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null (Ed.)Minor and trace elements in diamond-like carbon (DLC) are difficult to quantify using SIMS analysis because minor elemental and structural variations can result in major matrix effects even across individual, cm-sized samples. While this material is most commonly used for tribological coatings where minor element composition is not of critical importance, it is being increasingly used in electronic devices. However, it is a unique application that spurred this work: anhydrous, tetrahedrally-coordinated DLC (ta-C) was used as a solar wind (SW) collector material in the Genesis solar-wind sample return mission (NASA Discovery 5). So, for ∼15 years, we have been working on attaining accurate and precise measurement of minor and trace elements in the Genesis DLC using SIMS to achieve our mission goals. Specifically, we have learned to deal with relevant matrix effects in our samples, ion implants into ta-C. Our unknown element for quantification is SW Mg, a low-dose (1.67 × 10 12 at cm −2 ; ∼6 μg g −1 24 Mg), low-energy (∼24 keV average energy) implant; our standard is a high-dose (∼1 × 10 14 at cm −2 of both 25 Mg, 26 Mg) 75 keV laboratory implant for which the absolute 26 Mg/ 25 Mg ratio had been measured to account for variable instrumental mass fractionation. Analyses were performed using O 2 + primary ions having both a low impact energy and a current density of ∼2 × 10 14 ions per cm 2 . Although our unknown was solar wind, the method is applicable to many situations where minor elements in DLC need to be quantified. Recommendations are presented for modifying this data-reduction technique for other SIMS conditions.more » « less
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Rationale Back‐side thinning of wafers is used to eliminate issues with transient sputtering when analyzing near‐surface element distributions. Precise and accurate calibrated implants are created by including a standard reference material during the implantation. Combining these methods allows accurate analysis of low‐fluence, shallow features even if matrix effects are a concern.
Methods Implanted Na (<2.0 × 1011ions/cm2, peaking <50 nm) in diamond‐like carbon (DLC) film on silicon (solar wind returned by NASA's Genesis mission) was prepared for measurement as follows. Implanted surfaces of samples were epoxied to wafers and back‐side‐thinned using physical or chemical methods. Thinned samples were then implanted with reference ions for accurate quantification of the solar wind implant. Analyses used a CAMECA IMS 7f‐GEO SIMS in depth‐profiling mode.
Results Back‐side‐implanted reference ions reduced the need to change sample mounts or stage position and could be spatially separated from the solar wind implant even when measuring monoisotopic ions. Matrix effects in DLC were mitigated and the need to find an identical piece of DLC for a reference implant was eliminated. Accuracy was only limited by the back‐side technique itself.
Conclusions Combining back‐side depth profiling with back‐side‐implanted internal standards aides quantification of shallow mono‐ and polyisotopic implants. This technique helps mitigate matrix effects and keeps measurement conditions consistent. Depth profile acquisition times are longer, but if sample matrices are homogeneous, procedural changes can decrease measurement times.