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Baked Alaska

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BJORKEN, J.↗

IOTA Pre-Bake Test Development

The IOTA (Integrable Optics Test Accelerator) Bakeout project is intended to improve the quality of the vacuum within the IOTA ring. Impurities consisting of hydrogen and oxygen that build within the beampipe are reduced through applying heat to the beampipe’s exterior. Two versions of the Bakeout project exist, one as a smaller scale test setup, and one five times larger located within the IOTA ring. During my internship, I worked together with a team to bring this project from an effectively dormant state to ready for testing, working together to create full documentation of the PLC (Programmable Logic Controller) programs, making multiple new hardware configurations of this test possible, as well as an additional safety system.

Seagrave, Kayla [DuPage Coll.; Fermilab]↗

Enhancing the performance of solvent-borne poly(ethyl methacrylate) coatings for high-power laser applications via low-temperature drying

Organic polymers are a versatile class of materials employed in a broad range of optical coating applications. However, their use as coatings in high-power laser applications, particularly in the UV spectral region, has been limited in scope due to their relatively low laser-induced damage thresholds (LIDTs), which decrease further with exposure to multiple pulses. This study explores the effect of post-deposition drying temperature and residual solvent on the LIDT of solvent-borne polymer coatings. In this work, poly(ethyl methacrylate) (PEMA) coatings were deposited by first spin coating solutions of PEMA (dissolved in 2,2,2-trichloroethanol (TCE)) onto fused silica substrates, then baking at temperatures of either 130°C (soft-bake) or 180°C (hard-bake). Analysis of the two coatings revealed that the soft-bake coating retained a significant amount of TCE within the polymer matrix, which functioned to plasticize the coating and reduce internal stress. The laser-induced damage resistance of the two coatings was evaluated using 351-nm, 1-ns laser pulses. The testing protocols included single-pulse (1-on-1), 1-pulse ramp (R-on-1), and a 1000-pulse ramp (1000R-on-1) test. The results showed that the plasticized, soft-bake coating exhibits a significantly increased LIDT, especially for multipulse irradiation conditions.

36 MATERIALS SCIENCE↗

Aluminum and Other Coatings for the Passivation of Tritium Storage Vessels

Using a highly sensitive residual gas analyzer, the off-gassing of hydrogen, water, and hydrocarbons from surface-treated storage vessels containing deuterium was measured. The experimental storage vessels were compared to a low-off-gassing, electro-polished 304L canister. Alternative vessels were made out of aluminum, or were coatings on 304L steel. Coatings included powder pack aluminide, electro-plated aluminum, powder pack chromide, dense electro-plated chromium, copper plated, and copper plated with 25 and 50 percent nano-diamond. Vessels were loaded with low pressure deuterium to observe exchange with protium or hydrogen as observed with formation of HD and HDO. Off gas of D 2 O or possible CD 4 was observed at mass 20. The main off-gas in all of the studies was H 2 . The studies indicated that coatings required significant post-coating treatment to reduce off-gas and enhance the permeation barrier from gases likely added during the coating process. Dense packed aluminum coatings needed heating to drive off water. Electro-plated aluminum, chromium and copper coatings appeared to trap hydrogen from the plating process. Nano-diamond appeared to enhance the exchange rate with hydrogen off gas, and its coating process trapped significant amounts of hydrogen. Aluminum caused more protium exchange than chromium-treated surfaces. Aluminum coatings released more water, but pure aluminum vessels released small amounts of hydrogen, little water, and generally performed well. Chromium coating had residual hydrogen that was difficult to totally outgas but otherwise gave low residuals for water and hydrocarbons. Our studies indicated that simple coating of as received 304L metal will not adequately block hydrogen. The base vessel needs to be carefully out-gassed before applying a coating, and the coating process will likely add additional hydrogen that must be removed. Initial simple bake-out and leak checks up to 350° C for a few hours was found to be inadequate. All of the studies indicated that vessels needed several days of vacuum baking at 350-450° C to fully outgas the residual gases, which were mostly hydrogen. The current standard practice of out-gassing from ultra-clean, electro-polished 304L vessels with both vacuum bake-out and followed by an oxidative bake out to enhance the chromium surface performed the best in these studies.

08 HYDROGEN↗

Moisture Corrosion of LiH: A Kinetic Investigation by DRIFT Spectroscopy

Lithium hydride (LiH) is a unique, ionic compound with applications in a variety of industries. Unfortunately, LiH is very reactive toward H 2 O even at ppm levels, forming oxide (Li 2 O) and hydroxide (LiOH) corrosion layers while outgassing H 2 . An effective means to eliminate unwanted outgassing is vacuum-heating to convert LiOH into Li 2 O, although subsequent re-exposure to moisture during transport/handling reconverts some Li 2 O back to LiOH. A corrosion growth model for previously vacuum-baked LiH is necessary for long-term prediction of the hydrolysis of LiH. In this work, a para-linear hydroxide corrosion growth model is proposed for the reaction of previously vacuum-baked LiH samples with moisture. This model, composed of two competing diffusion reaction fronts at the LiOH/Li 2 O and Li 2 O/LiH interfaces, is validated experimentally by subjecting a previously vacuum-baked polycrystalline LiH sample to 35 ppm of H 2 O at room temperature while monitoring the corrosion growth as a function of time with diffuse-reflectance infrared Fourier transform (DRIFT) spectroscopy. The para-linear growth model for the hydrolysis of previously vacuum-baked LiH proposed in this report can also serve as a template for the hydrolysis of other hygroscopic oxides grown on metal or metal hydride substrates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The Kinetics of the Coherent Stage of Hydroxide Corrosion on Li 2 O-Covered LiH

The capability to model LiOH growth on vacuum-baked LiH is a necessary precursor to making kinetic predictions of undesirable hydrogen outgassing from corroded LiH materials when placed in sealed-system applications. Here, in this work, LiH samples with initial LiOH surface corrosion layers less than 1.1 μm were outgassed by vacuum baking at high temperature to convert LiOH to Li 2 O. Diffuse-reflectance infrared Fourier transform (DRIFT) spectroscopy was used to measure the subsequent LiOH regrowth during exposure to 25–375 ppm of H 2 O vapor at room temperature. Logarithmic kinetics best model the growth of this coherent hydroxide corrosion layer (up to 1.5 μm) on previously vacuum-baked LiH samples. The logarithmic kinetics are attributed to the dissociation of H 2 O on the corrosion layer and the establishment of a H + /OH – electric field across the thickening LiOH corrosion layer. A time-dependent model of LiOH corrosion growth as a function of both initial LiOH thickness before vacuum baking and moisture partial pressures during re-exposure was developed to help researchers better assess the unwanted hydrogen outgassing potential from LiH/LiD materials.

Matt, Sarah M. [Lawrence Livermore National Labora↗

Correlation of CsK{sub 2}Sb photocathode lifetime with antimony thickness

CsK{sub 2}Sb photocathodes with quantum efficiency on the order of 10% at 532 nm, and lifetime greater than 90 days at low voltage, were successfully manufactured via co-deposition of alkali species emanating from an effusion source. Photocathodes were characterized as a function of antimony layer thickness and alkali consumption, inside a vacuum chamber that was initially baked, but frequently vented without re-baking. Photocathode lifetime measured at low voltage is correlated with the antimony layer thickness. Photocathodes manufactured with comparatively thick antimony layers exhibited the best lifetime. We speculate that the antimony layer serves as a reservoir, or sponge, for the alkali.

36 MATERIALS SCIENCE↗

Hydride Bed Helium-3 Recovery and Partial Regeneration

Savannah River Tritium Enterprise has used LaNi 4.25 Al 0.75 (LANA75) hydride beds to store hydrogen isotopes for over two decades. A benefit of using LANA75 is that the 3He generated from tritium decay is retained in the hydride material, allowing the hydride beds to deliver high-purity product gas. A disadvantage is that the 3He accumulates in the LANA75 material over time, which forms a heel that cannot be removed under normal operating conditions. The heel traps hydrogen in the bed, slowly reducing the operational capacity of the bed as the heel grows. Eventually, the 3 He begins to release from the material, preventing the delivery of high-purity product. The hydride beds are replaced when (1) operational capacity is reduced such that it is impactive to routine operations, and/or (2) product purity is not maintained due to 3 He release.Several beds were operated beyond their design life. One of these beds was selected to undergo heating beyond its normal operating temperature to evaluate the possibility of removing a portion of the hydrogen and helium heel to improve bed function until a replacement could take place. This bake-out removed a portion of the hydrogen and helium heel, and preliminary data indicate that bake-outs may partially regenerate the beds. The bed’s performance will continue to be monitored, and additional bake-outs will likely be performed. Performing bake-outs results in increasing the recovery of 3 He, more efficient end-of-life activities (such as isotopic exchange), and extension of the useful service life of the bed.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Effect of Sb thickness on the performance of bialkali-antimonide photocathodes

The alkali species Cs and K were codeposited using an effusion source, onto relatively thick layers of Sb (50 nm to ∼7 μm) grown on GaAs and Ta substrates inside a vacuum chamber that was baked and not-vented, and also baked and vented with clean dry nitrogen but not rebaked. The characteristics of the Sb films, including sticking probability, surface roughness, grain size, and crystal properties were very different for these conditions, yet comparable values of photocathode yield [or quantum efficiency (QE)] at 284 V were obtained following codeposition of the alkali materials. Photocathodes manufactured with comparatively thick Sb layers exhibited the highest QE and the best 1/e lifetime. The authors speculate that the alkali codeposition enabled optimized stoichiometry for photocathodes manufactured using thick Sb layers, which could serve as a reservoir for the alkali materials.

42 ENGINEERING↗

Testing a GaAs cathode in SRF gun

RF electron guns with a strained superlattice GaAs cathode are expected to generate polarized electron beams of higher brightness and lower emittance than do DC guns, due to their higher field gradient at the cathode's surface and lower cathode temperature. We plan to install a bulk GaAs:Cs in a SRF gun to evaluate the performance of both the gun and the cathode in this environment. The status of this project is: In our 1.3 GHz 1/2 cell SRF gun, the vacuum can be maintained at nearly 10{sup -12} Torr because of cryo-pumping at 2K. With conventional activation of bulk GaAs, we obtained a QE of 10% at 532 nm, with lifetime of more than 3 days in the preparation chamber and have shown that it can survive in transport from the preparation chamber to the gun. The beam line has been assembled and we are exploring the best conditions for baking the cathode under vacuum. We report here the progress of our test of the GaAs cathode in the SRF gun. Future particle accelerators, such as eRHIC and the ILC require high-brightness, high-current polarized electrons. Strained superlattice GaAs:Cs has been shown to be an efficient cathode for producing polarized electrons. Activation of GaAs with Cs,O(F) lowers the electron affinity and makes it energetically possible for all the electrons, excited into the conduction band that drift or diffuse to the emission surface, to escape into the vacuum. Presently, all operating polarized electron sources, such as the CEBAF, are DC guns. In these devices, the excellent ultra-high vacuum extends the lifetime of the cathode. However, the low field gradient on the photocathode's emission surface of the DC guns limits the beam quality. The higher accelerating gradients, possible in the RF guns, generate a far better beam. Until recently, most RF guns operated at room temperature, limiting the vacuum to {approx}10{sup -9} Torr. This destroys the GaAs's NEA surface. The SRF guns combine the excellent vacuum conditions of DC guns and the high accelerating gradient of the RF guns, potentially offering a long lived cathode with very low emittance. Testing this concept requires preparation of the cathode, transportation to the SRF gun and evaluation of the performance of the cathode and the gun at cryogenic temperatures. In our work at BNL, we successfully activated the bulk GaAs in the preparation chamber. The highest quantum efficient was 10% at 532 nm that fell to 0.5% after 100 hours. We explored three different ways to activate the GaAs. We verified that the GaAs photocathode remains stable for 30 hours in a 10{sup -11} Torr vacuum. Passing the photocathode through the low 10{sup -9} Torr transfer section in several seconds caused the QE to drop to 0.8%. The photocathode with 0.8% QE can be tested for the SRF gun. The gun and beam pipe were prepared and assembled. After baking at 200 C baking, the vacuum of the gun and beam pipe can sustain a low 10{sup -11} Torr at room temperature. The final test to extract electrons from the gun is ongoing. In this paper, we discuss our progress with this SRF gun and the results of the photocathode in preparation chamber and in magnet transfer line.

43 PARTICLE ACCELERATORS↗

An in situ annealing route to [Bi6O6(OH)2](NO3)4·2H2O/g-C3N4 heterojunction and its visible-light-driven photocatalytic performance

Highlights: • The heterojunction (BBN-g-C{sub 3}N{sub 4}) was synthesized by in situ calcination route. • The baked Bi(NO{sub 3}){sub 3}·5H{sub 2}O as raw material is crucial to obtain highly crystalline BBN-g-C{sub 3}N{sub 4}. • BBN-g-C{sub 3}N{sub 4} exhibited better visible-light-driven photocatalytic activity than Bi{sub 2}O{sub 3}-g-C{sub 3}N{sub 4}. • BBN-g-C{sub 3}N{sub 4} prepared by calcining route possessed better photocatalytic activity than by mechanical mixing method. - Abstract: Known as incomplete hydrolysis products of Bi(NO{sub 3}){sub 3}·5H{sub 2}O, basic bismuth nitrates (BBN), were commonly obtained via a solution route. Herein, BBN-CN ([Bi{sub 6}O{sub 6}(OH){sub 2}](NO{sub 3}){sub 4}·2H{sub 2}O/g-C{sub 3}N{sub 4}) and Bi{sub 2}O{sub 3}-g-C{sub 3}N{sub 4} heterojunctions were prepared in situ by mixing g-C{sub 3}N{sub 4} with baked Bi(NO{sub 3}){sub 3}·5H{sub 2}O and subsequent calcining at 250 °C and 550 °C, respectively. The baked Bi(NO{sub 3}){sub 3}·5H{sub 2}O as a bismuth source was crucial to the formation of highly crystalline BBN, and otherwise, the product was poor-crystalline and low photoactive. The as-prepared BBN-CN exhibited better photocatalytic activity for rhodamine B (RhB) degradation under visible light irradiation than BBN, g-C{sub 3}N{sub 4}, and Bi{sub 2}O{sub 3}-g-C{sub 3}N{sub 4}, although Bi{sub 2}O{sub 3} is more visible-light-active. These could be attributed to higher surface areas and more negative conduction band potentials of BBN, which benefits for capturing the photogenerated electrons to form active O{sub 2}{sup −} radicals. Furthermore, the presence of g-C{sub 3}N{sub 4} plays a crucial role in enlarging visible light response.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Characterization of a linear device developed for research on advanced plasma imaging and dynamics

Within the scope of long term research on imaging diagnostics for steady-state plasmas and understanding of edge plasma physics through diagnostics with conventional spectroscopic methods, we have constructed a linear electron cyclotron resonance (ECR) plasma device named Research on Advanced Plasma Imaging and Dynamics (RAPID). It has a variety of axial magnetic field profiles provided by eight water-cooled magnetic coils and two dc power supplies. The positions of the magnetic coils are freely adjustable along the axial direction and the power supplies can be operated with many combinations of electrical wiring to the coils. Here, a 6 kW 2.45 GHz magnetron is used to produce steady-state hydrogen, helium, and argon plasmas with central magnetic fields of 875 and/or 437.5 G (second harmonic). In order to achieve the highest possible plasma performance within the limited input parameters, wall conditioning experiments were carried out. Chamber bake-out was achieved with heating coils that were wound covering the vessel, and long-pulse electron cyclotron heating discharge cleaning was also followed after 4 days of bake-out. A uniform bake-out temperature (150 deg. C) was achieved by wrapping the vessel in high temperature thermal insulation textile and by controlling the heating coil current using a digital control system. The partial pressure changes were observed using a residual gas analyzer, and a total system pressure of 5x10{sup -8} Torr was finally reached. Diagnostic systems including a millimeter-wave interferometer, a high resolution survey spectrometer, a Langmuir probe, and an ultrasoft x-ray detector were used to provide the evidence that the plasma performance was improved as we desired. In this work, we present characterization of the RAPID device for various system conditions and configurations.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗