A subscription to JoVE is required to view this content. Sign in or start your free trial.

Method Article

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

9.4K views

⸱

DOI:

10.3791/54030

⸱

July 12th, 2016

 ,  ,  , 

In This Article

Summary

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.

Abstract

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.

Introduction

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 pro....

Access restricted. Please log in or start a trial to view this content.

Protocol

1. Electrochemical Etching

  1. Experimental set-up
    1. 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.
      1. Make a tungsten rod holder from an approximately 100 mm long 6 mm diamet....

Access restricted. Please log in or start a trial to view this content.

Results

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.......

Access restricted. Please log in or start a trial to view this content.

Discussion

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.......

Access restricted. Please log in or start a trial to view this content.

Disclosures

The authors have nothing to disclose.

Acknowledgements

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.

....

Access restricted. Please log in or start a trial to view this content.

Materials

List of materials used in this article
NameCompanyCatalog NumberComments
Tungsten Rod 0.020" x 12"ESPI Metalshttp://www.espimetals.com/index.php/online-catalog/467-Tungsten 3N8 Purity
50% by weight NaOH solutionSigma-Aldrich415413-500ML500 ml
Separatory funnelCole-ParmerItem# WU-34506-03250 ml
DC Power supplyBK Precision1672Triple Output 0 - 32 V, 0 - 3 A DC Power Supply
AcetoneCole-ParmerItem# WU-88000-68500 ml
Data Acquisition CardNational InstrumentsNI PXI-622116 AI, 24 DIO, 2 AO
RelayMagnecraft276 XAXH-5D7 A, 30 V DC Reed Relay
6-way 6" conflat flange crossKurt J LeskerC6-0600
6" to 2-3/4" conflat zero length reducer flange  (x3)Kurt J LeskerRF600X275
2-3/4" conflat flange SHV feedthroughKurt J LeskerIFTSG041033
2-3/4" conflat flange BNC feedthroughKurt J LeskerIFTBG042033
2-3/4" conflat flange linear feedthroughMDC660006, REF# BLM-275-2
6" conflat flange blankoffKurt J LeskerF0600X000N
6" conflat flange windowKurt J LeskerVPZL-600
HV Power supplyKeithley InstrumentsKeithley Model #2290-50 - 5 kV DC HV Power Supply
PicoammeterKeithley InstrumentsKeithley Model #6485
Faraday CupBeam Imaging SolutionsModel FC-1 Faraday Cup

References

  1. Muller, E. W., Bahadur, K. Field Ionization of Gases at a Metal Surface and the Resolution of the Field Ion Microscope. Phys. Rev. 102, 624(1956).
  2. Binnig, G., Rohrer, H. Scanning Tunneling Microscopy. Helv. Phys. Acta. 55, 726-735 (1982).
  3. Melmed, A. J.

Access restricted. Please log in or start a trial to view this content.

Reprints and Permissions

Explore More Articles

Tungsten RodsSodium Hydroxide SolutionScanning Electron MicroscopyField Emission ModeElectron Beam CurrentVacuum Chamber SetupHigh Voltage SupplyPenning Trap Mass Spectrometry