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 1, P. Ross 1, J. Koch 1, A. MacPhee 2, O. Landen 2, D. Bradley 2, P. Bell 2, S. Nagel 2, T. Hilsabeck 4, N. Chen 5, S. Udin 5, A. Gopal 5, J. Feng 3 1 National Security Technologies, LLC 2 Lawrence Livermore National Laboratory 3 Lawrence Berkeley National Laboratory 4 General Atomics 5 NanoShift, LLC October 7, 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/2594--2631.

Outline Overview Motivation for the project. Yield enhancement at grazing incidence. Utilization of 3-D structures. Photocathode Design and Fabrication Details Photocathode design considerations and requirements for X-ray imagers. Recessed cavity design and expected yield. Fabrication details and results. Recent measurements show an increase in yield Project Accomplishments Future work

Future diagnostics will need a high QE photocathode in the 10 50 kev range X-Ray signal 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. New imaging sources will be generating X-ray photons at energies >10 kev, maybe a potential complication for current detectors.

A drop in sensitivity is seen above 10 kev for most cathode materials 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. Yield can be increased by going to the grazing incidence geometry.

Matching the X-ray path length to the escape depth at grazing incidence increases the electron yield e- e- e- 10 Å escape depth Not detected e- X 10 Å escape depth 700Å e- We measure yield generated within ~20 Å of the surface (photoelectron escape depth limited ) e- 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 Recessed Cavity Design 1 kev x-ray energy 1000 Å CsI cathode Si X-Ray signal From: D. Lowney, Proc. SPIE 5194 (2004) 139. Recessed cavity structures utilize this effect to improve yield.

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. <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. Last year we showed that the recessed structures satisfy these requirements.

Total yield enhancement expected to be 1.2-3 times at 10 kev Energy (kev) Recessed Geometry Incidence Angle Diameter (µm) Depth (µm) Δt (psec) Au Rel. Increase 10 Cone 10-15 9 3 1 1.6 10 Cone 10-15 9 8.4 ~10 2.36 10 Cone 10-15 9 16.8 ~200 2.81 Full Depth Shallow Depth Si Si 9 µm diameter chosen for ease of fabrication 10-15 degree wall angle chosen to increase enhanced surface area

Prototype requirements were based on recessed cavity modeling results Full Depth Shallow Depth Si Si 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 recipe developed by NanoShift, LLC includes 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 91.37 nm 91.61 nm 112.7 nm Prototypes with all 3 depths were received at the end of FY 15.

Recent measurements show an enhancement in yield of up to 2.7 times. Relative yield increase: 2.7 times for full depth (16µm) 2.3 times for mid depth (8 µm) 1.3 times for shallow (4 µm)

Yield as a function of incidence angle shows structure is symmetric and introduces an increase in yield at 0 Expected current from a flat surface

Project accomplishments Photocathode Model and Computer Simulation Used Fraser s model to predict yield for CsI and Au in the 10-50 kev Range. (FY 14) Built a CST Studio Suite model to test structured cathode designs. Predicts field strength, spatial resolution and temporal resolution. (FY 14) Device Fabrication and Testing First set of prototypes built in FY 15. Device performance characterized at a synchrotron facility in FY 15. Devices show clear evidence of yield improvement.

Further work Prototype performance characterization Finish analysis of yield data collected in the 4-12 kev range. Collect SEM and optical images of the prototype samples. Full scale development and testing Develop a full scale 5 x 31 mm photocathode for DISC. Fabricate prototypes with 6 and 3 degree wall angles and with varied Au thickness for high energy testing. Test in a calibrated DISC detector for full performance characterization. New designs Continue to explore novel structures and materials.

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.

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

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 4x10 6 V/m 2x10 6 V/m 0 V/m Field emission is suppressed and field is present within the cavity.

Spatial resolution element is limited by the emission from the structure walls and cavity diameter Cathode diameter and wall angle can be changed to satisfy requirements.

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 High Energy Cathode Development: October 7, 2015 Reflectivity Reflectivity 1.2 1 0.8 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, γ is the characteristic materials constant, a is the characteristic function a

Linear absorption coefficient The linear absorption coefficient is given by: I = I 0 e αt 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