanning of the surface was then undertaken to evaluate the conductivity of the probe tip or to evaluate the response of the surface to prolonged exposure of load, shear, and electrical bias. The former is referred to here as a probing scan and the latter a modification scan. The probing scans were used to track probe tip conductivity at a new surface location to observe for loss of conductive tip material and to regenerate probe tip conductivity in the event that tribofilms resulting from modification scans adhered to the tip. The relative locations of probing and

modification scans are shown in figure 2.15. A probing scan was performed before and to the left of every modification scan. A final probing scan was also performed to evaluate the final state of the tip. A gap of 1 μm was included between all scans so that any tribofilms or contaminants formed during scanning at one location would not affect evaluation at the next scan location.

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Figure 2.15: The relative location of probing and modification scans when testing the effect of load, shear, and electrical bias for Pt and N-UNCD contacts. A probing scan to evaluate the tip conductivity was performed before each group of modification scans. Scan locations are offset by 1 μm from one-another so that resultant tribofilms do not spread between test locations. The voltage during scanning is indicated at each location as the probing voltage, Vp, or the modification voltage at the ith test location, Vm,i. The tests terminated with a final probing scan.

The general process for both probing scans and modification scans involved four main components. The tip was first moved to a new, untouched location of the sample surface. A scan over the area of interest and for a duration of ~7 min. was then performed with the tip retracted several μm from the surface in order to reduce system drift at the new location. An FvD

measurement was then performed to evaluate the baseline load offset from the out-of-contact

V_p

V_m,1

V_p

V_p

V_p

V_m,2

V_m,n

1 x 1μm2

1

μm

1

μm

portion of interaction. This ensured that the load applied to the tip-surface was not subject to deflection drift of cantilever and that quoted loads were within several percent of those intended. A single probing scan under probing voltage Vp or multiple scans under modification scan voltage

Vm were then performed. Vp was selected to be just sufficient to yield statistically significant conductivity data on the probe state. The cantilever deflection offset was re-evaluated before each modification scan. An IV map was then taken inside the scan area after a probing scan or after a pre-determined number of contiguous modification scans to evaluate changes to the current-voltage response of the interface.

Both the probing scans and modification scans were performed over a 1 x 1 μm2 _area. The size of the area was chosen to be large enough to extract statistically-relevant conductivity data and to exceed drift of the MFP-3D AFM used for these studies (<100 nm per scan area) and yet small enough to ensure large electrical power density through the contact per unit scan time. The probing and modification scans were both performed at a rate of 0.2 Hz with 64 scan lines in the slow scan direction and 1024 points in the fast scan direction. All scans were performed at the same load for a specific probe, ranging from 25 – 50 nN depending on the particular test. Friction and conductivity in both the trace and retrace directions was collected with current amplification provided by the logarithmic amplifier described in section 2.2.

Two surfaces were interrogated under load, shear, and electrical bias using Pt-coated AFM probes. N-UNCD in the iPlas system at Argonne National Laboratory as described in section 2.5.2. Because of the age of the sample (several years), the sample was cleaned via sonication for 20 minutes each in acetone, methanol, and IPA. This was followed by drying using N2 blowoff from a nitrogen dewar. A Pt surface similar to that tested in section 3.6 was also interrogated in an as-deposited state within several months of deposition and after storage in an N2-purged dessicator. Contact mode probes of style PPP-CONT (Nanosensors, Neuchatel, Switzerland) and nominal stiffness of 0.2 nN/nm were coated with 70 – 85 nm of Pt using the Explorer14 sputterer. Deposition was performed on both the back and tip-side of the probes.

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In order to study the effect of operating environment and electrical power on surface degradation of Pt/Pt and Pt/N-UNCD, tests were run in both laboratory air and under N2 purging with Vm ranging from 0.25 to 8 V. In all cases, Vm was increased from Vm,1 to Vm,i, where i represents the total number of modification locations. A total of 7 and 12 contiguous modification scans at each location were used when investigating Pt/N-UNCD and Pt/Pt interfaces,

respectively.