Name: electrochemical etching and characterization of sharp field emission points for electron impact ionization
Uploaded: 2016-07-12T14:00:00
Description: Watch this Scientific Journal Video about Electrochemical Etching and Characterization of Sharp Field Emission Points for Electron Impact Ionization at JoVE.com

We acknowledge the services of Stanley Flegler, Carol Flegler, and Abigail Tirrell at the MSU Center for Advanced Microscopy. We thank Ray Clark and Mark Wilson for technical assistance with the set-up of the electrochemical etching apparatus. Earlier contributions from Anne Benjamin, Georg Bollen, Rafael Ferrer, David Lincoln, Stefan Schwarz and Adrian Valverde, and technical assistance from John Yurkon are also acknowledged. This work was partially supported by the National Science Foundation contract no. PHY-1102511 and PHY-1307233, Michigan State University and the Facility for Rare Isotope Beams, and Central Michigan University.

1. Electrochemical Etching
<ol>
	<li>Experimental set-up
	<ol>
		<li>Apparatus 
		Note: The electrochemically etching set-up requires a standard 0 - 30 V direct current (DC) benchtop power supply and appropriate cables, a separatory funnel, a wide base glass beaker, and standard rod and utility clamp with electrically insulating grips. Small screws, insulated stand-offs, and alligator clips will also be required. Additional items, described below and shown in the picture of the et...

<ol>
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Lett. 92, 220802 (2004).</li><li>Hobara, R., Yoshimoto, S., Hasegawa, S., Sakamoto, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dynamic+electrochemical-etching+technique+for+tungsten+tips+suitable+for+multi-tip+scanning+tunneling+microscopes.">Dynamic electrochemical-etching technique for tungsten tips suitable for multi-tip scanning tunneling microscopes.</a> e-J. Surf. Sci. Nanotechnol. 5, 94-98 (2007).</li><li>Klein, M., Schwitzgebel, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+improved+lamellae+drop-off+technique+for+sharp+tip+preparation+in+scanning+tunneling+microscopy.">An improved lamellae drop-off technique for sharp tip preparation in scanning tunneling microscopy.</a> Rev. Sci. Instrum. 68, 3099-3103 (1997).</li><li>Kerfriden, S., Nahl&#233;, A. H., Campbell, S. A., Walsh, F. C., Smith, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+electrochemical+etching+of+tungsten+STM+tips.">The electrochemical etching of tungsten STM tips.</a> Electrochim. Acta. 43, 1939-1944 (1998).</li><li>Lemke, H., G&#246;ddenhenrich, T., Bochem, H. P., Hartmann, U., Heiden, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improved+microtips+for+scanning+probe+microscopy.">Improved microtips for scanning probe microscopy.</a> Rev. Sci. Instrum. 61, 2538-2538 (1990).</li><li>Song, J. P., Pryds, N. H., Glejb&#248;l, K., M&#248;rch, K. A., Th&#246;l&#233;n, A. R., Christensen, L. 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We have described straightforward procedures to electrochemically etch sharp field emission points (FEPs) in a NaOH solution, and to test the FEPs by operating them in field emission mode. The etching procedure described is a variation of existing techniques-the lamella drop-off technique7,8 and the floating layer technique9,10. However, we found it to be more convenient and reliable to implement than the aforementioned methods.
Before starting the etching procedure, to m...

Sharp tips or points have long been used in microscopy applications, such as the field ion microscope (FIM)1 and the scanning tunneling microscope (STM)2, and a range of techniques for producing sharp tips of various materials have been developed3. These sharp tips can also be operated as field emission points (FEPs) by applying a high voltage to them, and serve as a convenient electron beam source. One application of such as source is ion production via electron impact ionization (EII). The FEP is particularly advantageous in applications where temperature fluctuations produced by thermal emitters are undesirable. For example, ion production via EII of background gas or vapor in high precision Penning traps4,5.
A simple method for fabricating FEPs is to electrochemically etch tungsten rods in a sodium hydroxide (NaOH) solution. This technique is relatively straightforward to implement with modest equipment and has been shown to be quite reproducible and reliable. A number of methods are described in the literature and improvements to these techniques continue to appear6. Here we describe a method for the electrochemical etching of tungsten tips in a NaOH solution. Our method is a variation of the lamella drop-off technique7,8 and the floating layer technique9,10. Like these two methods it enables the production of two tips from a single etching procedure. A picture of the experimental apparatus for etching the tips is shown in Figure 1.
<img alt="Figure 1" src="/files/ftp_upload/54030/54030fig1.jpg" /> 
Figure 1. Etching apparatus. Photograph of the experimental apparatus used for electrochemical etching of tungsten rods with NaOH solution. <a href="https://www.jove.com/files/ftp_upload/54030/54030fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
Electrochemical etching of tungsten in the aqueous NaOH base occurs via a two-stage process. First, intermediate tungsten oxides are formed, and second, these oxides are non-electrochemically dissolved to form the soluble tungstate anion. This process is described, in simplified form, by the two reactions
(1) W + 6OH- &#8594; WO3(S) + 3H2O + 6e-, and
(2)&#160;WO3(S) + 2OH- &#8594; WO42- + H2O.
The etching current and the NaOH solution molarity used affect the time and voltage required to etch through the tungsten rod. Studies of these effects are presented and discussed. More importantly, the etching parameters have an effect on the geometry of the tips and, as such, on their operation in field emission mode. The geometry of the tips we produced were characterized by imaging them with a scanning electron microscope (SEM). These images can be used to estimate, for example, the tip radius. In addition, the tips were operated in field emission mode by applying a negative voltage of typically a few hundred volts to a few kilovolts to them and monitoring the resulting electron emission current. The relationship between field emission current, I, and applied bias voltage, V, can be described by the Fowler-Nordheim equation11
(3) I = AV2 e-Creff/V,
where reff is the effective radius of the tip, A is a constant, and C is the second Fowler-Nordheim constant <img alt="Equation 9" src="/files/ftp_upload/54030/54030eq9.jpg" />, in which b = 6.83 eV-3/2V/nm, <img alt="Equation 11" src="/files/ftp_upload/54030/54030eq11.jpg" /> is the work function of tungsten (<img alt="Equation 11" src="/files/ftp_upload/54030/54030eq11.jpg" /> &#8776; 4.5 eV), k is a factor that depends on geometry (k &#8776; 5), and <img alt="Equation 12" src="/files/ftp_upload/54030/54030eq15.jpg" /> is the Nordheim image correction term (<img alt="Equation 12" src="/files/ftp_upload/54030/54030eq15.jpg" /> &#8776; 1)12. Hence, the effective radius of the tip can be determined by measuring the electron current as a function of bias voltage. Specifically, it can be obtained from the slope of a so-called Fowler-Nordheim (FN) plot of ln(I/V2) vs 1/V.

<table border="0" cellpadding="0" cellspacing="0" width="1230">
	<tbody>
		<tr height="20">
			<td height="20" style="height:20px;width:325px;">Tungsten Rod 0.020&#34; x 12&#34;</td>
			<td style="width:159px;">ESPI Metals</td>
			<td style="width:451px;"><a href="http://www.espimetals.com/index.php/online-catalog/467-Tungsten">http://www.espimetals.com/index.php/online-catalog/467-Tungsten&#160;</a></td>
			<td style="width:297px;">3N8 Purity</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">NaOH salt</td>
			<td>Cole-Parmer</td>
			<td>Item # WU-88404-71</td>
			<td>100 g</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Separatory funnel</td>
			<td>Cole-Parmer</td>
			<td>Item#&#160;WU-34506-03</td>
			<td>250 mL&#160;</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">DC Power supply</td>
			<td>BK Precision</td>
			<td>1672</td>
			<td>Triple Output 0 - 32 V, 0 - 3 A DC Power Supply</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Acetone</td>
			<td>Cole-Parmer</td>
			<td>Item#&#160;WU-88000-68</td>
			<td>500 mL</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Data Acquisition Card</td>
			<td>National Instruments</td>
			<td style="width:451px;">NI PXI-6221</td>
			<td>16 AI, 24 DIO, 2 AO</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Relay</td>
			<td>Magnecraft</td>
			<td>276 XAXH-5D</td>
			<td>7 A, 30 V DC Reed Relay</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">6-way 6&#34; conflat flange cross</td>
			<td>Kurt J Lesker</td>
			<td>C6-0600</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">6&#34; to 2-3/4&#34; conflat zero length reducer flange&#160; (x3)</td>
			<td>Kurt J Lesker</td>
			<td>RF600X275</td>
			<td></td>
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		<tr height="20">
			<td height="20" style="height:20px;">2-3/4&#34; conflat flange SHV feedthrough</td>
			<td>Kurt J Lesker</td>
			<td>IFTSG041033</td>
			<td></td>
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		<tr height="20">
			<td height="20" style="height:20px;">2-3/4&#34; conflat flange BNC feedthrough</td>
			<td>Kurt J Lesker</td>
			<td>IFTBG042033</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">2-3/4&#34; conflat flange linear feedthrough</td>
			<td>MDC</td>
			<td>660006, REF# BLM-275-2</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">6&#34; conflat flange blankoff</td>
			<td>Kurt J Lesker</td>
			<td>F0600X000N</td>
			<td></td>
		</tr>
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			<td height="20" style="height:20px;">6&#34; conflat flange window</td>
			<td>Kurt J Lesker</td>
			<td>VPZL-600</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">HV Power supply</td>
			<td>Keithley Instruments</td>
			<td>Keithley Model #2290-5</td>
			<td>0 - 5 kV DC HV Power Supply</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Picoammeter</td>
			<td>Keithley Instruments</td>
			<td>Keithley Model #6485</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Faraday Cup</td>
			<td>Beam Imaging Solutions</td>
			<td>Model FC-1 Faraday Cup</td>
			<td></td>
		</tr>
	</tbody>
</table>

electrochemical etching and characterization of sharp field emission points for electron impact ionization

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. The results of studies in which the etching current and the molarity of the NaOH solution used in the etching process were varied are presented. The investigation of the geometry of the tips, by imaging them with a scanning electron microscope, and by operating them in field emission mode is also described. The field emission tips produced are intended to be used as an electron beam source for ion production via electron impact ionization of background gas or vapor in Penning trap mass spectrometry applications.

Study of etching parameters
During the etching process the power supply is operated in constant current mode. The voltage required to maintain this constant current increases slightly as the tungsten rod is etched away (due to the increase in resistance of the rod). The current drops almost to zero when the tip etches all the way through. A small current continues to flow due to the fact that the upper tip is st...

Watch this Scientific Journal Video about Electrochemical Etching and Characterization of Sharp Field Emission Points for Electron Impact Ionization at JoVE.com

Electrochemical Etching and Characterization of Sharp Field Emission Points for Electron Impact Ionization

A method for electrochemically etching field emission tips is presented. Etching parameters are characterized and the operation of the tips in field emission mode is investigated.

A new variation of the drop-off method for fabricating field emission points by electrochemically etching tungsten rods in a NaOH solution is described. ...

electrochemical-etching-characterization-sharp-field-emission-points

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The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

The optical, electrical, and structural properties of dislocations and of grain boundaries in semiconductor materials can be determined by experiments performed in a scanning electron microscope. Electron microscopy has been used to investigate cathodoluminescence, electron beam induced current, and diffraction of backscattered electrons.

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications ...

Fabrication of White Light-emitting Electrochemical Cells with Stable Emission from Exciplexes

The authors present an approach for fabricating stable white light emission from polymer light-emitting electrochemical cells (PLECs) having an active layer which consists of blue-fluorescent poly(9,9-di-n-dodecylfluorenyl-2,7-diyl) (PFD) and &#960;-conjugated triphenylamine molecules. This white light emission originates from exciplexes formed between PFD and amines in electronically excited states. A device containing PFD, 4,4&#39;,4&#39;&#39;-tris[2-naphthyl(phenyl)amino]triphenylamine (2-TNATA), Poly(ethylene oxide) and K2CF3SO3 showed white light emission with Commission internationale de l&#39;&#233;clairage (CIE) coordinates of (0.33, 0.43) and a Color Rendering Index (CRI) of Ra = 73 at an applied voltage of 3.5 V. Constant voltage measurements showed that the CIE coordinates of (0.27, 0.37), Ra of 67, and the emission color observed immediately after application of a voltage of 5 V were nearly unchanged and stable after 300 sec.

The authors present a method for fabricating stable white-light-emitting electrochemical cells utilizing emission from exciplexes formed between a blue-emitting fluorene polymer and aromatic amines.

The authors present an approach for fabricating stable white light emission from polymer light-emitting electrochemical cells (PLECs) having an active ...

One-Step Approach to Fabricating Polydimethylsiloxane Microfluidic Channels of Different Geometric Sections by Sequential Wet Etching Processes

Polydimethylsiloxane (PDMS) materials are substantially exploited to fabricate microfluidic devices by using soft lithography replica molding techniques. Customized channel layout designs are necessary for specific functions and integrated performance of microfluidic devices in numerous biomedical and chemical applications (e.g., cell culture, biosensing, chemical synthesis, and liquid handling). Owing to the nature of molding approaches using silicon wafers with photoresist layers patterned by photolithography as master molds, the microfluidic channels commonly have regular cross sections of rectangular shapes with identical heights. Typically, channels with multiple heights or different geometric sections are designed to possess particular functions and to perform in various microfluidic applications (e.g., hydrophoresis is used for sorting particles and in continuous flows for separating blood cells6,7,8,9). Therefore, a great deal of effort has been made in constructing channels with various sections through multiple-step approaches like photolithography using several photoresist layers and assembly of different PDMS thin sheets. Nevertheless, such multiple-step approaches usually involve tedious procedures and extensive instrumentation. Furthermore, the fabricated devices may not perform consistently and the resulted experimental data may be unpredictable. Here, a one-step approach is developed for the straightforward fabrication of microfluidic channels with different geometric cross sections through PDMS sequential wet etching processes, that introduces etchant into channels of planned single-layer layouts embedded in PDMS materials. Compared to the existing methods for manufacturing PDMS microfluidic channels with different geometries, the developed one-step approach can significantly simplify the process to fabricate channels with non-rectangular sections or various heights. Consequently, the technique is a way of constructing complex microfluidic channels, which provides a fabrication solution for the advancement of innovative microfluidic systems.

Several methods are available for the fabrication of channels of non-rectangular sections embedded in polydimethylsiloxane microfluidic devices. Most of them involve multistep manufacturing and extensive alignment. In this paper, a one-step approach is reported for fabricating microfluidic channels of different geometric cross sections by polydimethylsiloxane sequential wet etching.

Polydimethylsiloxane (PDMS) materials are substantially exploited to fabricate microfluidic devices by using soft lithography replica molding techniques. ...

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of data that can be obtained from an individual sample and renders it difficult to produce statistically relevant data for unique and rare materials. Resonant cavity dielectric spectroscopy is a non-destructive, contactless technique which can simultaneously interrogate both sides of a sheeted material and provide measurements which are suitable for statistical interpretations. This offers analysts the ability to quickly discriminate between sheeted materials based on composition and storage history. In this methodology article, we demonstrate how contactless resonant cavity dielectric spectroscopy may be used to differentiate between paper analytes of varying fiber species compositions, to determine the relative age of the paper, and to detect and quantify the amount of post-consumer waste (PCW) recycled fiber content in manufactured office paper.

A protocol for the non-destructive analysis of the fiber content and relative age of paper.

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of ...