Hayabusa2 sample recovery and transportation to the Curation Facility without leaking.
On 5 December 2020 ,the reentry capsule was released from the spacecraft and enter the Earth’s atmosphere on 6 December 2020 , after a successful returning cruise from Ryugu to the Earth. The reentry capsule retrieval operation was carried out complying strictly to the Australian COVID-19 regulations. The landing area of the capsule was determined by receiving a beacon signal transmitted from the capsule using five antennas installed at different locations. The Marine radar systems and two Drones were also used for this retrieval operation of the capsule, the heat shields, and the parachute. The reentry capsule was located nearby the parachute, which was found from the helicopter observation. The safety check of the capsule was first completed at the landing location because pyrotechnic devices were used for the parachute deployment and separation. No damage to the capsule was observed, and the capsule was transported back to a Quick Look Facility (QLF) prepared in the Woomera Prohibited Area (WPA) with a permission from the Australian safety officer.
The reentry capsule was recovered from the landing site in the WPA, South Australia five hours after its landing, and transported to the QLF. The capsule was introduced into the clean booth in the QLF and the sample container was extracted from the capsule and cleaned on its outer surface after the safety check. The temperature monitor attached to the sample container indicated that the container was never heated up to 65°C.
The container was installed on the Hayabusa2 GAs Extraction and Analysis system (GAEA). After the overnight evacuation of the vacuum line of GAEA, on Dec. 7, the bottom of the sample was pierced with a tungsten carbide needle to release sample volatile components held inside the sample container22. The container was in vacuum, indicating the container seal held during reentry and therefore low terrestrial contamination. The gas extracted from the sample container was split into four gas tanks at room temperature, and the residual gas in the system was then trapped into two gas tanks cooled at liquid nitrogen temperature. A fraction of the gas was analyzed by a quadrupole mass spectrometer (WATMASS, Tokyo Electronics). The sample container was put into a nitrogen-purged anti-vibration transportation box and was safely transported to Extraterrestrial Sample Curation Center (ESCuC) in the Sagamihara Campus of JAXA on 8 December 2021 (~57 hours after the capsule landing). Then a heat shield made of carbon reinforced plastic was removed from an outer lid of the container after drilling work with a milling machine to expose head of bolts and remove them. The Hayabusa2 sample container was sealed with the metal-to-metal sealing system21,22. The container lid was pressed against the container edge with a pressure load of ~2700 N through pressure springs. To open the container in the clean chamber designed for Ryugu samples in vacuum, the container was installed into the container opening system. The pressure springs and the outer lid with latches were then taken apart from the container while keeping the pressure load constant. The container with the opening system was the attached to the clean chamber, designed to maintain the Ryugu samples in vacuum, on Dec. 11 (132 hours after its Earth landing) and was opened on Dec. 14 after the chamber evacuation.
As outer surface of the container was cleaned, the outer lid was firstly anchored to access to an inner lid, then the inner lid was anchored with rods to remove the outer lid and a frame for latches. Finally, the inner lid was anchored with the container opening system.
The Curation Facility for Hayabusa2 and its cleanliness control.
The concept of Hayabusa2 curation is to treat the returned samples for the initial description in the non-destructive manner and the delivery for further detailed investigations without any contamination of terrestrial materials and exposure to the terrestrial atmosphere. Therefore, the curation facility is equipped in the ISO 6 or Class 1000 clean room (1000 dust particles of ≥ 0.5µm in diameter in cubic feet)40. The clean chambers (CCs) for Hayabusa2-returned samples are prepared for handling samples under vacuum or ultra-purified nitrogen atmosphere without exposing to terrestrial atmosphere41. They are composed of five independent chamber; CC3-1 for opening the container in vacuum, CC3-2 for opening the chamber A of the catcher and remove a few particles from the chamber in vacuum, CC3-3 for exchanging environment from vacuum to purified nitrogen, CC4-1 for dismantling the catcher to extract the samples from each chamber, and CC4-2 for observation and weighing the samples. All the sample holders, pick-up devices, sample holders, and other jigs and tools used in the clean chambers are specially cleaned to avoid contaminations and their materials are highly limited to minimize the effect of chemical reactions with the samples42.
Pick-ups of the Hayabusa2 samples from the container
As the sample container opening system was connected to the CC3-1 with dry air purged condition, the chamber was evacuated to reach high vacuum as 10-6 Pa. Then the chamber was in static vacuum condition to open the inner lid of the container. Soon after opening the container, the chamber was evacuated again. The sample catcher which is combined with the inner lid was extracted from the container and bottom of the container was left behind the chamber. Then the catcher was turned upside down to make the cover of Chamber A of the catcher face upward, and it was transported from the CC3-1 to the CC3-2 and a gate valve between them was closed. In the CC3-2 of vacuum condition, the surface of the cover of the Chamber A was firstly cleaned with a Teflon spatula. Then all the screw bolts of the cover were unscrewed and the cover was removed with an electrostatic chuck to expose samples inside the Chamber A of the catcher. A large numbers of black particles of > mm size were observed inside the Chamber A.
A few particles of mm-size were removed from the chamber with a sample handling tool equipped with the CC3-2 and put into a quartz glass dish. A cover made of quartz glass was attached on the opening of the Chamber A of the catcher, and the catcher was transported from the CC3-2 to the CC3-3 and the gate valve between them was closed. The CC3-1 and CC3-2 continue being evacuated after that. The CC3-3 was slowly purged with purified nitrogen to reach atmospheric pressure. After that, the catcher was handled with tools and jigs manipulated with Viton-coated butyl gloves equipped in the CC3-3, CC4-1 and CC4-2. Firstly, a jig for handling was attached to the catcher and the screw bolts to connect the catcher with the inner lid were removed to separate the catcher from the lid.
Then the catcher was transported to CC4-2 through CC4-1 to measure its weight with a balance equipped in the CC4-2. Based on the design weight of the catcher and a tare weight of the attached jig, the total weight of samples inside the catcher is calculated to be 5.424 ± 0.217 grams. The balance used for weighing is Mettler-Toledo XP404s, modified on its outer cover from its original to that made of stainless steel 304 sealed with Viton and on its power and signal cables from its originals to those coated by Teflon tubes.
An optical microscope Nikon SMZ1270i with XYZ electric motors system is equipped above the CC4-2, and black particles inside the chamber A of the Catcher was photographed with the microscope. And then the catcher was transported to the CC4-1 and it was dismantled with tools and jigs to extract samples from each of the Chambers (A, B and C) to containers made of sapphire glass, set underneath funnels made of stainless steel 304. After several large particles were handpicked directly from the opening of the funnels with a vacuum tweezer, samples from the Chamber A and C were divided from the funnels into three sapphire containers with a spatula made of stainless steel. Samples inside the Chamber B, which was exposed to the sampler horn after the TD1 and before the TD2, were also recovered into a sapphire container, which are only a small amount of powders of 13 ± 0.5 mg, indicating only a limited amount of samples should be mixed up between three Chambers. The samples in the sapphire containers were measured their weights and spectral characters with the balance, an FT-IR, a MicrOmega and a visible spectrometer. Then particles of >1mm in size in the container were handpicked one by one with a vacuum tweezer having a nozzle made of stainless steel 304 into a sapphire dish for individual particles to be photographed, weighed, and measured with FT-IR and MicrOmega.
These obtained data are catalogued for further detailed researches that starts in summer 2021. Further, the sample will be open to the community and distributed through the Hayabusa2 Sample Allocation Committee in summer 2022.
Outline of measurements for sample description
Multiband optical images of Ryugu samples were taken using a nadir-viewing a nadir-viewing camera system with a macro lens and a CMOS detector covering from 0.48 - 0.86 µm with illumination at 30° from the nadir. In order to obtain high-resolution (~5 µm/pix) images, we used a nadir-viewing Nikon microscope with the same illumination angle. We used 5 filters (b: 0.48µm, v: 0.55 µm, Na: 0.59 µm, w: 0.70 µm, x: 0.86µm) compatible with the optical navigation camera telescope ONC-T of Hayabusa23,20 to the illumination for macro lens measurements and 4 filters (b, v, Na, and w) for microscope measurements.
Spectroscopy of Ryugu samples
The FT-IR used for this study is JASCO VIR-300, equipped to the CC4-2. Its can measure infrared spectrum from 1.0 µm to 4.0 µm in wavelength. Its minimum beam spot in focus position sizes 1 mm, and a nominal beam spot for bulk sample measurement sizes 2 mm. Incident beam comes through a sapphire viewport to illuminate samples inside an FT-IR chamber attached to the CC4-2 of purified nitrogen condition. Before and after the sample measurement, Both its incident and emission angles of infrared light are designed as 16 degree, thus phase angle for the samples is 32 degree. The NIRS3 spectrum was created by averaging 128 spectra acquired on May 15, 2019 (see the Extended Data Table 2 of Kitazato et al. (2021)43 for details). Its reflectance values have been corrected to the same viewing geometry (incidence = 16˚, emission = 16˚, phase = 32˚) using the latest photometric model44. Error bars are 1-sigma. The instrument which includes incident and reflected light paths is purged with nitrogen to decrease influences of absorption of atmospheric molecules like H2O and CO2. Infragold is measured before sample measurement for compensation of the background.
The detailed method about MicrOmega is detailed in another paper31. MicrOmega is mounted on the dedicated chamber attached to CC3-3. The samples are on the XYZ and rotation position changeable stage within the cleaned conditions, and observed with the MicrOmega through the sapphire window.
Density determination of Ryugu samples
The sizes of Ryugu particles are measured from their optical microscope images taken after their separation into individual containers. Note that separation of particles with the tweezer was made by curatorial members of the ESCuC, which might possibly cause a sampling bias. Major and minor diameters are calculated based on eclipses circumscribed to the binarized images of particles, and averages of the major and minor diameters are used as the size of the particles, Dp. A cumulative number of particles to their average diameters is plotted as Fig. 1, and a power index fitting to the distribution is calculated by maximum-likelihood fitting methods with goodness-of-fit tests based on the Kolmogorov–Smirnov statistic45,46. The volume of Ryugu particles is calculated as a following formula based on the reference47;
The densities of particles are calculated from the volumes calculated with the formula and weights measured with the balance in CC4-2 (Fig. 2). Typical errors of the densities range from 0.03 to 0.50 g/cm3.