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A Hydrogen Leak-Tight, Transparent Cryogenic Sample Container for Ultracold-Neutron Transmission Measurements

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A Hydrogen Leak-Tight, Transparent Cryogenic Sample Container for Ultracold-Neutron Transmission Measurements A hydrogen leak-tight, transparent cryogenic sample container for ultracold-neutron transmission measurements Stefan Döge1, 2, 3, ∗ and Jürgen Hingerl1, 2 1Institut Laue–Langevin, 71 avenue des Martyrs, F-38042 Grenoble Cedex 9, France 2Physik-Department, Technische Universität München, D-85748 Garching, Germany 3École Doctorale de Physique, Université Grenoble Alpes, F-38402 Saint-Martin-d’Hères, France The improvement of the number of extractable ultracold neutrons (UCNs) from converters based on solid deuterium (sD2) crystals requires a good understanding of UCN transport and how the crystal’s morphology influences its transparency to UCNs. Measurements of the UCN transmission through cryogenic liquids and solids of interest, such as hydrogen (H2) and deuterium (D2), require sample containers with thin, highly polished and optically transparent windows and a well defined sample thickness. One of the most difficult sealing problems is that of light gases like hydrogen and helium at low temperatures against a high vacuum. Here we report on the design of a sample container with two 1 mm thin amorphous silica windows cold-welded to aluminum clamps using indium wire gaskets, in order to form a simple, reusable and hydrogen-tight cryogenic seal. The container meets the above-mentioned requirements and withstands up to 2 bar hydrogen gas pressure against isolation vacuum in the range of 10−5 to 10−7 mbar at temperatures down to 4.5 K. Additionally, photographs of the crystallization process are shown and discussed. Published as: Review of Scientific Instruments 89, 033903 on 6 March 2018 https://doi.org/10.1063/1.4996296. I. INTRODUCTION II. THE NEED FOR AN IMPROVED SAMPLE CONTAINER If one wants to measure the transmission of ultracold The scattering of thermal and cold neutrons from cryo- neutrons through a cryogenic liquid or solid, the windows genic liquids and solids is a well established experimental of the sample container need to be as highly polished as technique. Most of the time, sample containers and their possible (center-line average roughness Ra < 10 Å) in or- neutron beam windows are machined from aluminum der to minimize undesired scattering from surfaces. Ma- alloy, because of its favorable post-irradiation behavior chined, rough-surface aluminum windows are fairly easy (short half-life of 2.5 min of the 28Al isotope, which is to make and have been used in UCN transmission ex- created by 27Al capturing a neutron), low neutron scat- periments before8–11. As our tests with single-side pol- tering and absorption cross section, and easy workabil- ished aluminum windows and unpolished as well as pol- ity. Thermal and cold neutrons have wavelengths of 1 to ished aluminum foils (Ra in the range of a few µm) have 10 Ångström and are therefore practically insensitive to shown, they are not suitable for UCN transmission ex- the aluminum’s neutron-optical potential, material inho- periments because of significant UCN scattering from the mogeneities and surface roughness. vacuum–aluminum and aluminum–sample interfaces due to surface roughness. Slow neutrons – especially ultracold neutrons (UCNs), In addition, thin aluminum windows in the range of with a velocity of only a few meters per second and a 0.15 to 0.3 mm tend to bulge at a pressure difference of wavelength of several hundred Ångström – are, however, about one bar. This results in a poorly defined sample 1 2,3 sensitive to surface roughness , material and magnetic thickness, which translates directly to a large error in the 4 inhomogeneities . Besides that, aluminum windows are scattering cross section. Atchison et al.8,9 used an initial not optically transparent and thus do not allow for an on- sample thickness of 10.0 mm. However, after bulging of line control of the sample. In UCN applications, the ad- the windows, computer simulations suggested an “effec- vantage of the low neutron-optical potential of aluminum tive thickness” of 11.1 mm. Considering the relation of arXiv:1803.10159v2 [physics.ins-det] 12 Jan 2021 (54 neV) is more than offset by the drawbacks that the sample thickness d and the total cross section σtot in the use of this material entails. transmission equation (eq. 1, where I0 is the transmit- ted UCN flux through an empty sample container, and In this article, we present an improved sample con- I(d) is the transmitted UCN flux through a sample of tainer design which addresses the issues of previous sam- thickness d, Nv is the molecular number density of the ple containers and permits reliable UCN transmission sample), one immediately understands the importance of measurements on cryogenic crystals, such as solid deu- a well defined sample thickness. terium (sD2). Measurements of this kind are needed to interpret the performance of operating sD2-based UCN I(d) −N σ d 5–7 = e v tot (1) sources worldwide . I0 2 Besides exhibiting a low surface roughness, sample con- Since the aforementioned suitable materials are com- tainer windows for UCN transmission experiments should monly supplied as flat wafers and it is very difficult to be made from a material with low absorption cross sec- make them into one-piece structures (like a flat window tion to maximize the neutron flux to the sample, and with plus clamp with screw holes) that would fit into our sam- a low neutron-optical potential12,13 to transmit UCNs ple container11, we had to develop a hydrogen-tight seal with an as low as possible energy. All materials are prac- to join the flat wafers and the clamps made from alu- tically impervious to UCNs with a kinetic energy below minum alloy AlMg3 (AA5754). their respective neutron-optical potential. Materials of choice are thus silicon, transparent vitreous silica and synthetic quartz (SiO2; naming convention suggested by III. DESIGN REQUIREMENTS OF THE Laufer14 to clarify the naming variations of quartz15), SAMPLE CONTAINER AND OPTICAL ACCESS and sapphire (Al2O3). The latter three are optically transparent and allow for an observation of the condensa- A thick and therefore mechanically strong glass slab or tion and crystal growth processes in the sample container collar does not present an obstacle in optical applications. along the neutron beam axis. Amorphous silica has the By contrast, in our case the glass windows need to be as unique advantage of not producing small-angle scatter- thin as possible to minimize the absorption of UCNs. 16 ing inside the material . In our sample containers we First we tried 0.5 mm thick vitreous silica windows in used transparent vitreous silica wafers purchased from our sample container, but they imploded in a vacuum Plan Optik AG, Elsoff, Germany. All of the following test at about 800 mbar pressure difference. Same-size reported results were obtained using sample containers windows, but with a thickness of 1.0 mm, withstood a with these wafers. pressure difference of 1 bar and more, and thus became The fact that the surfaces of the silica windows have a our window material of choice. negligible influence on the measured UCN transmission In brief, the design requirements were: is demonstrated by the virtually identical transmissivity through one d = 1.0 mm window and two d = 0.525 mm • highly polished and thin windows (d = 1 mm), the windows (see Fig. 1). If the surfaces had a large im- windows need to be easily removable pact, four vacuum–silica interfaces would transmit sub- • optically transparent windows with a low neutron- stantially less UCNs than two such interfaces. The calcu- optical potential and of high purity (no scattering lated neutron-optical potential12,13,17 of our amorphous length density inhomogeneities in the material) silica windows based on the volumetric mass density pro- 3 vided by the manufacturer (ρ = 2.203 g/cm ), is 90.6 neV • vacuum seal needs to be easily demountable and at room temperature and the same at cryo-temperatures hydrogen-tight down to 4.5 K due to a volume contraction of less than one per mille. • sample thickness needs to be well defined, the same 1 . 0 across the entire sample area, and adjustable over 0 . 9 a wide range within the same sample container 0 . 8 • sample container needs to withstand 2 bar hydro- gen pressure against high vacuum with a maximum n 0 . 7 −3 o i pressure of 10 mbar, preferably in the range of s s 0 . 6 −5 −7 i 10 to 10 mbar, in order for the closed-cycle re- m s 0 . 5 frigerator to work smoothly and to minimize UCN n a r t up-scattering on residual gas molecules. 0 . 4 e v i t 1 x 0 . 5 2 5 m m a m S i O a 2 The foot of the sample container was designed to be l 0 . 3 e 1 x 1 . 0 m m a m S i O R 2 mounted onto the two-stage cold-head of the cryostat 0 . 2 11 2 x 0 . 5 2 5 m m a m S i O 2 described in Döge et al. with a number of modifica- 2 x 1 . 0 m m a m S i O 0 . 1 2 tions: The stainless steel neutron guides facing directly 0 . 0 the sample container were removed. An illumination unit 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 with nine white LEDs was mounted on one side of the N e u t r o n v e l o c i t y i n m e d i u m [ m / s ] sample container (see Fig. 2). The LED support had a recess for a 50.8 mm double-side polished undoped sil- FIG.
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