Research Facilities

Research Facilities Fatigue and Fracture of Materials
For the establishment of the guidelines for the design of materials strength and the construction of a database, the basic principle of hydrogen embrittlement is being
investigated by the use of various high-pressure hydrogen fatigue testing machines and vessels, high-resolution microscopes and precise measurement instruments.

120MPa,100MPa Hydrogen Fatigue Testing Machine

100MPa Hydrogen Gas Vessel

To clarify the effect of hydrogen on materials strength, fatigue tests areconducted under hydrogen environments at pressures up to 120MP, 100MPa

For charging metallic materials and rubbers withhydrogen gas［120MPa Hydrogen Fatigue Testing Machine (3 unit)］●Gas pressure:120MPa(max.)●Environmental gas: hydrogen;helium;nitrogen●Testing frequency:10Hz(max.), 20Hz(max.)●Load capacity:±100kN(max.), ±50kN(max.)●Available specimen shape: round bar, plate, compact-tension●Testing temperature:-45 ～ 120℃
●Hydrogen vessel(inside): 145mm(dia.)×460mm(height)［100MPa Hydrogen Fatigue Testing Machine (1 uniit)］【120MPa Hydrogen Fatigue Testing Machine】●Gas pressure: 99MPa(max.)●Environmental gas: hydrogen;argon;helium●Testing frequency: 10Hz(max.)●Load capacity: ±100kN●Available specimen shape: round bar, plate, compact-tension●Testing temperature: -45 ～ 90℃●Hydrogen vessel(inside):150mm(dia.)×460mm(height)●Environmental gas: hydrogen●Gas pressure:100MPa (max.)●Operation temperature: 280℃ (max.)●Volume: 0.5ml(HYDROGENIUS)（41 machines [incl. low-pressure fatigue testing machines]）

Blister Testing Machine for Rubber

Secondary Ion Mass Spectrometry (SIMS)

To evaluate the durability of O-rings

To visualize the 2D/3D distribution of hydrogenin materials●Ion source: cesium (Cs)
●Resolution: 7 × 1016 at./cm3 (for H in Si)●XY resolution: < 1μm●Available measurement area: 35 ～ 250μm (dia.)●Environmental gas: hydrogen ●Pressure range: atmospheric pressure to 90 MPa●Holding time: 0 ～ 99h ●Pressure-increasing rate: 6MPa/s●Pressure-decreasing rate: 0.025 MPa/s ～ 20 MPa/s●Testing temperature range: -60℃～100℃(HYDROGENIUS)(HYDROGENIUS)

Thermal Desorption Spectrometry (TDS)

Thermal Field Emission Scanning Electron Microscope withElectron Backscatter Diffraction Analyzer

For the measurement of hydrogen content inmetallic materials

To analyze the crystallographic orientation of fracturesurface originating from hydrogen embrittlement●Electron gun: shot-key field emission type (ZrO/W cathode)●Resolution: 1.2 nm (for 30 kV), 3.0 nm (for 1 kV)●Accelerating voltage: 0.5 kV ～ 30 kV● Probe current: a few pA ～ 200 nA●Measurement resolution: 0.01 mass ppm●Measurement mass range: M/z:1 ～ 200●Measurement temperature range: RT ～ 1200℃●Vacuum pressure: < 5 × 10 -7 Pa(Kyushu University: 1/HYDROGENIUS: 1)(HYDROGENIUS)

9Research Facilities

Research Facilities Tribology
These test rigs and analyzers are used to study tribological properties of materials in hydrogen for establishing aproper design methodology of tribological elements used in hydrogen systems.

Hydrogen environment friction test rig

Friction test rig with highly-controlled environment

for conducting reciprocating sliding tests inhydrogen gas

for conducting sliding tests in hydrogen withcontrolled purity●Test gases: hydrogen,argon, helium, vacuum●Maximum gas pressure:0.2 MPa●Minimum pressure whenevacuated: less than 1 x10-5 Pa●Maximum frequency ofreciprocating motion: 20Hz
●Maximum normal load: 50 N

●Test gases: hydrogen,argon, helium, vacuum● Minimum pressure whenevacuated: less than 1x10-5Pa●Concentration of water
detected: down to 2 mass ppb●Concentration of oxygen
detected: down to 1 mass ppb●Test configuration: Pin-ondisk test or reciprocating
test●Maximum rotational
speed: 200 rpm●Maximum normal load: 200 N（HYDROGENIUS）（HYDROGENIUS）

Ultra high pressure hydrogen friction test rig

Auger Electron Spectroscope for hydrogen tests (AES)

for conducting pin-on-disk sliding tests in ultra-highpressure hydrogenfor analyzing surfaces before and after sliding
tests in hydrogen●Test gases: hydrogen,argon, helium●Maximum gas pressure:45 MPa●Temperature: -50 to 120 C●Minimum pressure whenevacuated: 0.1 Pa●Test configuration: Pinon-disk test
●Diameter of disk specimen:
between 15 and 60 mm●Maximum rotational
speed: 100 rpm●Maximum normal load: 50 N

●Ion guns: Shot key fieldemission ion gun●Resolution of secondary
electron images: 3 nm
●Resolution of Auger
images: 8 nm
●Minimum pressure whenevacuated: less than 5 x
10-8 Pa（HYDROGENIUS）（HYDROGENIUS）

X-ray Photoelectron Spectroscope for hydrogen tests (XPS)

Sealed transfer vessel for carrying tribology specimens

for analyzing surfaces before and after sliding
tests in hydrogenfor carrying specimens before or after friction
tests in hydrogen to the analyzers in highvacuum or inert gas●X-ray source: Al/Mg twin
target and Al target●Minimum diameter ofanalysis: 30 μm●Minimum pressure whenevacuated: less than 7 x
10-8 Pa●Test rigs to which thevessel can be attached: Thefriction test rig with highlycontrolled environment
and the ultra high pressurehydrogen friction test rig●Analyzers to which the vessel
can be attached:The X-ray
Photoelectron Spectroscope(XPS) and the Auger Electron
Spectroscope (AES)● Minimum pressure whenevacuated:less than 1 x 10-4
Pa

（HYDROGENIUS）（HYDROGENIUS）

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Research Facilities

Research Facilities Thermal engineering, Thermal properties
PVT property (Pressure-Volume-Temperature relationship), viscosity, and thermal conductivity of hydrogen are measured at high pressures
up to 100 MPa accurately by self-developed apparatuses. Permeability of hydrogen at high temperatures up to 500 ℃ is also measured.

Magnetic Suspension Densimeter

PVT Measurement Apparatus by theIsochoric Method

Density is measured based on the Archimedes
buoyancy principle.
The sinker in the pressure vessel is levitated by
the magnetic coupling of a permanent magnet
and electromagnet, and thebuoyancy force working
on the sinker is measured
by an electronic balance.
The density in the vessel
is determined from thebuoyancy force and thevolume of the sinker.

PVT is measured using the isochoric method.
In this method, the pressure vessel is filled
w i t h sample fluid,
and the temperatureand pressure aremeasured along theisochores.

●Temperature range：from200 ℃ to 500 ℃●Pressure range：up to●Temperature range：from room

100 MPa

temperature to 250 ℃●Volume of the pressure●Pressure range：up to 100 MPa

vessel：250 cc●Sinker： mass 28 g, volume 3.3 cc（HYDROGENIUS）（HYDROGENIUS）

Viscosity Measurement Apparatus

Thermal Conductivity Measurement Apparatus

Viscosity is measured using the vibrating wire method. AC
voltage with different frequencies is supplied to the wire set ina magnetic field, and viscosity is determined from the resonant
curve obtained by the measurements of induced voltages.

Thermal conductivity is measured using the transient short hotwire method. A small electrical current is supplied to a fine platinum
wire inside the pressure vessel, and the thermal conductivity isdetermined from the transient temperature change of the wire.

●Temperature range：from -40 ℃ to 500 ℃●Temperature range：from room temperature to 500 ℃●Pressure range：up to 1 MPa●Pressure range：up to 100 MPa●Wire dimensions：diameter 50 μm, length 24 mm●Wire dimensions：diameter 10 μm, length 15 mm（HYDROGENIUS）（HYDROGENIUS）

Hydrogen Permeability Measurement
Apparatus

Flow Rate Through Orifice
Measurement Apparatus

Hydrogen is filled in a seamless coiled tube,
and permeability of hydrogen through metals
is measured from the pressure drop. The
permeability is alsomeasured using agas chromatograph.

High-pressure hydrogen is rapidly expandedfrom a pressure vessel through an orifice imitatinga crack of container,
and the temperatureand pressure changesof the sample during
the expansion aremeasured.
●Temperature range：room temperature●Pressure range：up to●Temperature range：from100 MPa

300 ℃ to 500 ℃●Diameter of the orifice：●Pressure range：up to 1 MPa

0.2 mm●Volume of the vessel：50 cc（HYDROGENIUS）（HYDROGENIUS）

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Research Facilities

Research Facilities Fuel Cells
We have been conducting a wide range of fuel cell R&D, from materials to systems using advanced facilities suchas highest-resolution FESEM-EDX and STEM-FIB systems and fuel-cell evaluation systems as shown below.

Fuel Cell (SOFC) Evaluation Systems

Fuel Cell (PEFC) Evaluation Systems

Automatic electrochemical evaluation system
for SOFCs which can continuously monitor theovervoltages caused
by electrode reactions
and ohmic resistanceof the component
materials separately aswell as current-voltage
characteristics of SOFCs.

Automatic electrochemical evaluation system forPEFCs which can measure the overvoltages caused
by electrode reactions
and ohmic resistanceof the component
materials separately aswell as current-voltage
characteristics of PEFCs.

●Anode gas: H2, CO2, CO, CH4,N2 (< 200 ml min-1)●Cathode gas: Air (< 200 mlmin-1)●Current resolution: 1 mA
●Voltage resolution: 1 mV

●Anode gas: H2 (< 200 ml min-1)●Cathode gas: Air (< 200 mlmin-1)●Current resolution: 1 mA
●Voltage resolution: 1 mV

（Hydrogen Utilization Processes Lab., Kyushu University: 50/Fuel Cell System Lab., Kyushu University: 3）（Hydrogen Utilization Processes Lab., Kyushu University: 10/Fuel Cell System Lab., Kyushu University: 5）

Scanning Transmission Electron Microscope

Focused Ion Beam System

Ultra high-resolution scanning transmission
electron microscope (STEM) equipped with highlysensitive EDX and EELSsystems.

Processing machine for micro-sampling of a specificpart of materials under investigation with a thicknessof less than 100 nm for
STEM observation.

●Magnification: x 4,000,000●Resolution: 0.204 nm●Accelerating voltage: 200 kV●Electron gun: cold FE
attachment:highly-sensitive
EDX and EELS system●Resolution: 6 nm at 40 kV●Accelerating voltage: 10 ～40 kV●Ion source: Ga●Specimen holder: compatible
holder available for STEM

（Hydrogen Utilization Processes Lab., Kyushu University）（Hydrogen Utilization Processes Lab., Kyushu University）

Automatic Gas ChromatographInductively Coupled Plasma (ICP) Emission Spectrometer

Gas chromatograph for long-term consecutive
measurement of fuel gas composition equippedwith automatic dataoutput system.

ICP spectrometer features high ppb level detection
ability, broad 5-6 digit analysis concentration
ranges, and batch
analysis of multiple
elements. Measurements
are completed in only afew minutes.

●Gas species detectable:H 2,O2, N2, CH4, CO, CO2, C2-C6●Carrier gas: He, N2●Detector: TCD●Minimum analyzing time: 20min●Accuracy: 0.01%●Crystal oscillator: 1.6 kW●Output stability: within 0.3%

（Hydrogen Utilization Processes Lab., Kyushu University: 3/Next - FC: 1）（Hydrogen Utilization Processes Lab., Kyushu University）

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