High Yield Structured X-ray Photo-Cathode Development and Fabrication

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High Yield Structured X-ray Photo-Cathode Development and Fabrication K. Opachich, P. Ross, J. Koch (NSTec, LLC) A. MacPhee, O. Landen, D. Bradley, P. Bell, S. Nagel (LLNL) T. Hilsabeck (GA) N. Chen, S. Udin, A. Gopal (NanoShift, LLC) August 13, 2015 This work was done by National Security Technologies, LLC, under Contract No. DE-AC52-06NA25946 with the U.S. Department of Energy. DOE/NV/25946--2534.

Outline Overview X-ray detectors at NIF. What are structured photocathodes? Yield enhancement at grazing incidence. Utilization of 3-D structures. Photocathode Modeling Design and Fabrication Details Effects of photocathode geometries on detector performance. Photocathode design considerations and requirements for X-ray imagers. CST studio suite simulation results for recessed photocathode geometries. Fabrication details and results. Future work.

X-ray Detectors at NIF: DISC, SPIDER and DIXI Dilation X-ray Imager (DIXI) Effective gate time <10 ps. Best spatial resolution at focus 225 µm. Uses CsI and Au photocathodes in pulsed mode (up to -1 kv at peak). Used currently in the 1-8 kev X-ray range.

X-ray Detectors at NIF: DISC, SPIDER and DIXI Diagnostic Insertion Manipulator Imaging Streak Camera (DISC) and Streaked Polar Instrumentation for Diagnosing Energetic Radiation (SPIDER) Kentech low magnification streak camera Best temporal resolution (10 ps) Best spatial resolution at focus 90 µm Uses CsI and Au photocathodes Used in the 1-8 kev X-ray range

Advanced Radiographic Capability (ARC) will push the X-ray Energies >20 kev T. Hara RSI Vol. 71 (10) p 3624-10 kv 2 mm e - Mesh E Field - 15 kv Cathode X-ray Yield drops above 10 kev. Difficult to use due to low signal levels.

Matching the X-ray path length to the escape depth at grazing incidence increases the electron yield e- Not detected e- e-x We really measure yield generated within ~20 215 Å of the surface (photoelectron escape depth limited ) e- 10 Å escape depth 700Å 10 Å escape depth X-ray beam Shallow incidence angles are needed to increase X-ray path length through the top most emission surface.

Previous Measurements show ~4x increase in yield at grazing incidence 1 kev X-ray energy 1000 Å CsI cathode D. Lowney Proc. of SPIE Vol. 5194 p 139 Electron yield shows an angle dependence near the critical angle (~5 degrees for 1 kev X-ray photons).

Predicted Yield Increase for a Au Photocathode at several X-ray energies An incidence angle of 10-15 degrees was chosen as the initial model parameter. How is this implemented at normal incidence?

A 3-D structure can be utilized to generate a yield increase in current detectors Si substrate At 15 the X-ray interaction length is increased to 75Å 200 Å of Au X-ray incidence angle of ~15 degrees X-ray beam Shape would vary depending on energy range and detector requirements.

Several structures were modeled in CST Studio suite Pillar geometries Recessed geometries

Photocathode Design Considerations for Time Dilated and Streaked X-ray Imagers Geometry: -Self supporting, large area cathodes are needed. Spatial Resolution: -The spatial resolution requirement is ~50 µm for DISC and <200 µm for DIXI. Temporal Resolution: -The temporal resolution must be within the current best NIF X-ray diagnostic resolution. Current resolution is ~10 ps (for DISC). High E - Field: -Structure must not field emit in large voltage gradients (as high as 10 kv/mm). Cathode Materials: -Currently Au and CsI are used and must be supported by the structure design.

Photocathode geometry will impact the detector performance Field emission from corners Degradation in spatial resolution depends on: Wall angle, field strength and structure separation. Loss of field between walls causes temporal resolution degradation

High Energy Cathode Design Cone Cavity Structures Field Gradient Model Field emission is suppressed and field present within the cavity. 4x10 6 V/m 2x10 6 V/m 0 V/m

Spatial resolution element is limited by the emission from the structure walls The diameter of the emitted resolution element is set by the structure diameter, the secondary electron energy and the E- Field.

Spatial resolution shows a dependence on structure geometry and can be easily adjusted

Total Yield Enhancement is on the order of 2-3 at 14 kev Photon Energy Energy (kev) Recessed Geometry Incidence Angle Diameter (µm) Depth (µm) Au Rel. Increase 14 Cone 15 9 3 1.6 14 Cone 15 9 8.4 2.36 14 Cone 15 9 16.8 2.81 Temporal spread from 9 x3 µm geometry ~1 ps. Temporal spread from 9 x 16.8 µm geometry ~100-200 ps. Full cone geometry yield increase ~4 x. Design can be easily tailored to meet X-ray detector requirements.

Prototypes have been developed based on the recessed cone geometry Requirement # Description Value Tolerance 1 Wall Angle 12º ±2.5 2 Depth 3/8.4/16.8 (µm) ±2 (µm) 3 Pitch 2 (µm) ±0.2 (µm) 4 Width 9 ±0.2 (µm) 5 Coating Thickness 20 Å Ti / 700 Å Au ±200 Å 6 Coating Roughness 200 Å 7 Substrate Thickness 150 (µm) ±2 (µm)

The fabrication steps developed by NanoShift, LLC include 6 Deep Reactive-ion Etching (DRIE) steps Photoresist Device Layer Box Layer Handle Layer Metal Layer Substrates coated with Ti+Au using sputter deposition.

Final prototypes meet the fabrication requirements (a) (b) (c) (d) 91.37 nm 91.61 nm 112.7 nm

Further work Prototype testing Conduct a direct comparison of measured TEY from planar and structured photocathodes at a synchrotron source in the 5-12 kev range. Full scale development and testing Develop a full scale 5 x 31 mm photocathode for DISC. Test in a calibrated DISC detector for full performance characterization.

References Fraser, G. W. (1983). "The characterization of soft X-ray photocathodes in the wavelength band 1-300 A. II. Caesium iodide and other insulators of high photoelectric yield." Nuclear Instruments and Methods in Physics Research 206(1-2): 265-279. Fraser, G. W. (1983). "THE CHARACTERIZATION OF SOFT-X-RAY PHOTO- CATHODES IN THE WAVELENGTH BAND 1-300 A.1. LEAD GLASS, LITHIUM- FLUORIDE AND MAGNESIUM FLUORIDE." Nuclear Instruments & Methods in Physics Research 206(1-2): 251-263. Henke, B. L. (1972). "Ultrasoft X-ray reflection refraction and production of photoelectrons (100-1000-eV region)." Physical Review A (General Physics) 6(1): 94-104.

References Henke, B. L., E. M. Gullikson, et al. (1993). "X-Ray Interactions: Photoabsorption, Scattering, Transmission, and Reflection at E = 50-30,000 ev, Z = 1-92." Atomic Data and Nuclear Data Tables 54(2): 181-342. Henke, B. L., J. P. Knauer, et al. (1981). "The characterization of x-ray photocathodes in the 0.1--10-keV photon energy region." Journal of Applied Physics 52(3): 1509-1520. Lowney, D. P., P. A. Heimann, et al. (2004). "Characterization of CsI photocathodes at grazing incidence for use in a unit quantum efficiency x-ray streak camera." Review of Scientific Instruments 75(10): 3131-3137.

Total Yield Enhancement is on the order of 2-3 at 14 kev Photon Energy Energy (kev) Au TEY Rel. Increase CsI TEY Rel. Increase Recessed Incidence Diameter Depth Geometry Angle (µm) (µm) 14 Cone 15 6 3 1.76 1.77 14 Pyramid 15 6 3 1.85 1.85 14 Cone 15 4 2 1.66 1.67 14 Pyramid 15 4 2 1.74 1.74 14 Cone 10 6 3 1.88 1.87 14 Pyramid 10 6 3 2.12 2.11 14 Cone 10 4 2 1.77 1.76 14 Pyramid 10 4 2 1.97 1.97 d Temporal spread from 6x3 µm geometry ~1 ps Temporal spread from 6x11 µm geometry ~100 ps Full cone geometry yield increase ~4 x Standard emission surface area Enhanced emission surface area Projected enhanced surface area

Spatial resolution shows a dependence on cathode type

Field Gradient Simulation Results Planar photocathode Pillar Cone (15 degree wall angle) Recessed pillar Recessed cone (15 degree wall angle)

High Energy Cathode Design Flat Photocathode Field Gradient Model Flat photocathode geometry is currently used in NIF streak camera detectors and in the DIXIE detector

High Energy Cathode Design Pillar Structures Field Gradient Model Field emission at the pillar edges is seen

High Energy Cathode Design Pillar Cavities Field Gradient Model Field emission is suppressed field present within the structure

High Energy Cathode Design Cone Pillar Structures Field Gradient Model Field emission at the pillar edges is seen

Reflectivity Reflectivity 1.2 1 0.8 Reflectivity 0.6 0.4 0.2 0-0.2 0 0.5 1 1.5 2 2.5 3 3.5 4 Angle of Incidence (theta) Reflectivity 6397 ev Reflectivity 1000eV Reflectivity 500 ev Reflectivity 9886 ev Reflectivity 14165 ev

Fresnel Equations Treat x-ray interaction as a boundary-value problem for reflection and refraction of a plane electromagnetic wave at an absorbing medium. The reflection coefficient I/I 0 if electric vector is perpendicular to the plane of incidence: The reflection coefficient I/I 0 if two states of incident beam polarization: The reflection coefficient I/I 0 for an un-polarized incident beam: φ is the angle of incidence, γγ is the characteristic materials constant, a is the characteristic function a

Linear absorption coefficient The linear absorption coefficient is given by: II = II 0 ee ααtt Where is the sample thickness.

Pillar Samples Available at LLNL 1cm x 1cm Substrate thickness is 215 µm, pillars 25 µm 2 µm diameter and 2 µm separation Structure similar to the high density model DBA6-33 after 1 minute Si wet etch stirred Coated with 30 Angstroms of Cr and 1000A of Au Pillar Samples to Kathy Opachich (NIF) Feb. 4, 2011 POC, R. Nikolic, 3-7389

High Energy Cathode Design Pillar Geometry Results Pillar spacing either reduced the field between pillars to zero, or increase the field at the pillar tips to cause field emission.

High Energy Cathode Design Pillar Geometry Results Reducing the Pillar height did not increase the field gradient within the structure

Fraser s Model: used to identify incidence angle (1-30 kev) The total electron yield is determined by considering: The probability of an x-ray photon being absorbed in layer z+dz The number of electrons generated within a thin layer z+dz in the cathode The probability of the secondary electron escaping to the surface R(α) is the Fresnel reflectivity P s (0) is the secondary electron escape probability (~0.2 ) E x is the x-ray energy Γ 0 beam intensity photons/cm 2 /s ε is the energy required to promote a secondary electron from the valence band with sufficient energy to escape into vacuum (7eV) T is the cathode thickness (1000 Angstroms) µ is the linear absorption coefficient α is the x-ray incidence angle α is the angle of the refracted x-ray f(z) is the fraction of x-ray energy available for generation of secondary electrons Ls is the secondary electron escape length (215 Angstroms for CsI)

Fraser s Model: used to identify incidence angle (1-30 kev) The secondary photocurrent (X c ) s is then: (1) Where: Assigning conversion efficiency a value independent of depth below cathode surface (f=1) gives: Y(T) is relative yield versusthickness function: R(α) is the Fresnel reflectivity P s (0) is the secondary electron escape probability (~0.2 ) E x is the x-ray energy ε is the energy required to promote a secondary electron from the valence band with sufficient energy to escape into vacuum (7eV) T is the cathode thickness (1000 Angstroms) µ is the linear absorption coefficient α is the x-ray incidence angle α is the angle of the refracted x-ray f(y) is the fraction of x-ray energy available for generation of secondary electrons Ls is the secondary electron escape length (215 Angstroms)

Incidence Angle Definition and Yield Secondary e- Primary e- z=0 z=t α angle of refraction α angle of incidence 1000Å of CsI Does changing the incidence, and thus increasing the x-ray path-length, improve yield in reflection and transmission modes?

The angular distribution at the mesh was predicted using CST