Abstract

We have developed an electron beam excitation ultra-soft X-ray add-on device for a scanning electron microscope with a reflective zone plate mulichannel spectrometer in order to analyse ultra-light elements such as Li and B. This spectrometer has high (λ/Δλ~100) resolving power in the energy range of 45 eV – 1120 eV. Metallic Li samples were examined and fluorescence spectra successfully measured. Energy resolution of 0.49 eV was measured in the ultra-low energy range using the Al L2,3 line at 71 eV. High sensitivity of Boron detection was demonstrated on a B4C sample with layer thicknesses of 1-50 nm, detecting an amount of metallic Boron as small as ~0.57 fg.

© 2015 Optical Society of America

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References

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  1. M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).
  2. H. Takahashi, P. McSwiggen, and C. Nielsen, “A unique wavelength-dispersive soft X-ray emission spectrometer for electron probe X-ray microanalyzers,” Microsc. Anal. (Am. Ed.) 28(7), 4–7 (2014).
  3. T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
    [Crossref]
  4. A. Erko, A. Firsov, and F. Senf, “Novel parallel vacuum ultra-violet/X-ray fluorescence spectrometer,” Spectrochim. Acta B At. Spectrosc. 67, 57–63 (2012).
    [Crossref]
  5. A. Erko, A. Firsov, R. Gubzhokov, A. Bjeoumikhov, A. Günther, N. Langhoff, M. Bretschneider, Y. Höhn, and R. Wedell, “New parallel wavelength-dispersive spectrometer based on scanning electron microscope,” Opt. Express 22(14), 16897–16902 (2014).
    [Crossref] [PubMed]
  6. A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
    [Crossref]
  7. J. John, Friel, X-Ray and Image Analysis in Electron Microscopy 2nd ed. (Princeton Gamma-Tech, 2005), p. 26.
  8. J. A. Catterall and J. Trotter, “Soft x-ray emission spectra from lithium and lithium-magnesium alloys,” Philos. Mag. 4(46), 1164–1170 (1959).
    [Crossref]
  9. D. E. Bedo and D. H. Tomboulian, “K-emission spectrum of metallic lithium,” Phys. Rev. 109(1), 35–40 (1958).
    [Crossref]
  10. R. S. Crisp and S. E. Williams, “The K emission spectrum of metallic lithium,” Philos. Mag. 5(53), 525–527 (1960).
    [Crossref]

2014 (3)

H. Takahashi, P. McSwiggen, and C. Nielsen, “A unique wavelength-dispersive soft X-ray emission spectrometer for electron probe X-ray microanalyzers,” Microsc. Anal. (Am. Ed.) 28(7), 4–7 (2014).

A. Erko, A. Firsov, R. Gubzhokov, A. Bjeoumikhov, A. Günther, N. Langhoff, M. Bretschneider, Y. Höhn, and R. Wedell, “New parallel wavelength-dispersive spectrometer based on scanning electron microscope,” Opt. Express 22(14), 16897–16902 (2014).
[Crossref] [PubMed]

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

2012 (2)

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

A. Erko, A. Firsov, and F. Senf, “Novel parallel vacuum ultra-violet/X-ray fluorescence spectrometer,” Spectrochim. Acta B At. Spectrosc. 67, 57–63 (2012).
[Crossref]

1997 (1)

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

1960 (1)

R. S. Crisp and S. E. Williams, “The K emission spectrum of metallic lithium,” Philos. Mag. 5(53), 525–527 (1960).
[Crossref]

1959 (1)

J. A. Catterall and J. Trotter, “Soft x-ray emission spectra from lithium and lithium-magnesium alloys,” Philos. Mag. 4(46), 1164–1170 (1959).
[Crossref]

1958 (1)

D. E. Bedo and D. H. Tomboulian, “K-emission spectrum of metallic lithium,” Phys. Rev. 109(1), 35–40 (1958).
[Crossref]

Bedo, D. E.

D. E. Bedo and D. H. Tomboulian, “K-emission spectrum of metallic lithium,” Phys. Rev. 109(1), 35–40 (1958).
[Crossref]

Berglund, M.

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

Bjeoumikhov, A.

Bretschneider, M.

Catterall, J. A.

J. A. Catterall and J. Trotter, “Soft x-ray emission spectra from lithium and lithium-magnesium alloys,” Philos. Mag. 4(46), 1164–1170 (1959).
[Crossref]

Crisp, R. S.

R. S. Crisp and S. E. Williams, “The K emission spectrum of metallic lithium,” Philos. Mag. 5(53), 525–527 (1960).
[Crossref]

Eggenstein, F.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Erko, A.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

A. Erko, A. Firsov, R. Gubzhokov, A. Bjeoumikhov, A. Günther, N. Langhoff, M. Bretschneider, Y. Höhn, and R. Wedell, “New parallel wavelength-dispersive spectrometer based on scanning electron microscope,” Opt. Express 22(14), 16897–16902 (2014).
[Crossref] [PubMed]

A. Erko, A. Firsov, and F. Senf, “Novel parallel vacuum ultra-violet/X-ray fluorescence spectrometer,” Spectrochim. Acta B At. Spectrosc. 67, 57–63 (2012).
[Crossref]

Firsov, A.

Follath, R.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Gubzhokov, R.

Günther, A.

Hambach, D.

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

Handa, N.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Hertz, H. M.

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

Höhn, Y.

Imazono, T.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Kawachi, T.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Koeda, M.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Koike, M.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Künstner, S.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Kuramoto, S.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Langhoff, N.

Mast, M.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

McSwiggen, P.

H. Takahashi, P. McSwiggen, and C. Nielsen, “A unique wavelength-dispersive soft X-ray emission spectrometer for electron probe X-ray microanalyzers,” Microsc. Anal. (Am. Ed.) 28(7), 4–7 (2014).

Murano, T.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Nagano, T.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Nielsen, C.

H. Takahashi, P. McSwiggen, and C. Nielsen, “A unique wavelength-dispersive soft X-ray emission spectrometer for electron probe X-ray microanalyzers,” Microsc. Anal. (Am. Ed.) 28(7), 4–7 (2014).

Niemann, B.

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

Oue, Y.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Rymell, L.

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

Sasai, H.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Schäfers, F.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Schmidt, J.-S.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Senf, F.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

A. Erko, A. Firsov, and F. Senf, “Novel parallel vacuum ultra-violet/X-ray fluorescence spectrometer,” Spectrochim. Acta B At. Spectrosc. 67, 57–63 (2012).
[Crossref]

Siewert, F.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Sokolov, A. A.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Takahashi, H.

H. Takahashi, P. McSwiggen, and C. Nielsen, “A unique wavelength-dispersive soft X-ray emission spectrometer for electron probe X-ray microanalyzers,” Microsc. Anal. (Am. Ed.) 28(7), 4–7 (2014).

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Terauchi, M.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Tomboulian, D. H.

D. E. Bedo and D. H. Tomboulian, “K-emission spectrum of metallic lithium,” Phys. Rev. 109(1), 35–40 (1958).
[Crossref]

Trotter, J.

J. A. Catterall and J. Trotter, “Soft x-ray emission spectra from lithium and lithium-magnesium alloys,” Philos. Mag. 4(46), 1164–1170 (1959).
[Crossref]

Wedell, R.

Wilhein, T.

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

Williams, S. E.

R. S. Crisp and S. E. Williams, “The K emission spectrum of metallic lithium,” Philos. Mag. 5(53), 525–527 (1960).
[Crossref]

Yonezawa, Z.

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Zeschke, T.

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Appl. Phys. Lett. (1)

T. Wilhein, D. Hambach, B. Niemann, M. Berglund, L. Rymell, and H. M. Hertz, “Off-axis reflection zone plate for quantitative soft x-ray source characterization,” Appl. Phys. Lett. 71(2), 190–192 (1997).
[Crossref]

JEOL News (1)

M. Terauchi, H. Takahashi, N. Handa, T. Murano, M. Koike, T. Kawachi, T. Imazono, M. Koeda, T. Nagano, H. Sasai, Y. Oue, Z. Yonezawa, and S. Kuramoto, “A new WDS spectrometer for valence electron spectroscopy based on electron microscopy,” JEOL News 47(1), 23–28 (2012).

Microsc. Anal. (Am. Ed.) (1)

H. Takahashi, P. McSwiggen, and C. Nielsen, “A unique wavelength-dispersive soft X-ray emission spectrometer for electron probe X-ray microanalyzers,” Microsc. Anal. (Am. Ed.) 28(7), 4–7 (2014).

Opt. Express (1)

Philos. Mag. (2)

J. A. Catterall and J. Trotter, “Soft x-ray emission spectra from lithium and lithium-magnesium alloys,” Philos. Mag. 4(46), 1164–1170 (1959).
[Crossref]

R. S. Crisp and S. E. Williams, “The K emission spectrum of metallic lithium,” Philos. Mag. 5(53), 525–527 (1960).
[Crossref]

Phys. Rev. (1)

D. E. Bedo and D. H. Tomboulian, “K-emission spectrum of metallic lithium,” Phys. Rev. 109(1), 35–40 (1958).
[Crossref]

Proc. SPIE (1)

A. A. Sokolov, F. Eggenstein, A. Erko, R. Follath, S. Künstner, M. Mast, J.-S. Schmidt, F. Senf, F. Siewert, T. Zeschke, and F. Schäfers, “An XUV optics beamline at BESSY II,” Proc. SPIE 9206, 92060J (2014).
[Crossref]

Spectrochim. Acta B At. Spectrosc. (1)

A. Erko, A. Firsov, and F. Senf, “Novel parallel vacuum ultra-violet/X-ray fluorescence spectrometer,” Spectrochim. Acta B At. Spectrosc. 67, 57–63 (2012).
[Crossref]

Other (1)

J. John, Friel, X-Ray and Image Analysis in Electron Microscopy 2nd ed. (Princeton Gamma-Tech, 2005), p. 26.

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Figures (6)

Fig. 1
Fig. 1

RAW CCD image with 0th and −1st diffraction orders marked. H0 indicates the calculated distance between the edge of the specular reflex (zone plate) and focus of −1st order.

Fig. 2
Fig. 2

Composition of the thin layer B4C samples.

Fig. 3
Fig. 3

Full B4C spectra with subtracted Si background and normalized data for different B4C layer thicknesses.

Fig. 4
Fig. 4

Al L spectrum, showing the Fermi edge (left). The resolution is estimated based on the FWHM of the derivative.

Fig. 5
Fig. 5

Metallic lithium sample. Lighter color shows oxidized areas and darker color shows pure Li metal.

Fig. 6
Fig. 6

Normalized spectrum of metallic Li with a marked Fermi edge width.

Tables (2)

Tables Icon

Table 1 Characteristic fluorescence line energies for the 17-channel RZPs and their efficiency in % (theoretical calculations, B – measured value))

Tables Icon

Table 2 Characteristic fluorescence line energies for the 14-channel RZPs and their efficiency in %, measured values.

Equations (5)

Equations on this page are rendered with MathJax. Learn more.

R=0.064 E 0 1.68 E c 1.68 ρ ,
V=π ( Δx 2 ) 2 l=2.89 10 22 m 3 .
N= N A ρV M B 4 C =7.94 10 6 ,
m= M B N B N A =5.72 10 16 g.
m=0.57fg±0.144fg.

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