liquid-metal-jet - national institute of standards and ... · liquid-metal-jet x-ray tube...

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LIQUID-METAL-JET X-RAY TUBE TECHNOLOGY FOR NANOELECTRONICS CHARACTERIZATION AND METROLOGY EXTREME BRIGHTNESS POWER LOADING CAPABILITY The x-ray power of all electron-impact x-ray genera- tors is limited by the thermal power loading of the an- ode. In conventional solid anode technology, the sur- face temperature of the anode must be well below the melting point in order to avoid damage and this is fun- damentally limited by the anode target material proper- ties, primarily the melting point, the vapor pressure and especially the thermal conductivity. The liquid-metal anode is different since the limitation to maintain the target at well below melting point in removed. This is due to the fact that the material is already molten and that it is regenerative by nature, supplying new fresh target material at a rate of close to 100 m/s. This means that the electron beam and anode interaction may be destructive. EXTREME BRIGHTNESS Somewhat counter intuitively, the power loading capa- bility of small-focus x-ray tubes roughly scale with the diameter and not the area of the e-beam focus. There- fore, the brightness is inversely proportional with the source diameter. By combining extreme power loading capability and a small electron focus, a liquid-jet-source can achieve unprecedented brightness at micron spot sizes. 0 500 1000 1500 2000 2500 3000 0.1 1 10 100 1000 Power Density [kW/mm2] Apparent Source Diameter [µm] E-beam power density Liquid Metal Jet Rotating Anode (1:10 line focus) Solid Target Solid Target (1:10 line focus) Transmission Target 0 1 10 100 1000 10000 100000 0.1 1 10 100 1000 Power [W] Apparent Source Diameter [µm] E-beam Power Liquid Metal Jet Rotating Anode (1:10 line focus) Solid Target Solid Target (1:10 line focus) Transmission Target Extreme performance for 5-40 μm source diameter SOURCE SCHEMATICS Advanced electro- magnetic focusing and correctional optics together with a high brightness LaB 6 cathode results in a very high qual- ity e-beam focus. Pumps etc. are housed in a 19” box. Electronics is housed in two 19” boxes. The path of the continuously recycled liquid metal alloy. 691 mm 335 mm X-rays are emitted from the interaction point between the metal jet and the e-beam. STATE OF THE ART HOME LAB SCATTERING The MetalJet-technology is very well suited for Small Angle X-ray Scattering (SAXS), due to the small spot-size and high brightness. This has been proven in traditional SAXS, and in the figure be- low, you will find an comparison of different X-ray tubes, where rat tail tendon was studied. SMALL ANGLE SCATTERING Data courtesy of J. Lange, A. Schwamberger and K. Erlacher of Bruker-AXS. Integral of reflection 1: 1.2 counts per second Integral of reflection 2: 1 counts per second Integral of reflection 1: 22 counts per second Integral of reflection 2: 29 counts per second Integral of reflection 1: 68 counts per second Integral of reflection 2: 89 counts per second Solid Anode Microfocus X-ray Tube Rotating Anode Microfocus X-ray Tube MetalJet Microfocus X-ray Tube 57× - 89× improvement 3.1× improvement CRITICAL DIMENSION-SAXS Research on critical dimension small angle X-ray scattering (CD-SAXS) [1] have identified that lab- based X-ray sources with higher brightness than previously available, at energies higher than 20 keV are needed for non-synchrotron CD-SAXS. The MetalJet source technology with indium K-α emis- sion at 24 keV show great promise towards meeting the requirements. 1. R. J. Kline, D. F. Sunday, D. Windover and W. Wu, ‘Bringing CD-SAXS to the Fab’, SEMICON West 2014, 2014. CURRENTLY AVAILABLE SOURCE MetalJet D2 TECHNICAL SPECIFICATIONS Cathode LaB 6 Min. focal spot size ~5 μm Target Material 1 Ga or In rich alloy Emission stability 3 < 1% Max current 4.3 mA Position stability 3 < 1 μm Voltage 2 10 - 70 kV / 160 kV Min. focus-object distance 4 18mm Power 0 - 300 W / 1000 W Beam angle 13° or 30° 1) The room temperature liquid metal alloys supplied for the MetalJet source consist mainly of gallium, indium and tin. They have low reactivity and low toxicity but should be handled according to their safety data sheets and local regulations. 2) Depending on source version 3) Standard deviation 4) Without a shutter PERFORMANCE EXAMPLES (Exally G1, 70kV) Spot size 5 [μm, FWHM] E-Beam Power [W] Ga Kα Flux [Photons/(smrad 2 line)] Ga Kα Peak Brightness [Photons/(smm 2 mrad 2 line)] 5 50 3.0×10 6 1.0×10 11 10 100 6.0×10 6 5.2×10 10 20 200 1.2×10 7 2.6×10 10 5) Actual e-beam spot has a 1:4 aspect-ratio line focus, but the projected spot dimension is essentially circular. True round focal spots for, e.g., large-angle imaging can typically generate ¼ power compared to the numbers above. MetalJet D2 The MetalJet D2 is the second “off the shelf” commer- cially available liquid-metal-jet x-ray source. This is a fully radiation shielded dual port source with shutters. The source can be operated stand alone or is easily inte- grated. −50 0 50 0 0.2 0.4 0.6 0.8 1 Line profile through maximum [μm] [a.u.] Horizontal Vertical SPOT SIZE AND STABILITY SPOT QUALITY Thanks to advanced electro- magnetic focusing and cor- rectional optics together with a high brightness LaB 6 cath- ode, a high quality e-beam focus is achieved. Together with a continuously generated smooth liquid target surface, the source produces x-ray spots of very high quality. TUNABLE SIZE Both the spot size and the as- pect ratio can be tuned freely. SOURCE STABILITY The spatial stability of the source is very high. The images to the left illustrate a spot centroid stan- dard deviation of < 0.1 μm over 24 hours, as taken with pinhole camera mechanically coupled to the source. -0.4 -0.3 -0.2 -0.1 0 0.1 0.2 0.3 0.4 -0.2 -0.1 0 0.1 0.2 0.3 X position [μm] Y position [μm] 0 5 10 15 20 0.3 0.2 0.1 0 0.1 0.2 Position [μm] x − center of mass y − center of mass Time [h] Spot position over 24h Spot position over 24h [mm] [mm] X−ray spot -50 0 50 50 0 -50 0 500 1000 1500 Image of JIMA resolution target with 6x6 μm x-ray spot centered on liquid jet. 4 μm horizontal lines and 2 μm vertical lines are clearly resolved, supporting the high spot quality. X-RAY SPECTRA X-RAY SPECTRA OF LIQUID METAL In order to reach different x-ray emission lines, different metal alloys are used. First generation metal-jet sources feature metal alloys that are molten at more or less room temperature. Still, several alloys have emis- sion characteristics similar to regular solid anodes. Future upgrades can also include al- loys with higher melting points. GALLIUM ALLOY A gallium (Ga) rich alloy is available. It’s 9.2 keV Kα emission line is close to the copper (Cu) Kα emission line. INDIUM ALLOY An indium (In) rich alloy is also available. It’s 24.2 keV Kα emission line is close to the silver (Ag) Kα emission line. 1E+07 1E+08 1E+09 1E+10 1E+11 1E+12 0 20 40 60 X-Ray Flux [au] Energy [keV] Spectra of Gallium alloy and Copper Gallium (Ga) Alloy Copper (Cu) Ga Kα Cu Kα 1E+07 1E+08 1E+09 1E+10 1E+11 1E+12 0 20 40 60 X-Ray Flux [au] Energy [keV] Spectra of Indium alloy and Silver Indium (In) Alloy Silver (Ag) In Kα Ag Kα TXRF USING METALJET Total reflection X-ray spectroscopy (TXRF) is a power- ful analytical technique for qualitative and quantitative analysis of trace and ultra-trace elements in a sample. Historically several different x-ray sources has been used for this technique. A. Maderitsch et al. from Atominstitut, Vienna University of Technology, has performed TXRF- measurements with the MetalJet technology [4]. A TXRF spectrometer designed at the Atominstitut was adapted to the MetalJet, and several measurements were performed. As a reference, the same spectrometer was used with a 2 kW diffraction long fine focus x-ray tube (Cu-Kα). For comparison, the measurements were normalized to the x-ray tube current and to the counts per second (cps). The results are presented in the spectrum to the right. The high brilliance of the MetalJet gives a great yield of the primary photons. Also, the normalized Mn signal is higher with the MetalJet, even though the excitation of Mn is better with Cu-Kα radiation. 4. A. Maderitsch, S. Smolek, P. Wobrauschek, C. Streli and P. Takman, Feasibility study of TXRF using a liquid metal jet X-Ray tube, Spectrochimica Acta Part B: Atomic Spectroscopy, TXRF2013 special issue X-RAY MICROSCOPY 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 0 2000 4000 6000 8000 10000 12000 14000 Transmission Photon energy (eV) Filter transmission, 0.2 µm filter Si Cu Traditionally the MetalJet-technology has been used extensively for phase-contrast imaging, both in propagation- and grating-based x-ray phase contrast imaging. The MetalJet-technology is very well suited for this type of imaging due to the fine spot-size and very high-brightness. More recently, a growing interest in using the MetalJet-technology for imaging of nanoelectronics has emerged. The highest available res- olution in lab-based X-ray micro- scopes is achieved with zone-plate based projection microscopes [2]. Such microscopes, however, typi- cally use Cu Kα (~8 keV) radiation which is not so well suited to see copper structures in silicon due to poor contrast between copper and silicon at that energy. As illustrated by the graph to the right, the Kα of gallium, which is used in MetalJet sources, is just above the K-absorption edge of copper [3] and thus much better suited to create a sufficient contrast between copper and silicon. 2. T. Beetz, ‘High-resolution X-ray Tomography Imaging Systems’, CHESS Users’ Meeting Ithaca, NY, 2008. 3. E. Gullikson, Filter transmission, http://henke.lbl.gov/optical_constants/filter2.html, visited on 2015-03-24. Gallium Kα DETAILS A conventional microfocus x-ray tube with the solid-metal anode replaced by a liquid-metal jet. The metal jet supports higher electron-beam power and can therefore generate higher x-ray flux. Emil Espes, Björn A. M. Hansson, Oscar Hemberg, Göran Johansson,Mikael Otendal, Tomi Tuohimaa and Per Takman www.excillum.com [email protected]

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Page 1: LIQUID-METAL-JET - National Institute of Standards and ... · liquid-metal-jet x-ray tube technology for nanoelectronics characterization and metrology extreme brightness power loading

LIQUID-METAL-JET X-RAY TUBE TECHNOLOGYFOR NANOELECTRONICS CHARACTERIZATION AND METROLOGY

EXTREME BRIGHTNESSPOWER LOADING CAPABILITYThe x-ray power of all electron-impact x-ray genera-tors is limited by the thermal power loading of the an-ode. In conventional solid anode technology, the sur-face temperature of the anode must be well below the melting point in order to avoid damage and this is fun-damentally limited by the anode target material proper-ties, primarily the melting point, the vapor pressure and especially the thermal conductivity. The liquid-metal anode is different since the limitation to maintain the target at well below melting point in removed. This is due to the fact that the material is already molten and that it is regenerative by nature, supplying new fresh target material at a rate of close to 100 m/s. This means that the electron beam and anode interaction may be destructive.

EXTREME BRIGHTNESSSomewhat counter intuitively, the power loading capa-bility of small-focus x-ray tubes roughly scale with the diameter and not the area of the e-beam focus. There-fore, the brightness is inversely proportional with the source diameter.

By combining extreme power loading capability and a small electron focus, a liquid-jet-source can achieve unprecedented brightness at micron spot sizes.

0

500

1000

1500

2000

2500

3000

0.1 1 10 100 1000

Pow

er D

ensi

ty [k

W/m

m2]

Apparent Source Diameter [µm]

E-beam power density

Liquid Metal Jet

Rotating Anode(1:10 line focus)Solid Target

Solid Target(1:10 line focus)TransmissionTarget

0

1

10

100

1000

10000

100000

0.1 1 10 100 1000

Pow

er [W

]

Apparent Source Diameter [µm]

E-beam Power

Liquid Metal Jet

Rotating Anode(1:10 line focus)Solid Target

Solid Target(1:10 line focus)TransmissionTarget

Extreme performance for 5-40 μm source

diameter

SOURCE SCHEMATICS

Advanced electro-magnetic focusing and correctional optics together with a high brightness LaB6 cathode results in a very high qual-ity e-beam focus.Pumps etc. are

housed in a 19” box.

Electronics is housed in two 19” boxes.

The path of the continuously recycled liquid metal alloy.

691 mm

335 mm

X-rays are emitted from the interaction point between the metal jet and the e-beam.

STATE OF THE ART HOME LAB SCATTERINGThe MetalJet-technology is very well suited for Small Angle X-ray Scattering (SAXS), due to the small spot-size and high brightness. This has been proven in traditional SAXS, and in the fi gure be-low, you will fi nd an comparison of different X-ray tubes, where rat tail tendon was studied.

SMALL ANGLE SCATTERING

Data courtesy of J. Lange, A. Schwamberger and K. Erlacher of Bruker-AXS.

Integral of reflection 1:1.2 counts per second

Integral of reflection 2:1 counts per second

Integral of reflection 1:22 counts per second

Integral of reflection 2:29 counts per second

Integral of reflection 1:68 counts per second

Integral of reflection 2:89 counts per second

Solid Anode Microfocus X-ray Tube

Rotating Anode Microfocus X-ray Tube

MetalJet Microfocus X-ray Tube

57× - 89× improvement

3.1× improvement

CRITICAL DIMENSION-SAXSResearch on critical dimension small angle X-ray scattering (CD-SAXS) [1] have identifi ed that lab-based X-ray sources with higher brightness than previously available, at energies higher than 20 keV are needed for non-synchrotron CD-SAXS. The MetalJet source technology with indium K-α emis-sion at 24 keV show great promise towards meeting the requirements.

1. R. J. Kline, D. F. Sunday, D. Windover and W. Wu, ‘Bringing CD-SAXS to the Fab’, SEMICON West 2014, 2014.

CURRENTLY AVAILABLE SOURCE

MetalJet D2 TECHNICAL SPECIFICATIONSCathode LaB6 Min. focal spot size ~5 μm

Target Material1 Ga or In rich alloy Emission stability3 < 1%

Max current 4.3 mA Position stability3 < 1 μm

Voltage2 10 - 70 kV / 160 kV Min. focus-object distance4 18mm

Power 0 - 300 W / 1000 W Beam angle 13° or 30°1) The room temperature liquid metal alloys supplied for the MetalJet source consist mainly of gallium, indium and tin. They have low reactivity and low toxicity but should be handled according to their safety data sheets and local regulations. 2) Depending on source version3) Standard deviation4) Without a shutter

PERFORMANCE EXAMPLES (Exally G1, 70kV)Spot size5

[μm, FWHM]E-Beam Power

[W]Ga Kα Flux

[Photons/(s∙mrad2∙line)]Ga Kα Peak Brightness

[Photons/(s∙mm2∙mrad2∙line)]5 50 3.0×106 1.0×1011

10 100 6.0×106 5.2×1010

20 200 1.2×107 2.6×1010

5) Actual e-beam spot has a 1:4 aspect-ratio line focus, but the projected spot dimension is essentially circular. True round focal spots for, e.g., large-angle imaging can typically generate ¼ power compared to the numbers above.

MetalJet D2The MetalJet D2 is the second “off the shelf” commer-cially available liquid-metal-jet x-ray source. This is a fully radiation shielded dual port source with shutters. The source can be operated stand alone or is easily inte-grated.

−50 0 500

0.2

0.4

0.6

0.8

1

Line profile through maximum

[µm]

[a.u.]

HorizontalVertical

SPOT SIZE AND STABILITYSPOT QUALITYThanks to advanced electro-magnetic focusing and cor-rectional optics together with a high brightness LaB6 cath-ode, a high quality e-beam focus is achieved. Together with a continuously generated smooth liquid target surface, the source produces x-ray spots of very high quality.

TUNABLE SIZEBoth the spot size and the as-pect ratio can be tuned freely.

SOURCE STABILITYThe spatial stability of the source is very high. The images to the left illustrate a spot centroid stan-dard deviation of < 0.1 µm over 24 hours, as taken with pinhole camera mechanically coupled to the source.

-0.4 -0.3 -0.2 -0.1 0 0.1 0.2 0.3 0.4

-0.2

-0.1

0

0.1

0.2

0.3

X position [μm]

Y po

sitio

n [μ

m]

0 5 10 15 20

0.3

0.2

0.1

0

0.1

0.2

Pos

ition

[µm

]

x − center of massy − center of mass

Time [h]

Spot position over 24h Spot position over 24h

[mm]

[mm

]

X−ray spot

-50 0 50

50

0

-50 0

500

1000

1500

Image of JIMA resolution target with 6x6 µm x-ray spot centered on liquid jet. 4 µm horizontal lines and 2 µm vertical lines are clearly resolved, supporting the high spot quality.

X-RAY SPECTRAX-RAY SPECTRA OF LIQUID METALIn order to reach different x-ray emission lines, different metal alloys are used. First generation metal-jet sources feature metal alloys that are molten at more or less room temperature. Still, several alloys have emis-sion characteristics similar to regular solid anodes. Future upgrades can also include al-loys with higher melting points.

GALLIUM ALLOYA gallium (Ga) rich alloy is available. It’s 9.2 keV Kα emission line is close to the copper (Cu) Kα emission line.

INDIUM ALLOYAn indium (In) rich alloy is also available. It’s 24.2 keV Kα emission line is close to the silver (Ag) Kα emission line.

1E+07

1E+08

1E+09

1E+10

1E+11

1E+12

0 20 40 60

X-Ra

y Fl

ux [a

u]

Energy [keV]

Spectra of Gallium alloy and Copper

Gallium (Ga) Alloy

Copper (Cu)

Ga Kα

Cu Kα

1E+07

1E+08

1E+09

1E+10

1E+11

1E+12

0 20 40 60

X-Ra

y Fl

ux [a

u]

Energy [keV]

Spectra of Indium alloy and Silver

Indium (In) Alloy

Silver (Ag)

In Kα

Ag Kα

TXRF USING METALJETTotal refl ection X-ray spectroscopy (TXRF) is a power-ful analytical technique for qualitative and quantitative analysis of trace and ultra-trace elements in a sample. Historically several different x-ray sources has been used for this technique. A. Maderitsch et al. from Atominstitut, Vienna University of Technology, has performed TXRF-measurements with the MetalJet technology [4].

A TXRF spectrometer designed at the Atominstitut was adapted to the MetalJet, and several measurements were performed. As a reference, the same spectrometer was used with a 2 kW diffraction long fi ne focus x-ray tube (Cu-Kα). For comparison, the measurements were normalized to the x-ray tube current and to the counts per second (cps). The results are presented in the spectrum to the right.

The high brilliance of the MetalJet gives a great yield of the primary photons. Also, the normalized Mn signal is higher with the MetalJet, even though the excitation of Mn is better with Cu-Kα radiation.

4. A. Maderitsch, S. Smolek, P. Wobrauschek, C. Streli and P. Takman, Feasibility study of TXRF using a liquid metal jet X-Ray tube, Spectrochimica Acta Part B: Atomic Spectroscopy, TXRF2013 special issue

X-RAY MICROSCOPY

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

0 2000 4000 6000 8000 10000 12000 14000

Tran

smiss

ion

Photon energy (eV)

Filter transmission, 0.2 µm filter

Si

Cu

Traditionally the MetalJet-technology has been used extensively for phase-contrast imaging, both in propagation- and grating-based x-ray phase contrast imaging. The MetalJet-technology is very well suited for this type of imaging due to the fi ne spot-size and very high-brightness.

More recently, a growing interest in using the MetalJet-technology for imaging of nanoelectronics has emerged. The highest available res-olution in lab-based X-ray micro-scopes is achieved with zone-plate based projection microscopes [2]. Such microscopes, however, typi-cally use Cu Kα (~8 keV) radiation which is not so well suited to see copper structures in silicon due to poor contrast between copper and silicon at that energy. As illustrated by the graph to the right, the Kα of gallium, which is used in MetalJet sources, is just above the K-absorption edge of copper [3] and thus much better suited to create a suffi cient contrast between copper and silicon.

2. T. Beetz, ‘High-resolution X-ray Tomography Imaging Systems’, CHESS Users’ Meeting Ithaca, NY, 2008.3. E. Gullikson, Filter transmission, http://henke.lbl.gov/optical_constants/fi lter2.html, visited on 2015-03-24.

Gallium Kα

DETAILS

A conventional microfocus x-ray tube with the solid-metal anode replaced by a liquid-metal jet. The metal jet supports higher electron-beam power and can therefore generate higher x-ray flux.

Emil Espes, Björn A. M. Hansson, Oscar Hemberg, Göran Johansson,Mikael Otendal, Tomi Tuohimaa and Per Takman

[email protected]