thermophyical property measurement results of ultra-high

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

1©JAXA


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


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…


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


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


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


Electrostatic levitation furnace in the International Space Station (ISS-ELF)

7

©NASA/JAXA


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


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


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.

http://en.wikipedia.org/wiki/File:SpaceX_Dragon_-_2007_X-Prize_Cup.JPG


Levitation and solidification of molten Al2O3

11


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


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]


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


Oscillation excitation/ detection

Bottom electrode

Slit

Power meter

sample

Sinusoidalwave

Top electrode

He-Ne Laser

Uncertainty:γ ±３％

η ±10-15％15


Surface tension and viscosity of molten Al2O3

16

𝜏𝜏 = 0.0515 sec

𝜔𝜔2 = 1090 𝑟𝑟𝑟𝑟𝑟𝑟/𝑠𝑠

η = 13.8 mPas

𝛾𝛾 = 592 mN/m


Utilization Plan

17

• 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.


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


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

thermophyical property measurement results of ultra-high

Documents