Fabrication and Characterization of Silicon Micro-Funnels and Tapered Micro-Channels for Stochastic Sensing Applications

We present a simplified, highly reproducible process to fabricate arrays of tapered silicon micro-funnels and micro-channels using a single lithographic step with a silicon oxide (SiO2) hard mask on at a wafer scale. Two approaches were used for the fabrication. The first one involves a single wet anisotropic etch step in concentrated potassium hydroxide (KOH) and the second one is a combined approach comprising Deep Reactive Ion Etch (DRIE) followed by wet anisotropic etching. The etching is performed through a 500 μm thick silicon wafer, and the resulting structures are characterized by sharp tapered ends with a sub-micron cross-sectional area at the tip. We discuss the influence of various parameters involved in the fabrication such as the size and thickness variability of the substrate, dry and wet anisotropic etching conditions, the etchant composition, temperature, diffusion and micro-masking effects, the quality of the hard mask in the uniformity and reproducibility of the structures, and the importance of a complete removal of debris and precipitates. The presence of apertures at the tip of the structures is corroborated through current voltage measurements and by the translocation of DNA through the apertures. The relevance of the results obtained in this report is discussed in terms of the potential use of these structures for stochastic sensing.

[1]  Warren K. Mino,et al.  A method for reproducibly preparing synthetic nanopores for resistive-pulse biosensors. , 2007, Small.

[2]  C. Trautmann,et al.  Microstructured glass chip for ion-channel electrophysiology. , 2001, Physical review. E, Statistical, nonlinear, and soft matter physics.

[3]  A. Steckenborn,et al.  Micropyramidal hillocks on KOH etched {100} silicon surfaces: formation, prevention and removal , 1999 .

[4]  Susan Daniel,et al.  Ionic conductivity of the aqueous layer separating a lipid bilayer membrane and a glass support. , 2006, Langmuir : the ACS journal of surfaces and colloids.

[5]  Miko Elwenspoek,et al.  Guidelines for etching silicon MEMS structures using fluorine high-density plasmas at cryogenic temperatures , 2002 .

[6]  J. Judy,et al.  Design and fabrication of a micromachined planar patch-clamp substrate with integrated microfluidics for single-cell measurements , 2006, Journal of Microelectromechanical Systems.

[7]  Adam S. Foster,et al.  An atomistic introduction to anisotropic etching , 2007 .

[8]  P. Ferreira,et al.  Exploiting differential etch rates to fabricate large-scale nozzle arrays with protudent geometry , 2007 .

[9]  Christina Trautmann,et al.  An Asymmetric Polymer Nanopore for Single Molecule Detection , 2004 .

[10]  Horst Vogel,et al.  Chip based biosensor for functional analysis of single ion channels , 2000 .

[11]  Hongbo Peng,et al.  Fabrication of nanopores in silicon chips using feedback chemical etching. , 2007, Small.

[12]  H. S. Wolff,et al.  iRun: Horizontal and Vertical Shape of a Region-Based Graph Compression , 2022, Sensors.

[13]  G. Kovacs Micromachined Transducers Sourcebook , 1998 .

[14]  Zuzanna S Siwy,et al.  Detecting single porphyrin molecules in a conically shaped synthetic nanopore. , 2005, Nano letters.

[15]  H. Andersson,et al.  Microfluidic devices for cellomics: a review , 2003 .

[16]  Ming Lei,et al.  Hard and soft micromachining for BioMEMS: review of techniques and examples of applications in microfluidics and drug delivery. , 2004, Advanced drug delivery reviews.

[17]  Chien-Chung Fu,et al.  Different fabrication methods of out-of-plane polymer hollow needle arrays and their variations , 2007 .

[18]  A. Heuberger,et al.  Anisotropic Etching of Crystalline Silicon in Alkaline Solutions II . Influence of Dopants , 1990 .

[19]  Xuesong Liu,et al.  Fabrication of keyhole-free ultra-deep high-aspect-ratio isolation trench and its applications , 2005 .

[20]  M. Madou Fundamentals of microfabrication , 1997 .

[21]  M. Hines,et al.  Etchant anisotropy controls the step bunching instability in KOH etching of silicon. , 2004, Physical review letters.

[22]  K. Bean,et al.  Anisotropic etching of silicon , 1978, IEEE Transactions on Electron Devices.

[23]  A. Heuberger,et al.  Anisotropic Etching of Crystalline Silicon in Alkaline Solutions I . Orientation Dependence and Behavior of Passivation Layers , 1990 .

[24]  Irena Zubel,et al.  Silicon anisotropic etching in alkaline solutions II on the influence of anisotropy on the smoothness of etched surfaces , 1998 .

[25]  Masayoshi Esashi,et al.  Micro instrumentation for characterizing thermoelectric properties of nanomaterials , 2005 .

[26]  J. Esteve,et al.  TMAH/IPA anisotropic etching characteristics , 1993 .

[27]  Thomas Laurell,et al.  Design and development of a silicon microfabricated flow-through dispenser for on-line picolitre sample handling , 1999 .

[28]  Luca Berdondini,et al.  Generic technological platform for microfabricating silicon nitride micro- and nanopipette arrays , 2005 .

[29]  Zuzanna S Siwy,et al.  Resistive-pulse DNA detection with a conical nanopore sensor. , 2006, Langmuir : the ACS journal of surfaces and colloids.

[30]  H. Thurman Henderson,et al.  Ultra-deep anisotropic etching of (110) silicon , 1999 .

[31]  Irena Zubel,et al.  The effect of isopropyl alcohol on etching rate and roughness of (1 0 0) Si surface etched in KOH and TMAH solutions , 2001 .

[32]  Dorian Liepmann,et al.  Microfabricated Polysilicon Microneedles for Minimally Invasive Biomedical Devices , 2000 .

[33]  L. A. Baker,et al.  Conical nanopore membranes: solvent shaping of nanopores , 2006 .

[34]  G. Kovacs,et al.  Bulk micromachining of silicon , 1998, Proc. IEEE.

[35]  A. van den Berg,et al.  Micromachining of buried micro channels in silicon , 2000, Journal of Microelectromechanical Systems.

[36]  Hywel Morgan,et al.  Dielectrophoretic manipulation of avidin and DNA , 1998, Proceedings of the 20th Annual International Conference of the IEEE Engineering in Medicine and Biology Society. Vol.20 Biomedical Engineering Towards the Year 2000 and Beyond (Cat. No.98CH36286).

[37]  Marc Gershow,et al.  DNA molecules and configurations in a solid-state nanopore microscope , 2003, Nature materials.

[38]  Peng Chen,et al.  Atomic Layer Deposition to Fine-Tune the Surface Properties and Diameters of Fabricated Nanopores. , 2004, Nano letters.

[39]  C. R. Martin,et al.  Conical nanopore membranes. Preparation and transport properties. , 2004, Analytical chemistry.

[40]  Dong-il Dan Cho,et al.  In-plane single-crystal-silicon microneedles for minimally invasive microfluid systems , 2004 .