In-situ growth optimization in focused electron-beam induced deposition

We present the application of an evolutionary genetic algorithm for the in-situ optimization of nanostructures prepared by focused electron-beam-induced deposition. It allows us to tune the properties of the deposits towards highest conductivity by using the time gradient of the measured in-situ rate of change of conductance as fitness parameter for the algorithm. The effectiveness of the procedure is presented for the precursor W(CO)6 as well as for post-treatment of Pt-C deposits obtained by dissociation of MeCpPt(Me)3. For W(CO)6-based structures an increase of conductivity by one order of magnitude can be achieved, whereas the effect for MeCpPt(Me)3 is largely suppressed. The presented technique can be applied to all beam-induced deposition processes and has great potential for further optimization or tuning of parameters for nanostrucures prepared by FEBID or related techniques

Directed deposition of silicon nanowires using neopentasilane as precursor and gold as catalyst

In this work the applicability of neopentasilane (Si(SiH3)4) as a precursor for the formation of silicon nanowires by using gold nanoparticles as a catalyst has been explored. The growth proceeds via the formation of liquid gold/silicon alloy droplets, which excrete the silicon nanowires upon continued decomposition of the precursor. This mechanism determines the diameter of the Si nanowires. Different sources for the gold nanoparticles have been tested: the spontaneous dewetting of gold films, thermally annealed gold films, deposition of preformed gold nanoparticles, and the use of “liquid bright gold”, a material historically used for the gilding of porcelain and glass. The latter does not only form gold nanoparticles when deposited as a thin film and thermally annealed, but can also be patterned by using UV irradiation, providing access to laterally structured layers of silicon nanowires

A hybrid polymer/ceramic/semiconductor fabrication platform for high-sensitivity fluid-compatible MEMS devices with sealed integrated electronics

Active microelectromechanical systems can couple the nanomechanical domain with the electronic domain by integrating electronic sensing and actuation mechanisms into the micromechanical device. This enables very fast and sensitive measurements of force, acceleration, or the presence of biological analytes. In particular, strain sensors integrated onto MEMS cantilevers are widely used to transduce an applied force to an electrically measurable signal in applications like atomic force microscopy, mass sensing, or molecular detection. However, the high Young's moduli of traditional cantilever materials (silicon or silicon nitride) limit the thickness of the devices, and therefore the deflection sensitivity that can be obtained for a specific spring constant. Using softer materials such as polymers as the structural material of the MEMS device would overcome this problem. However, these materials are incompatible with high-temperature fabrication processes often required to fabricate high quality electronic strain sensors. We introduce a pioneering solution that seamlessly integrates the benefits of polymer MEMS technology with the remarkable sensitivity of strain sensors, even under high-temperature deposition conditions. Cantilevers made using this technology are inherently fluid compatible and have shown up to 6 times lower force noise than their conventional counterparts. We demonstrate the benefits and versatility of this polymer/ceramic/semiconductor multi-layer fabrication approach with the examples of self-sensing AFM cantilevers, and membrane surface stress sensors for biomolecule detection

Direct-write nanoscale printing of nanogranular tunnelling strain sensors for sub-micrometre cantilevers

The sensitivity and detection speed of cantilever-based mechanical sensors increases drastically through size reduction. The need for such increased performance for high-speed nanocharacterization and bio-sensing, drives their sub-micrometre miniaturization in a variety of research fields. However, existing detection methods of the cantilever motion do not scale down easily, prohibiting further increase in the sensitivity and detection speed. Here we report a nanomechanical sensor readout based on electron co-tunnelling through a nanogranular metal. The sensors can be deposited with lateral dimensions down to tens of nm, allowing the readout of nanoscale cantilevers without constraints on their size, geometry or material. By modifying the inter-granular tunnel-coupling strength, the sensors’ conductivity can be tuned by up to four orders of magnitude, to optimize their performance. We show that the nanoscale printed sensors are functional on 500 nm wide cantilevers and that their sensitivity is suited even for demanding applications such as atomic force microscopy

Analysis of local deformation effects in resistive strain sensing of a submicron-thickness AFM cantilever

Incorporating resistive strain-sensing elements into MEMS devices is a long-standing approach for electronic detection of the device deformation. As the need for more sensitivity trends the device dimensions downwards, the size of the strain-sensor may become comparable to the device size, which can have significant impact on the mechanical behaviour of the device. To study this effect, we modelled a submicron-thickness silicon nitride AFM cantilever with strain-sensing element. Using finite element analysis, we calculated the strain in the sensor elements for a deflected cantilever. The sensor element contributes to a local stiffening effect in the device structure which lowers the strain in the sensor. By varying the sensor geometry, we investigated the degree to which this effect impacts the strain. Minimizing the sensor size increases the strain, but the reduction in sensor cross-sectional area increases the resistance and expected sensor noise. The optimal sensor geometry must therefore account for this effect. We used our analysis to optimize geometric variations of nanogranular tunnelling resistor (NTR) strain sensors arranged in a Wheatstone bridge on a silicon nitride AFM cantilever. We varied the dimensions of each sensor element to maintain a constant cross-sectional area but maximize the strain in the sensor element. Through this approach, we expect a 45% increase in strain in the sensor and corresponding 20% increase in the Wheatstone bridge signal. Our results provide an important consideration in the design geometry of resistive strain-sensing elements in MEMS devices

Focused electron beam induced deposition: A perspective

Background: Focused electron beam induced deposition (FEBID) is a direct-writing technique with nanometer resolution, which has received strongly increasing attention within the last decade. In FEBID a precursor previously adsorbed on a substrate surface is dissociated in the focus of an electron beam. After 20 years of continuous development FEBID has reached a stage at which this technique is now particularly attractive for several areas in both, basic and applied research. The present topical review addresses selected examples that highlight this development in the areas of charge-transport regimes in nanogranular metals close to an insulator-to-metal transition, the use of these materials for strain- and magnetic-field sensing, and the prospect of extending FEBID to multicomponent systems, such as binary alloys and intermetallic compounds with cooperative ground states. Results: After a brief introduction to the technique, recent work concerning FEBID of Pt–Si alloys and (hard-magnetic) Co–Pt intermetallic compounds on the nanometer scale is reviewed. The growth process in the presence of two precursors, whose flux is independently controlled, is analyzed within a continuum model of FEBID that employs rate equations. Predictions are made for the tunability of the composition of the Co–Pt system by simply changing the dwell time of the electron beam during the writing process. The charge-transport regimes of nanogranular metals are reviewed next with a focus on recent theoretical advancements in the field. As a case study the transport properties of Pt–C nanogranular FEBID structures are discussed. It is shown that by means of a post-growth electron-irradiation treatment the electronic intergrain-coupling strength can be continuously tuned over a wide range. This provides unique access to the transport properties of this material close to the insulator-to-metal transition. In the last part of the review, recent developments in mechanical strain-sensing and the detection of small, inhomogeneous magnetic fields by employing nanogranular FEBID structures are highlighted. Conclusion: FEBID has now reached a state of maturity that allows a shift of the focus towards the development of new application fields, be it in basic research or applied. This is shown for selected examples in the present review. At the same time, when seen from a broader perspective, FEBID still has to live up to the original idea of providing a tool for electron-controlled chemistry on the nanometer scale. This has to be understood in the sense that, by providing a suitable environment during the FEBID process, the outcome of the electron-induced reactions can be steered in a controlled way towards yielding the desired composition of the products. The development of a FEBID-specialized surface chemistry is mostly still in its infancy. Next to application development, it is this aspect that will likely be a guiding light for the future development of the field of focused electron beam induced deposition

Catalytic Purification of Directly Written Nanostructured Pt Microelectrodes

In the majority of cases, nanostructures prepared by focused electron beam induced deposition employing an organometallic precursor contain predominantly carbon-based ligand dissociation products. This is unfortunate with regard to using this high-resolution direct-write approach for the preparation of nanostructures for various fields, such as mesoscopic physics, micromagnetism, metaoptical phenomena in the visible spectral range, or others. Following early attempts of postprocessing Pt-based structures prepared by focused electron beam induced deposition at several hundred degrees Celsius in a reactive gas atmosphere, recent work has focused on developing in situ purification processes by using a stationary O₂ flux in combination with electron irradiation to oxidize the carbonaceous component of the deposits. Here we show that this purification process is driven by the catalytic activity of Pt and in fact does not rely on the parallel electron irradiation process to function, if the O₂ exposure is done in a pulsed fashion. We suggest a multistep cleaning mechanism which results in pure, nanoporous Pt. By suitably chosen beam parameters, high-resolution Pt dot and line structures with dimensions below 10 nm can thus be conveniently obtained. In temperature-dependent resistance measurements, we find the typical metallic behavior of Pt. In low-temperature magnetoresistance measurements, we see clear evidence for weak antilocalization effects and deduce a dephasing length of 234 nm at 1.2 K. We consider this to be a promising starting point for developing this approach into a versatile preparation technique for Pt-based mesoscopic structures, in particular since the purification process can be run in parallel on different deposits. We furthermore anticipate that our results will spur further research on purification approaches for nanostructures prepared by focused electron beam induced deposition containing a catalytically active metal species such as Pd-, Fe-, or Co-based deposits

Focused electron beam induced deposition: a perspective

Background: Focused electron beam induced deposition (FEBID) is a direct-writing technique with nanometer resolution, which has received strongly increasing attention within the last decade. In FEBID a precursor previously adsorbed on a substrate surface is dissociated in the focus of an electron beam. After 20 years of continuous development FEBID has reached a stage at which this technique is now particularly attractive for several areas in both, basic and applied research. The present topical review addresses selected examples that highlight this development in the areas of charge-transport regimes in nanogranular metals close to an insulator-to-metal transition, the use of these materials for strain- and magnetic-field sensing, and the prospect of extending FEBID to multicomponent systems, such as binary alloys and intermetallic compounds with cooperative ground states. Results: After a brief introduction to the technique, recent work concerning FEBID of Pt–Si alloys and (hard-magnetic) Co–Pt intermetallic compounds on the nanometer scale is reviewed. The growth process in the presence of two precursors, whose flux is independently controlled, is analyzed within a continuum model of FEBID that employs rate equations. Predictions are made for the tunability of the composition of the Co–Pt system by simply changing the dwell time of the electron beam during the writing process. The charge-transport regimes of nanogranular metals are reviewed next with a focus on recent theoretical advancements in the field. As a case study the transport properties of Pt–C nanogranular FEBID structures are discussed. It is shown that by means of a post-growth electron-irradiation treatment the electronic intergrain-coupling strength can be continuously tuned over a wide range. This provides unique access to the transport properties of this material close to the insulator-to-metal transition. In the last part of the review, recent developments in mechanical strain-sensing and the detection of small, inhomogeneous magnetic fields by employing nanogranular FEBID structures are highlighted. Conclusion: FEBID has now reached a state of maturity that allows a shift of the focus towards the development of new application fields, be it in basic research or applied. This is shown for selected examples in the present review. At the same time, when seen from a broader perspective, FEBID still has to live up to the original idea of providing a tool for electron-controlled chemistry on the nanometer scale. This has to be understood in the sense that, by providing a suitable environment during the FEBID process, the outcome of the electron-induced reactions can be steered in a controlled way towards yielding the desired composition of the products. The development of a FEBID-specialized surface chemistry is mostly still in its infancy. Next to application development, it is this aspect that will likely be a guiding light for the future development of the field of focused electron beam induced deposition