JOURNAL OF APPLIED PHYSICS 109, 013301 2011

Microdischarge extreme ultraviolet source with alkali metal vapor for surface morphology application
Takeshi Higashiguchi,1,2,a Hiromitsu Terauchi,1 Takamitsu Otsuka,1 Mami Yamaguchi,1 Keisuke Kikuchi,1 Noboru Yugami,1,2 Toyohiko Yatagai,1 Wataru Sasaki,3 Rebekah DArcy,4 Padraig Dunne,4 and Gerry OSullivan4
1

Department of Advanced Interdisciplinary Sciences, Center for Optical Research and Education (CORE), Utsunomiya University, Yoto 7-1-2, Utsunomiya, Tochigi 321-8585, Japan 2 CREST, Japan Science and Technology Agency, 4-1-8 Honcho, Kanagawa, Saitama 332-0012, Japan 3 NTP Inc., Gakuen Kibanadai Nishi 1-1, Miyazaki 889-2192, Japan 4 School of Physics, University College Dublin, Beleld, Dublin 4, Ireland

Received 28 September 2010; accepted 18 November 2010; published online 3 January 2011 We have characterized a discharge-produced potassium plasma extreme ultraviolet XUV source. Potassium ions produced strong broadband emission around 40 nm with a bandwidth of 8 nm full width at half-maximum . By comparison with atomic structure calculations, the broadband emission is found to be primarily due to 3d 3p transitions in potassium ions ranging from K2+ to K4+. The current-voltage characteristics of the microdischarge suggest that the source operates in a hollow cathode mode and consequently the emitting ions may be localized on the potassium electrode surface at the hole into the capillary. To understand the spectral behavior from the potassium plasmas we compared the spectra from the discharge-produced plasma with that from a laser-produced plasma. The spectra from the different electric and laser plasmas at the same electron temperature 12 eV were almost the same. This compact capillary XUV source with a photon energy of 30 eV is a useful XUV emission source for surface morphology applications. 2011 American Institute of Physics. doi:10.1063/1.3528165
I. INTRODUCTION

Photon energies between 10 and 100 eV correspond to wavelengths between 12 and 120 nm in the electromagnetic spectrum. These photon energies are high enough to induce photochemical reactions in most materials, including hydrogen, carbon, and oxygen. Short wavelengths are generally necessary for surface material processing.13 Light sources in these spectral regions will thus be applied in various scientic and engineering elds, such as semiconductor lithography,46 diagnostics in dense plasmas, materials processing, photochemistry, biological imaging, and so on. Recently, a desorption spectrometer employing a compact, efcient discharge-produced microplasma extreme ultraviolet XUV source in the 20100 nm broadband spectral region has been proposed, which has the advantage of neither damaging or melting the surface after irradiation.7 A plasma light source in the hollow cathode mode produced in microdischarge geometries is found to be an efcient source in these spectral regions. Operation under high pressure and with high-energy electrons favors the formation of excimers, leading to a maximum efciency of 7% at 172 nm from xenon gas.8 These microplasma sources in hollow cathodes have been demonstrated under high-pressure conditions.8,9 Discharge-excited XUV lasers via the production of a plasma column, have also been demonstrated.1012 An XUV laser operating at 46.9 nm based on a fast capillary discharge has been reported as a short wavelength light source.10 The operation of this argon-gas-based XUV laser at
a

Electronic mail: higashi@cc.utsunomiya-u.ac.jp.

46.9 nm, in a fast pulsed capillary discharge laser system, however, requires a large capacitor power supply typically a Marx bank conguration to produce high peak current and a differential vacuum pumping system. To facilitate the operation of an XUV source in a high vacuum environment for the desorption-spectrometer application, a metal vapor was used. It is well known that the highest quartet level of the highest J of a given conguration in an alkali metal atom is metastable against both autoionization and radiation in the XUV spectral region.13 The properties of XUV emission from multiply charged alkali metal ions have not been investigated in detail. The generation of discharge-pumped XUV sources, however, requires the presence of a substantial density of high purity metal vapor in a capillary. Our approach is to use a potassium K target operating in a hollow cathode discharge mode. This source produced a spectroscopically pure potassium vapor jet from a room temperature target by rapidly heating the electrode with a hollow cathode discharge. XUV emission from the multiply charged potassium ions should be produced in hollow cathode mode in order to realize a practical light source for surface processing of materials. In this paper, we report on a discharge-produced microplasma XUV source emitting at around 40 nm based on a pure potassium vapor. We used a pure potassium electrode to produce the intense XUV emission under hollow cathode mode in a capillary. The potassium ions produced strong broadband emission around 40 nm with a bandwidth of 8 nm full width at half-maximum FWHM . To characterize the discharge-produced potassium plasma and optimize it for emission of 30 eV photons, we observe the spectrum of a
2011 American Institute of Physics

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109, 013301-1

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1.2 1 0.8 0.6 0.4 0.2 0 20 1.2 1 0.8 0.6 0.4 0.2 0 20 30 40 50 30 40 50

J. Appl. Phys. 109, 013301 2011

Intensity (arb. units)

Potassium

Cu electrode Hole

(a)
O2+ O3+ O2+ O3+ O2+ O3+ O2+ Cu+ Cu+ O3+ O+

Pumping outlet
Cu Capillary Hollow structure

C3+ C2+

Spectrometer - H.V.

Wavelength (nm)

60

70

O4+

80

90

100

Intensity (arb. units)

K
C3+ C2+ O2+ O3+

GND

(b)
O+ Cu+ O
2+

O3+

FIG. 1. Color online Schematic diagram of the experimental setup. The inset shows the electrode structure of the XUV source.

laser-produced plasma and compare the two types of spectra at the same electron temperature of 12 eV. The spectrum of the discharge-produced plasma is compared with that of the laser-produced plasma because a polytetrauoroethylene PTFE capillary-based discharge plasma produces O, H, and C ionic emission, as well as with the potassium K emission, and the comparison permits identication of the contribution of the latter.

Wavelength (nm)

60

O2+ O4+

70

X-ray CCD camera

O3+

80

90

Cu+

3+

100

FIG. 2. Time-integrated spectra of the discharge-produced potassium plasmas for capillary inner diameters of 1 mm a and 500 m b , respectively.

III. EXPERIMENTAL RESULT AND DISCUSSION

II. EXPERIMENTAL SETUP

Figure 1 shows a schematic diagram of the experimental setup, where the capillary is placed in a vacuum chamber. The capillary was a 1 mm long pipe with diameters of 500 and 1000 m made in a PTFE block. The capillary discharge produced the initial electrons to initiate an efcient hollow cathode discharge at the potassium electrode. The maximum discharge voltage and current are 30 kV and 200 A using a pulsed power supply connecting a condenser capacity of 2 nF at a repetition rate of 10 Hz. The discharge voltage and current were monitored by use of a high-voltage probe and a Rogowski coil connected to a 2 GHz sampling digital oscilloscope. All equipment was connected to a personal computer for data acquisition and processing. The maximum discharge current has a pulse duration of 150 ns with the light source as the load. During the operation of the light source, the pressure in the chamber was maintained below 3 103 Pa. The axial emission of the discharge in the XUV spectral region was analyzed with a normal incidence vacuum spectrograph using an iridium coated grating with 1200 lines/mm Acton VM502 . The distance between the exit of a capillary and the entrance slit of the spectrometer was 1 m. The timeintegrated spectra were obtained by a thermoelectrically cooled back-illuminated x-ray charge coupled device CCD camera. The typical spectral resolution was better than 0.5 nm. Pressure in the spectrometer was maintained less than 3 105 Pa.

Figure 2 shows a typical time-integrated XUV emission spectrum between 25 and 100 nm. Pulsed electric power was applied to a capillary with the optimum capillary diameter of 1000 a and 500 m b at a maximum discharge current of 200 A. The wavelength-integrated energy from 25 to 60 nm was maximized under this condition. Potassium ions produced strong broadband emission around 40 nm, which was mainly due to 3p 3d transitions from K2+ to K4+ ions, together with several oxygen lines. The spectral bandwidth of the potassium emission was about 8 nm FWHM at 40 nm. To identify the transitions responsible for the emission centered on 40 nm, calculations were performed using the multiconguration HARTREE-FOCK code developed by Cowan.14 Transitions between the congurations 3s23pn and 3s23pn13d1, 3 n 7 were calculated for one to four times ionized potassium. In a similar way to n = 4 to n = 4 transitions in the spectrum of a laser-produced tin plasma,15 the 3p 3d transitions from the range of potassium ions present in the discharge-produced microplasma overlap to form a relatively narrow band of emission. We performed a theoretical evaluation to nd scaling of the optimum plasma parameter using a hydrodynamic model. This model assumed collisional-radiative equilibrium CRE process in a plasma that was optically thin for all radiation.16 Figure 3 represents the numerically calculated spectrum from 20 to 70 nm at an electron temperature of 12 eV around the electrode surface at an electron density of 1020 cm3. The experimentally observed spectrum in Fig. 2 b is quite similar to the calculated spectrum. The numerical calculation, therefore, represents a clear insight into the optimization of the spectral control and may be useful for the design of future experiments. Figure 4 shows the dependence of the normalized XUV yield from 25 to 60 nm on the inner diameter at an aspect ratio of 2. The XUV yield was maximized when the inner

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Intensity (arb. units)

0.8 0.6 0.4 0.2 0 20 30 40 50 60 70

CE (arb. units)

1 0.8 0.6 0.4 0.2 0 0 100 200 300 400

Wavelength (nm)
FIG. 3. Numerical calculated spectrum at the electron temperature of 12 eV.

Discharge current (A)

FIG. 5. Discharge current dependence of the XUV yield from 25 to 60 nm spectral region. The solid line represents the result of the simulation.

diameter was 500 m, corresponding to the spectrum in Fig. 2 b . At inner diameters smaller than 500 m, the XUV yield decreased, which was attributed to high impedance. In addition, the XUV yield also decreased at inner diameters larger than 500 m due to the low input energy density in the large-volume capillary. The dependence of the wavelength-integrated XUV emission conversion efciency CE on the discharge current is shown in Fig. 5. Here the XUV CE was dened as a ratio between the XUV emission energy between 25 and 60 nm and the input discharge electric energy. The CE increased with increasing discharge current. The numerical calculation result is shown as a solid line in Fig. 4. The calculation gives a peak XUV CE at a discharge current of 220 A. Unfortunately, it was possible in our setup to only generate a maximum current of 200 A, however the decrease in the peak CE value with low discharge current is also reproduced. The population of effective potassium ions of K3+ and K4+ that emit at around 40 nm depends on the electron temperature as well as electron density. The optimum electron temperatures of the maximum population were calculated to be 6 and 8 eV from a steady-state CRE model.16 The temporally and spatially integrated electron temperature, which was evaluated by using the intensity ratios of the line emissions of oxygen ions in the time-integrated XUV spectra, linearly increased with the increase in the discharge current, as shown in Fig. 6. At a discharge current of 200 A, the electron temperature was observed to be about 10 eV. In the XUV spectral region, the discharge current is usually required to be in the kiloamperes range to obtain sufcient plasma heating to produce multiply charged ions. The scheme reported here would allow an effective discharge XUV source in a low discharge current less than 1 kA thus
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reducing the heat load on both the pulsed power supply and the plasma light source. Figure 7 shows the discharge current dependence on voltage for this source. The sustaining voltage of the discharge was almost 1 kV for a current of 100 200 A. This type of dependence is expected for a hollow cathode discharge mode.8,17 The high density and highenergy electrons are produced by the strong electric eld in the sheath near the cathode electrode surface with the potassium metal. These electrons excite multiply charged ions, this excitation is attributed to the impact of electrons from the plasma on the potassium electrode. In addition, the electron temperature of the potassium plasma increases with an increase in the discharge current due to Joule heating in the hollow cathode discharge mode. As a result, the increase in the emission intensity originating from the multiply charged potassium ions is attributed to the high energy electrons in the hollow cathode discharge at the potassium electrode surface. The effective potassium ion density responsible for the 40 nm XUV emission increases near the potassium electrode surface. The angular distribution of the XUV emission was measured to be 170 mrad, as shown in Fig. 8. Here, 0 rad corresponds to the axis of the capillary. This distribution is evaluated to be 150 mrad when limited by the capillary wall and the light source at the potassium electrode into a capillary. In other words, the emitting ions may be localized around the potassium electrode at the hole into the capillary due to the hollow cathode discharge mode.18
IV. COMPARISON SPECTRA WITH A LASERPRODUCED POTASSIUM PLASMA

The spectrum of the discharge-produced plasma was compared with that of a laser-produced plasma as the PTFE
Electron temperature (eV)
15

XUV yield (arb. units)

1 0.8 0.6 0.4 0.2 0 0 0.5 1.0 1.5 2.0 2.5

10

0 0

50

100

150

200

250

Inner diameter (mm)

FIG. 4. Capillary inner diameter dependence of the XUV yield integrated from 25 to 60 nm.

Discharge current (A)

FIG. 6. The electron temperature as a function of the discharge current. The dashed line shows a linear t.

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J. Appl. Phys. 109, 013301 2011

1.5 1 0.5 0 100

XUV yield (arb. units)

Sustaining voltage (kV)

150

200

250

400

600

800

Discharge current (A)

FIG. 7. Current-voltage characteristics of the microplasma running in hollow cathode mode. The dashed line is the tting line by use of the numerical simulation.

Emission angle

(mrad)

FIG. 8. Angular distribution of the XUV yield integrated from 25 to 60 nm at the capillary inner diameter of 500 m. The dashed line is proportional rad is the angle of the target normal. The tting curve to cosn , where corresponds to n 75.

capillary-based discharge plasma produces potassium emission, together with O, H, and C ionic emissions see Fig. 2 . To analyze and characterize the emission spectra from a pure potassium plasma, we did a numerical simulation assuming CRE in the plasma and combining these results with theoretical speactra calculate with the multiconguration HARTREE14 FOCK code. In addition, we also have the radiative hydrodynamics model.19 We use a laser-produced potassium plasma to evaluate the spectra and electron temperature because a discharge-produced potassium plasmas includes other elements, originating in the capillary material and the oxide lm on the potassium target surface. Use of a laserproduced plasma enables one to control the plasma parameters by changing the laser intensity power density and the wavelength, as the electron temperature and the critical density depend on the laser intensity and wavelength, respectively. To understand the plasma dynamics and to optimize the capillary discharge near the hollow electrode surface, we characterize and compare the emission spectra from the laser-produced pure potassium plasma. 40 nm emission is produced at an electron temperature of about 12 eV when the discharge current is about 200 A in a capillary of 500 m diameter. Figure 9 shows the comparison of discharge- and laser-produced potassium plasmas. A Q-switched Nd:yttrium-aluminum-garnet Nd:YAG laser at 1064 nm produced a maximum pulse energy of 400 mJ with a pulse width of 10 ns FWHM . The laser light was focused on a planar potassium target with a thickness of 1 mm placed in a vacuum chamber by use of a lens with a focal length of 40 cm. The maximum focused intensity was
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2 1010 W / cm2 with a focal spot size of 250 m FWHM . This spot size was chosen to minimize the plasma hydrodynamic expansion loss.20 The focal spot size was monitored by use of a CCD camera placed at a laser exit port by removing the potassium planar target. Figure 9 shows spectra from 20 to 60 nm from the discharge-produced plasma and the laser-produced plasma at an electron temperature close to 12 eV. The dischargeproduced plasma spectrum in Fig. 9 a is similar to the laserproduced plasma spectrum in Fig. 9 b . This similarity demonstrates that the emission from the discharge-produced plasma occurs in a region of high electron density close to 1020 cm3. Figure 10 shows the fractional ion populations in a potassium plasma as a function of electron temperature up to 15 eV for an electron density of the order of 1020 cm3. A range of ion stages is present in the plasma at any given electron temperature while higher electron temperatures produce higher ion stages. Note that the dominant species at any temperature comprises about 50% to 60% of the total ion population. Simple calculations show that the population of K4+ ions maximizes around 1013 eV at a plasma density of 1020 cm3. In addition, the ion population from K3+ to K4+ is maximized at electron temperatures from 8 to 11 eV. To determine the ion distribution, the rate equations can also be solved using the simultaneous equation method. This method is more general than the recursive relation method and can be used to include energy level populations within an ion stage, mixed ion species, and a time-dependent solution of the rate equations.
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1

1 0.8 0.6 0.4 0.2 0 20 30 40 50

(a)

Intensity (arb. units)

Intensity (arb. units)

(b)

0.8 0.6 0.4 0.2 0 20 30 40 50 60

60

Wavelength (nm)

Wavelength (nm)

FIG. 9. Time-integrated spectra from a capillary discharge-produced plasma a and from a Nd:YAG laser-produced plasma b at the laser intensity of 2 1010 W / cm2 with a focal spot size of 250 m FWHM .

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Pupulation (arb. units)

J. Appl. Phys. 109, 013301 2011

1 0.8 0.6 0.4 0.2 0 0

KI

KII KIII KIV

KV

KVI

KVII 5 10 Electron temperature (eV) 15

FIG. 10. Color online Steady-state potassium ion distributions vs temperature at the electron density of 1020 cm3.

emission intensity, which can be attributed to the K2+ to K4+ ions, because the weighted oscillator strength from the Cowan code calculation is predicted to be strong. In addition, the ion stage is increased due to higher ionization attainable at the higher electron temperature, shown in Fig. 10. The K3+ and K4+ ion emission is dominant at electron temperatures higher than 10 eV, as can be seen from Figs. 11 c 11 e . At a laser intensity of 2 1010 W / cm2, the electron temperature is evaluated to be about 10 eV. The observed spectra in Fig. 9 closely resembles the numerically calculated spectrum in Fig. 11 c which showed that 3d 3p transitions in potassium ions ranging from K2+ to K4+ present in the potassium plasma overlap to form a relatively narrow band of emission.

To understand the spectral behavior for the emission centered on 40 nm, the numerical calculations were performed using a hydrodynamic model implemented in the 19 PRISMSPECT code. This simulation code is a CRE spectral analysis code designed to simulate the atomic and radiative properties of local thermodynamic equilibrium LTE and non-LTE plasmas spanning a wide range of conditions. The spectra at different electron temperatures but at the same electron density of 1 1020 cm3 are shown in Fig. 11. When the electron temperature is low, as shown in Figs. 11 a and 11 b , emission from 50 to 55 nm is dominant due to K2+ and K3+. According to the Cowan code calculation, the weighted oscillator strength is weak. When the electron temperature increases at an electron density of the order of 1020 cm3, the main peaks move from 52 nm to the short wavelength spectral region at 38 nm with the increase in
Intensity (arb. units)
1.2 1 0.8 0.6 0.4 0.2 0 20 25 30 35 40 45 50 55 60

V. SUMMARY

In summary, we have demonstrated a compact, discharge-produced microplasma XUV source using pure potassium vapor. Potassium ions produced strong broadband emission around 40 nm with a bandwidth of 8 nm FWHM at a discharge current of 200 A and a repetition rate of 10 Hz. We have also discussed the possibility of a hollow cathode mode in the potassium plasma where the emitting ions were localized on the potassium electrode surface at the hole into the capillary. To analyze and characterize the spectra from the pure potassium plasmas, we compared the spectra of the discharge-produced plasma with that of a laser-produced plasma. The spectra at the same electron temperatures at 12 eV were almost the same. This compact capillary XUV
Intensity (arb. units)
1.2 1 0.8 0.6 0.4 0.2 0 20 25 30 35 40 45 50 55 60

(a)

(b)

Wavelength (nm)

Wavelength (nm) (c)

Intensity (arb. units)

Intensity (arb. units)

1.2 1 0.8 0.6 0.4 0.2 0 20 25 30 35 40 45 50 55 60

1.2 1 0.8 0.6 0.4 0.2 0 20 25 30 35 40 45 50 55 60

(d)

Wavelength (nm)

Wavelength (nm) (e)

Intensity (arb. units)

1.2 1 0.8 0.6 0.4 0.2 0 20 25 30 35 40 45 50 55 60

Wavelength (nm)
FIG. 11. Calculated spectra at different electron temperatures of 6 a , 8 b , 10 c , 12 d , and 14 eV e with the electron density of 1020 cm3.

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J. Appl. Phys. 109, 013301 2011 Appl. Phys. Lett. 88, 201503 2006 . T. Otsuka, D. Kilbane, J. White, T. Higashiguchi, N. Yugami, T. Yatagai, W. Jiang, A. Endo, P. Dunne, and G. OSullivan, Appl. Phys. Lett. 97, 111503 2010 . 7 N. Hirashita, M. Kinoshita, I. Aikawa, and T. Ajioka, Appl. Phys. Lett. 56, 451 1990 . 8 A. El-Habachi and K. Schoenbach, Appl. Phys. Lett. 73, 885 1998 . 9 B.-J. Lee, H. Rahaman, I. Petzenhauser, K. Frank, and K. P. Giapis, Appl. Phys. Lett. 90, 241502 2007 . 10 J. J. Rocca, V. N. Shlyaptsev, F. G. Tomasel, O. D. Cortazar, D. Hartshorn, and J. L. A. Chilla, Phys. Rev. Lett. 73, 2192 1994 . 11 G. Niimi, Y. Hayashi, M. Nakajima, M. Watanabe, A. Okino, K. Horioka, and E. Hotta, J. Phys. D 34, 2123 2001 . 12 M. Shuker, A. Ben-kish, A. Fisher, and A. Ron, Appl. Phys. Lett. 88, 061501 2006 . 13 A. J. Mendelsohn, C. P. J. Barty, M. H. Sher, J. F. Young, and S. E. Harris, Phys. Rev. A 35, 2095 1987 . 14 R. D. Cowan, The Theory of Atomic Structure and Spectra University of California Press, Berkeley, 1981 . 15 G. OSullivan and R. Faulkner, Opt. Eng. Bellingham 33, 3978 1994 . 16 D. Colombant and G. F. Tonon, J. Appl. Phys. 44, 3524 1973 . 17 A. Fiala, L. C. Pitchford, and J. P. Boeuf, Phys. Rev. E 49, 5607 1994 . 18 T. Higashiguchi, H. Terauchi, N. Yugami, T. Yatagai, W. Sasaki, R. DArcy, P. Dunne, and G. OSullivan, Appl. Phys. Lett. 96, 131505 2010 . 19 http://www.prism-cs.com/ 20 R. C. Spitzer, T. J. Orzechowski, D. W. Phillion, R. L. Kauffman, and C. Cerjan, J. Appl. Phys. 79, 2251 1996 .
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source with a photon energy of 30 eV is a useful XUV emission source for surface morphology applications.
ACKNOWLEDGMENTS

The authors are also grateful to Jin-xiang Bai and Masashi Irino for their unparalleled technical support. A part of this work was performed under the auspices of MEXT Ministry of Education, Culture, Science and Technology, Japan and Distinguished Research Projects of Utsunomiya University. One of the authors T.H. also acknowledges support from Research Foundation for Opto-Science and Technology. The UCD group acknowledges support from Science Foundation Ireland under Principal Investigator Research Grant No. 07/IN.1/B1771.
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