12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Thermophyical property measurement results of ultra-high melting temperature oxides using
Electrostatic Levitation Furnace (ELF) onboard ISS-KIBO
Hideki SARUWATARI,1) Takehiko ISHIKAWA,2) Haruka TAMARU,1) Chihiro KOYAMA,1)
Masato OHSHIO,1) Hirohisa ODA,1) and Yasuhiro NAKAMURA1)
1) Human Spaceflight Technology Directorate, JAXA, Tsukuba, Japan 2) Institute of Space and Astronautical Science, JAXA, Tsukuba, Japan
12th Asian Microgravity Symposium - 201812 - 16 November, 2018
Zhuhai, China
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Levitation = Containerless technique
Its advantages : – High temperature liquid, with a melting temperature
higher than 2,000 deg. C, can be handled without contamination. Handling without contamination enables accurate measurements of thermophysical properties.
– The lack of a crucible enables larger degree of undercooling and increases the possibility of producing new functional materials such as glasses or to access metastable states of matter.
22
Melt
Container ContainerlessContainer
Nucleation
Melt
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Molten density (ρ), surface tension (γ), viscosity (η)
Industrial crystals or glasses are manufactured from high temperature melts.
Accurate thermophysical properties of melts are required for the material processing and structural analysis of melts.
Structure of melt
Takeda et al. Jap. Assoc. Cryst. Growth, 20 (1993) 27
Material processing
V.V. Kalaev et al. J. Cryst Growth, 250
(2003) 203.
Ex.) Si: 1687 K, Fe: 1811 K, SiO2: 1923 K, YAG: 2213 K, Al2O3: 2345 K,Lanthanoid oxides : over 2500 K
Melting temperature (Tm) of industrial material
33
Casting, Wilding, Thermal spraying and so on…
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
New functional materials processed by levitation technique
4
0
50000
100000
150000
0 50 100 150 200 250 300
1k Hz10k Hz100k Hz
Temperature (K)
ε
(c)BTO-C
0
2000
4000
6000 1 kHz10k Hz100 kHz
(a)BTO-A
ε
The dielectric constant is 30 times more than conventional dielectrics -> Ultra-compact capacitor
by TDK Corporation
70 60 50 40 30 20 101.4
1.6
1.8
2.0
2.2
2.4
n d
ν
Creation of high refractive-index glass(Highest refractive index of 2.4)-> Ball lens for high-density DVD
by Nippon Sheet Glass Co., Ltd.
JAXA Glass (●)
Commercial glass (●)<SiO2, etc. >
Refr
activ
e in
dex
Abbe's number
2 mm
Single crystal with hexagonal crystal system (high-temperature phase)
<BaTi2O5>
BaTiO3 capacitor commonly usedBaTiO3 capacitor manufactured by ELF
Die
lect
ric c
onst
ant
(Per
form
ance
of c
apac
itor)
0 300Temperature (K)
J. Yu, P.-F. Paradis, T. Ishikawa, and S. Yoda, “Huge Dielectric Constant of Transparent Hexagonal BaTiO3 Obtained by Containerless Processing” Ferroelectrics, 301(2004), 199–201.
A. Masuno, J. Yu, J. Jpn Soc. Microgravity Appl. 26 (2009),134
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Levitation techniques
5
Only the electrostatic levitation under the micro gravity environment can levitate and melt ultra-high temperature oxides.
Electrostatic levitation on the ground (in vacuum)
Aerodynamic levitationElectromagnetic levitation
Can not observe whole imageLarge temperature gradient Only conductorEasy evaporation
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Electrostatic Levitation Method
6
• Developed by W.-K. Rhim @JPL.• Use Coulomb force between charged sample and electrodes.• Need High speed feed back for
position control.• Less disturbances
Rhim et al., Rev. Sci. Instrum., 64 (1993),2961.
[1] Ishikawa et al., J. Jpn Soc. Microgravity Appl., 18 (2001),106
Type Voltage (Electric discharge)
Atmosphere(Evaporation)
sample
On the ground [1] High (8kVcm-1<)(occur)
Vacuum (difficult to control) Metals and few oxides
On ISS low (<3kVcm-1)(does not occur)
Pressurized gas or vacuum(easy to control)
Metal, alloy, and oxides
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Electrostatic levitation furnace in the International Space Station (ISS-ELF)
7
©NASA/JAXA
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
binary oxides
Mel
ting
tem
pera
ture
Mission Objectives of the ISS-ELF
8
1. Measure thermophysical properties of molten oxides whose Tm is over 2000 K.
• The database of thermophysical properties will be open to the public.
• Alloy is also available.
rare earth oxides
2. Search for Novel materials• samples return to Earth by
solidification from undercooling.• Analysis about solid state properties• Consider the possibility of industrial
applications
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Melt by Heating Laser
Camera etc.
sampleCharged by UV Lamp
• Sample size : about 1.5-2.1mm in diameter• Voltage between electrodes: Max. 3 kV• Atmosphere : pressurized air, N2, Ar (2 atm.), Vacuum(approx. 300Pa)
HeatingPosition measuring
Laser
Damper
Observation
Pyrometer
Camera
Laser
Senser
On the ground
in Space
Sample Cartridge
Overview of the ISS-ELF
Overview Camera
Pyrometer
Magnifying Camera
Oxygen sensor
Heating Laser
Position sensorlight source
UV fiber head
Hiigh Voltage Connector
UV LampPressure sensor
9 9
THREE-AXIS CONTROL
4 directions
Experiment Volume- 26 sides (polyhedral)
Observation System- in all directions
electrodes(X/Y/Z)position control
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Transferred to the ISS Samples are retrieved by return vehicle
Operation cycle
ELF
MSPRUV Lamp Installed in the Small Experiment Area(SEA)
15 samples per Holder
Installed in the Work Volume
Regularlylaunched/retrieved
Sample Holder
Sample Cartridge
・assembled in JEM・Installed in the MSPR
Initial check out
Multi Purpose Small Payload Rack
10 10
JAXA Demonstration Mission
all resources (power, communication, coolong, vacuum etc.) get from MSPR
Perform experiments continuously without Astronauts.
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Levitation and solidification of molten Al2O3
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12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
M: mass (measured before heating)V: volume (from image analysis)
Chung et al., Rev. Sci. Instrum. 67 (1996), 3517
VM /=ρ
( ) ( )∑=
=5
0cos
nnnPar θθ
( ) θθθπ πdrV sin
32
0
3∫=Tm
Pn cosθ: Legendre polynomial
Density measurement
12
Al2O3
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Density of molten Al2O3
13
Measured correctly in the wide range of temperature including undercooling.
[1] Paradis, et al., J. Jpn. Appl. Phys. 43 (2004) 1496. [2] Glorieux et al., AIP Conf. Proc. 552 (2001) 316.[3] Kirshenbaum et al., J. Inorg. Nucl. Chem. 14 (1960) 283. [4] Florian Kargl et al., Int. J. Microgravity Sci. Appl. 32 (2015) 320200 .
Estimated with the weight measured before heating.
Temperature (K)
Den
sity
(kg/
m3 )
2400
2600
2800
3000
3200
1800 2200 2600 3000 3400
This work
Tm
Tboiling
Florian [4]
Kirschenbaum [3]
Glorieux [2]
Paradis [1]
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Surface tension and viscosity
τρη
ρωγ
5
82
0
30
22
r
r
=
=
ω2: Freq. of mode 2 oscillationτ: Decay constant ρ: density r0:radius of sampleγ: surface tension η: viscosity
Rhim et al., Rev. Sci. Instrum. 70 (1999), 2796
Oscillating drop method
14
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Oscillation excitation/ detection
Bottom electrode
Slit
Power meter
sample
Sinusoidalwave
Top electrode
He-Ne Laser
Uncertainty:γ ±3%
η ±10-15%15
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Surface tension and viscosity of molten Al2O3
16
𝜏𝜏 = 0.0515 sec
𝜔𝜔2 = 1090 𝑟𝑟𝑟𝑟𝑟𝑟/𝑠𝑠
η = 13.8 mPas
𝛾𝛾 = 592 mN/m
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
Utilization Plan
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• Interfacial Energy (2018-2019)• Interfacial tension measurement of molten steel and oxides as
basic research on a steel refining process
• Fragility (2018-2019)• Density and viscosity measurements of high temperature molten
oxides for elucidating the origin of the vitrification
• Technical Demonstration (2017-2019)• Thermophyisical property measurement of binary oxides.
• NASA experiments (2020)• Under the Japan-U.S. Open Platform Partnership Program (Japan-U.S. OP3),
four experiments will be conducted.• Establishing framework for JAXA-NASA Material Science research
collaboration is on going.
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
0
2
4
6
8
10
2300 2400 2500 2600 2700 2800 2900 3000
Present work
Temperature (K)
TmVisc
osity
(mPa・
s) Nb: viscosity
thermophysical properties
Giant permittivity of BaTiO3
2 mm
New glass with high reflection index Casting Simulation
Contribution to Material Science
18
Computer-based casting simulation in order to
develop efficient turbines, aircraft, and jet engines.
Investigation the unknown liquid states of oxidized materials will achieve breakthroughs in science and materials development..
Combined structural analysis of high temperature liquid with X-rays on the ground and ISS-ELF
Novel material synthesisis open the way for future practical application and
production on Earth.
ContributeEarth Benefits
12th Asian Microgravity Symposium 12 - 16 November, 2018 Zhuhai, China
SummaryDensity measurement of molten Al2O3, Fe2O3, Er2O3 and Gd2O3
Surface tension and viscosity of Al2O3, etc.→ ELF’s all functions were verified successfully.
Establishing International Collaboration framework is on-going.
19
Density Density, Surface tension, Viscosity
Target Material