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 etching apparatus in Figure 1, must be fabricated.
		<ol>
			<li>Make a tungsten rod holder from an approximately 100 mm long 6 mm diameter aluminum rod. Drill a 0.5 mm diameter approximately 8 mm deep hole in the center, and make a tapped hole for a 4-40 screw in the side to hold the rod in place.</li>
			<li>Make a counter electrode from an approximately 100 mm x 30 mm x 3 mm thick copper plate with an approximately 75 mm x 20 mm x 1.5 mm deep reservoir milled into it, and a 1.5 mm diameter hole in the center. Attach approximately 15 mm long insulated stand-offs to the backside of the counter electrode.</li>
			<li>Make an FEP catcher by drilling a 6 mm diameter 8 mm deep hole into an approximately 75 x 20 x 20 mm copper block.</li>
		</ol>
		</li>
		<li>Preparation of tungsten rod
		<ol>
			<li>Use wire clippers to cut the 0.5 mm diameter tungsten rods into approximately 25 mm lengths.</li>
			<li>Clean the rods in acetone in an ultrasonic bath for 15 min.</li>
			<li>Rinse the rods with deionized water.</li>
		</ol>
		</li>
		<li>Etching solution 
		Caution: NaOH solution is a corrosive alkali solution-NFPA 704 label: Flammability (0), Health (3), Instability/Reactivity (0), Special (COR)-and can cause chemical burns if it comes in contact with the skin or eyes. Inhalation of fumes can cause irritation and burns to the respiratory tract. When handling NaOH solution, wear chemical splash goggles and face shield to protect the eyes, and gloves and an apron to protect the skin. Perform the etching procedure in a fume hood or wear a respirator. Care should be taken when performing step 1.1.3.1 to produce the diluted NaOH solution. This process is highly exothermic and can release heat that may cause burns or ignite flammables, and could cause the solution to splash out of the container.
		<ol>
			<li>Make a 1.5 M NaOH solution by combining 30 ml of 50% by weight NaOH solution with 370 ml of deionized water to make a 400 ml total volume.</li>
			<li>Fill a separatory funnel with the NaOH solution.</li>
		</ol>
		</li>
		<li>Cut-off circuit 
		Note: If the DC power supply is to be operated manually, then the operator will turn the power supply off once the tungsten rod has etched all the way through (see 1.2.2). In case of manual operation, skip to step 1.2. For automatic cut-off of the DC power supply, the cut-off circuit (shown in Figure 2 and described below), should be constructed. Here, we implement the computer control using a DAQ card.
		<ol>
			<li>Connect an ammeter in series with the DC power supply.</li>
			<li>Connect two resistors, R1 and R2 in series and place in parallel with the tungsten rod/counter electrode etching leg of the circuit. (Nominal values for R1 and R2 are R1 = 5&#160;k&#937;&#160;and R2 = 10 k&#937;.)</li>
			<li>Monitor the voltage across one of the resistors with an analog-to-digital convertor (ADC) and suitable computer control software, e.g., LabVIEW. The monitored voltage, Vmon, can be related to the voltage across both resistors and hence, the voltage across the etching leg, Vetch, via 
			(4) <img alt="Equation 19" src="/files/ftp_upload/54030/54030eq19.jpg" />, 
			where the voltage is being monitored across R1.</li>
			<li>Connect a low resistance resistor, RL = 1 &#937;, in series in the etching circuit. Use a second channel on the ADC to record the voltage across this resistor. The etching current is then found via ietch &#8776; VL/RL. (Only about 1 mA flows throw the monitor leg of the circuit.)</li>
			<li>In software, create a program to output a 5 V TTL signal from the digital input/output channel (DI/O) when either the etching voltage increases above a set-value, or the etching current drops below a set value, indicating that the tungsten rod has etched all the way through. These values depend on the etching current and NaOH solution molarity being used and should be determined with a test run of the experiment.</li>
			<li>As shown in Figure 2, arrange for the 5 V TTL signal to open a relay to stop the current flow.</li>
		</ol>
		</li>
	</ol>
	</li>
</ol>
<img alt="Figure 2" src="/files/ftp_upload/54030/54030fig2.jpg" /> 
Figure 2. Schematic of etching circuit. A schematic drawing of the etching circuit used to provide the constant DC etching current. The current is determined by monitoring the voltage across a low resistance resistor and the voltage is recorded by monitoring the voltage across a high resistance resistor using an ADC. A computer program monitors the current and provides a 5 V output signal to a relay that opens the etching circuit once the current drops below a specified value. <a href="https://www.jove.com/files/ftp_upload/54030/54030fig2large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<ol start="2">
	<li>Etching procedure
	<ol>
		<li>Apparatus preparation
		<ol>
			<li>Set up the apparatus as shown in Figure 1, with the copper FEP catcher block placed inside the wide base glass beaker and the copper cathode located above it, spaced off by the insulating stand-offs.</li>
			<li>Set the current on the DC power supply to the desired value, typically 200 mA.</li>
			<li>Place a tungsten rod in the holder and connect the positive terminal of the DC power supply to the 4-40 holding screw with an alligator clip.</li>
			<li>Insert the tungsten rod through the hole in the copper cathode so that approximately 12 mm of the tungsten rod passes through the hole.</li>
			<li>Connect the negative terminal of the power supply to the copper cathode with another alligator clip.</li>
		</ol>
		</li>
		<li>Etching
		<ol>
			<li>Manually adjust the drip rate of the separatory funnel to match the drip rate through the hole, about 1 drip every 3 sec. Wait for the reservoir in the copper cathode to become full.</li>
			<li>Turn on the DC power supply to begin etching.</li>
			<li>If operating in manual mode, turn off the DC power supply once the bottom part of the tip etches all the way through and drops off. If operating with an automatic shut-off switch, the etching current will be cut-off automatically once the rod etches through.</li>
		</ol>
		</li>
	</ol>
	</li>
</ol>
2. Characterization of Field Emission Points
<ol>
	<li>Inspection of tips
	<ol>
		<li>Carefully remove the bottom tip from the catcher block using pliers or tweezers. Remove the upper tip from the tungsten rod holder by loosening the 4-40 screw and gently pulling the upper tip out with the pliers or tweezers.</li>
		<li>Rinse with acetone and then with deionized water.</li>
		<li>Examine with an optical microscope. Tips should be seen to taper to a fine point. Those that do not, e.g., because they are bent or do not have a regular cone structure, should be discarded. Figure 3 shows an example of (a) a good tip and (b) a bent tip.</li>
		<li>Store tips in a desiccator.</li>
	</ol>
	</li>
</ol>
<img alt="Figure 3" src="/files/ftp_upload/54030/54030fig3.jpg" /> 
Figure 3. Optical image of FEP tips. Picture of (a) a good tip and (b) a bad tip, as viewed through an optical microscope. <a href="https://www.jove.com/files/ftp_upload/54030/54030fig3large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<ol start="2">
	<li>Scanning Electron Microscope (SEM) Imaging
	<ol>
		<li>For SEM Imaging, secure FEP tips to a conducting holder using conducting tape or by screwing them to it (e.g., see Figure 4) and image in a SEM according to manufacturer&#39;s protocol at magnifications of approximately 1,800X and 37,000X to view the cone of the tip and the end of the tip, respectively.</li>
	</ol>
	</li>
</ol>
<img alt="Figure 4" src="/files/ftp_upload/54030/54030fig4.jpg" /> 
Figure 4. FEP holder for SEM imaging. A picture of (a) the top and (b) the bottom of the holder used to secure FEPs while imaging with the SEM. <a href="https://www.jove.com/files/ftp_upload/54030/54030fig4large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 5" src="/files/ftp_upload/54030/54030fig5.jpg" /> 
Figure 5. Field emission apparatus. Schematic of the apparatus used to apply a HV to the FEPs while under vacuum to produce an electron beam. The electron beam current is monitored on the Faraday cup with a picoammeter. <a href="https://www.jove.com/files/ftp_upload/54030/54030fig5large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<ol start="3">
	<li>Field Emission Tests
	<ol>
		<li>Apparatus 
		Note: For the field emission tests the following, or similar, equipment is required: a 6-way 6&#34; conflat flange cross to serve as a vacuum chamber, three 6&#34; to 2 &#190;&#34; conflat flange zero length adaptors, an SHV (safe high voltage) feedthrough on a 2 &#190;&#34; conflat flange, a BNC feedthrough on a 2 &#190;&#34; conflat flange, a linear feedthrough on a 2 &#190;&#34; conflat flange, a 6&#34; conflat flange window, a 6&#34; conflat flange blank off, a turbo vacuum pump mounted to a 6&#34; conflat flange, and a backing pump (e.g., a scroll pump) for the turbo. A high voltage (HV) power supply capable of delivering up to -5 kV is required to bias the FEP, and a picoammeter is required to monitor the electron current emitted from the FEP and collected on a Faraday cup, see e.g., 13. In lieu of a Faraday cup, a simple conducting collection plate can be used. A schematic of the field emission set-up is shown in Figure 5.
		<ol>
			<li>Make a second tungsten rod holder (see step 1.1.1.1). In the opposite end of the holder to the FEP drill a 1 mm diameter hole and drill and tap a hole in the side of the rod for a 4-40 screw to secure it to the vacuum side of the SHV feedthrough.</li>
			<li>Set-up the field emission apparatus as shown in Figure 5. The Faraday cup should be about 2 cm from the end of the FEP.</li>
			<li>Connect the HV supply to the SHV feedthrough that the FEP holder is attached to, and connect the picoammeter to the BNC feedthrough that the Faraday cup is attached to.</li>
			<li>Pump down the set-up to a pressure of 10-6 mbar or below.</li>
		</ol>
		</li>
		<li>Field emission
		<ol>
			<li>Gradually increase the bias on the FEP and monitor the electron beam current on the Faraday cup with a picoammeter. When field emission begins, a current will be observed on the picoammeter.</li>
			<li>Increase the HV in incremental steps (of around 50 V) and record the average electron beam current on the picoammeter at each step. (This process can be computer controlled e.g., by a LabVIEW program if desired, or can be done manually). Keep the electron beam current below 1 &#956;A.</li>
		</ol>
		</li>
		<li>Conditioning
		<ol>
			<li>Condition the tip by operating in field emission mode at 5 nA for 1 hr.</li>
			<li>Repeat the current vs HV scan of 2.3.2.2.</li>
		</ol>
		</li>
	</ol>
	</li>
</ol>

<ol>
	<li>Muller, E. W., Bahadur, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Field+Ionization+of+Gases+at+a+Metal+Surface+and+the+Resolution+of+the+Field+Ion+Microscope.">Field Ionization of Gases at a Metal Surface and the Resolution of the Field Ion Microscope.</a> Phys. Rev. 102, 624 (1956).</li><li>Binnig, G., Rohrer, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Scanning+Tunneling+Microscopy.">Scanning Tunneling Microscopy.</a> Helv. Phys. Acta. 55, 726-735 (1982).</li><li>Melmed, A. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+art+and+science+and+other+aspects+of+making+sharp+tips.">The art and science and other aspects of making sharp tips.</a> J. Vac. Sci. Technol. B. 9, 601-608 (1990).</li><li>Shi, W., Redshaw, M., Myers, E. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Atomic+masses+of+32,33S,+84,86Kr,+and+129,132Xe+with+uncertainties+0.1+ppb.">Atomic masses of 32,33S, 84,86Kr, and 129,132Xe with uncertainties 0.1 ppb.</a> Phys. Rev. A. 72, 022510 (2005).</li><li>Van Dyck, R. S., Zafonte, S. L., Van Liew, S., Pinegar, D. B., Schwinberg, D. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultraprecise+Atomic+Mass+Measurement+of+the+&#945;+particle+and+4He.">Ultraprecise Atomic Mass Measurement of the &#945; particle and 4He.</a> Phys. Rev. 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. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+development+in+the+preparation+of+sharp+scanning+tunneling+microscopy+tips.">A development in the preparation of sharp scanning tunneling microscopy tips.</a> Rev. Sci. Instrum. 64, 900-903 (1993).</li><li>Fowler, R. H., Nordheim, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electron+Emission+in+Intense+Electric+Fields.">Electron Emission in Intense Electric Fields.</a> Proc. R. Soc. Lond. A. , 119-173 (1928).</li><li>Kim, Y. -. G., Choi, E. -. H., Kang, S. -. O., Cho, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Computer-controlled+fabrication+of+ultra-sharp+tungsten+tips.">Computer-controlled fabrication of ultra-sharp tungsten tips.</a> J. Vac. Sci. Technol. B. 16, 2079 (1998).</li><li>Brown, K. L., Tautfest, G. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Faraday-Cup+Monitors+for+High-Energy+Electron+Beams.">Faraday-Cup Monitors for High-Energy Electron Beams.</a> Rev. Sci. Instrum. 27, 696 (1956).</li><li>Redshaw, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+and+characterization+of+field+emission+points+for+ion+production+in+Penning+trap+applications.">Fabrication and characterization of field emission points for ion production in Penning trap applications.</a> Int. J. Mass Spectrom. 379, 187-193 (2015).</li><li>Ibe, J. P., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=On+the+electrochemical+etching+of+tips+for+scanning+tunneling+microscopy.">On the electrochemical etching of tips for scanning tunneling microscopy.</a> J. Vac. Sci. Technol. A. 8, 3570 (1990).</li><li>Ekvall, I., Wahlstr&#246;m, E., Claesson, D., Olin, H., Olsson, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Preparation+and+characterization+of+electrochemically+etched+W+tips+for+STM.">Preparation and characterization of electrochemically etched W tips for STM.</a> Meas. Sci. Technol. 10, 11-18 (1999).</li><li>Schiller, C., Koomans, A. A., van Rooy, T. L., Sch&#246;nenberger, C., Elswijk, H. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Decapitation+of+tungsten+field+emitter+tips+during+sputter+sharpening.">Decapitation of tungsten field emitter tips during sputter sharpening.</a> Surf. Sci. 339, L925-L930 (1995).</li></ol>

The authors have nothing to disclose.

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>
		</tr>
		<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>
		</tr>
		<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>
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			<td height="20" style="height:20px;">6&#34; conflat flange blankoff</td>
			<td>Kurt J Lesker</td>
			<td>F0600X000N</td>
			<td></td>
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		<tr height="20">
			<td height="20" style="height:20px;">6&#34; conflat flange window</td>
			<td>Kurt J Lesker</td>
			<td>VPZL-600</td>
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			<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>
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			<td height="20" style="height:20px;">Picoammeter</td>
			<td>Keithley Instruments</td>
			<td>Keithley Model #6485</td>
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			<td height="20" style="height:20px;">Faraday Cup</td>
			<td>Beam Imaging Solutions</td>
			<td>Model FC-1 Faraday Cup</td>
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	</tbody>
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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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9.4K vistas.  Central Michigan University. 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.

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

Fabrication of VB2/Air Cells for Electrochemical Testing

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for synthesizing nanoscopic VB2 is presented as well as step-by-step procedure for applying a zirconium oxide coating to the VB2 particles for stabilization upon discharge. The process for disassembling existing zinc/air cells is shown, in addition construction of the new working electrode to replace the conventional zinc/air cell anode with a the nanoscopic VB2 anode. Finally, discharge of the completed VB2/air battery is reported. We show that using the zinc/air cell as a test bed is useful to provide a consistent configuration to study the performance of the high-energy high capacity nanoscopic VB2 anode.

Fabrication of VB2/Air Cells for Electrochemical Testing

A protocol is presented to study multi-electron metal/air battery systems by using previous technology developed for the zinc/air cell. Electrochemical testing is then performed on fabricated batteries to evaluate performance.

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for ...

Spatial Separation of Molecular Conformers and Clusters

Gas-phase molecular physics and physical chemistry experiments commonly use supersonic expansions through pulsed valves for the production of cold molecular beams. However, these beams often contain multiple conformers and clusters, even at low rotational temperatures. We present an experimental methodology that allows the spatial separation of these constituent parts of a molecular beam expansion. Using an electric deflector the beam is separated by its mass-to-dipole moment ratio, analogous to a bender or an electric sector mass spectrometer spatially dispersing charged molecules on the basis of their mass-to-charge ratio. This deflector exploits the Stark effect in an inhomogeneous electric field and allows the separation of individual species of polar neutral molecules and clusters. It furthermore allows the selection of the coldest part of a molecular beam, as low-energy rotational quantum states generally experience the largest deflection. Different structural isomers (conformers) of a species can be separated due to the different arrangement of functional groups, which leads to distinct dipole moments. These are exploited by the electrostatic deflector for the production of a conformationally pure sample from a molecular beam. Similarly, specific cluster stoichiometries can be selected, as the mass and dipole moment of a given cluster depends on the degree of solvation around the parent molecule. This allows experiments on specific cluster sizes and structures, enabling the systematic study of solvation of neutral molecules.

We present a technique that allows the spatial separation of different conformers or clusters present in a molecular beam. An electrostatic deflector is used to separate species by their mass-to-dipole moment ratio, leading to the production of gas-phase ensembles of a single conformer or cluster stoichiometry.

Gas-phase molecular physics and physical chemistry experiments commonly use supersonic expansions through pulsed valves for the production of cold ...

Characterization of Recombination Effects in a Liquid Ionization Chamber Used for the Dosimetry of a Radiosurgical Accelerator

Most modern radiation therapy devices allow the use of very small fields, either through beamlets in Intensity-Modulated Radiation Therapy (IMRT) or via stereotactic radiotherapy where positioning accuracy allows delivering very high doses per fraction in a small volume of the patient. Dosimetric measurements on medical accelerators are conventionally realized using air-filled ionization chambers. However, in small beams these are subject to nonnegligible perturbation effects. This study focuses on liquid ionization chambers, which offer advantages in terms of spatial resolution and low fluence perturbation. Ion recombination effects are investigated for the microLion detector (PTW) used with the Cyberknife system (Accuray). The method consists of performing a series of water tank measurements at different source-surface distances, and applying corrections to the liquid detector readings based on simultaneous gaseous detector measurements. This approach facilitates isolating the recombination effects arising from the high density of the liquid sensitive medium and obtaining correction factors to apply to the detector readings. The main difficulty resides in achieving a sufficient level of accuracy in the setup to be able to detect small changes in the chamber response.

A growing number of radiation therapy devices offer the advantage of delivering the dose through very small beams to the tumor, allowing for increased conformity and higher doses per fraction. Many different detectors can be used for the dosimetry of these small fields. In the present study, the effect of ion recombination is investigated for a liquid ionization chamber using a stereotactic radiation therapy system.

Most modern radiation therapy devices allow the use of very small fields, either through beamlets in Intensity-Modulated Radiation Therapy (IMRT) or via ...

Electron Channeling Contrast Imaging for Rapid III-V Heteroepitaxial Characterization

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging (ECCI) in a scanning electron microscope (SEM). ECCI allows for imaging of defects and crystallographic features under specific diffraction conditions, similar to that possible via plan-view transmission electron microscopy (PV-TEM). A particular advantage of the ECCI technique is that it requires little to no sample preparation, and indeed can use large area, as-produced samples, making it a considerably higher throughput characterization method than TEM. Similar to TEM, different diffraction conditions can be obtained with ECCI by tilting and rotating the sample in the SEM. This capability enables the selective imaging of specific defects, such as misfit dislocations at the GaP/Si interface, with high contrast levels, which are determined by the standard invisibility criteria. An example application of this technique is described wherein ECCI imaging is used to determine the critical thickness for dislocation nucleation for GaP-on-Si by imaging a range of samples with various GaP epilayer thicknesses. Examples of ECCI micrographs of additional defect types, including threading dislocations and a stacking fault, are provided as demonstration of its broad, TEM-like applicability. Ultimately, the combination of TEM-like capabilities &#8211; high spatial resolution and richness of microstructural data &#8211; with the convenience and speed of SEM, position ECCI as a powerful tool for the rapid characterization of crystalline materials.

The use of electron channeling contrast imaging in a scanning electron microscope to characterize defects in III-V/Si heteroexpitaxial thin films is described. This method yields similar results to plan-view transmission electron microscopy, but in significantly less time due to lack of required sample preparation.

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging ...

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

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 for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
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 ...