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New HYDROGENIUS for 2015 and beyond
Joichi SugimuraKyushu University
January 31, 2014
Kyushu University
Kyushu UniversityKyushu University
1877 Fukuoka Hospital1903 Fukuoka Medical College (of Kyoto Imperial University)1911 Kyushu Imperial College founded - College of Engineering1911 Kyushu Imperial College founded - College of Engineering1947 Name changed to Kyushu University1949 Reorganized under the new School Education Law2005 St t d t It C2005 Started a move to Ito Campus
Number of students about 19,000 (1,700 from overseas)Number of faculty members about 2 200Number of faculty members about 2,200
2
Building Ito campus – hydrogen campus
JR Kyuudaigakkentoshi Station
Humanity depts. (plan)NEXT-FC (2013.5)
I2CNER (2012.11) Science depts. (plan)
INAMORI Frontier Research CenterSolar cells
General Undergraduate Education
Engineering depts.HYDROGENIUS(2007.11)
Dept. of Hydrogen Energy Systems
Hydrogen Station
International Research Center Lens wind turbine
p y g gy y
for Hydrogen Energy
R ti Agriculture depts. (plan)
3
Reservation zone
Center of Excellence in Hydrogen
Education ResearchEducation ResearchThe 21st Century Center of Excellence Program (MEXT)
International Research Center for Hydrogen Energy
KYUSHU UNIVERSITYDepartment of
Hydrogen Energy Systems
HYDROGENIUS
y g gy
KYUSHU UNIVERSITYAIST
FUKUOKA PREFECTURE
Systems Graduate School,
Kyushu Univ.I2CNER
NEXT-FCFukuoka Strategy Conference
for Hydrogen Energy
FUKUOKA PREFECTURE Fukuoka Personnel
Training Centerfor Hydrogen Energy
NEXT-FC
o yd oge e gy
Expositions, Forum & Symposia
Enlightenment
4
Missions of HYDROGENIUSMissions of HYDROGENIUSin the first stage (2007-2012)
NEDO“Fundamental Research Project on Advanced Hydrogen Science”j y g
to study fundamentals of hydrogen and materials to be used in hydrogen including mechanism of hydrogen embrittlement ,and to provide data necessary for the development of FCVs stationary FC systems andnecessary for the development of FCVs, stationary FC systems and hydrogen infrastructure
to provide principles for design testing and use of materials forto provide principles for design, testing and use of materials for prolonged use in hydrogen
to contribute to revision of regulations and standardization of materials to co t bute to e s o o egu at o s a d sta da d at o o ate a sfor hydrogen systems
Back to Basics
5
Back to Basics
HYDROGENIUS
h h lFatigue and fracture of structural materials
Thermophysical properties
Polymers & elastomers Tribology
H2 H2
6
Hydrogen supply network High pressure天然ガス or LPG
水素
電力
天然ガス or LPG
水素
電力
Hydrogen supply network
Thermophysicalproperties
High pressure hydrogen
電力電力
Compressor
properties
Structural materials
Polymers/elastomers
Storage tanks
materials
TribologyMain body, Pipes, Components, g
Dispenser
gyp ,Piston ring/liners,Seals, Bearings
p
Pressure vessels, Pipes, Valves, Seals
FCVPipes, Valves, Hose Coupler, Seals
7
Tanks, Pipes, Valves, Seals
HYDROGENIUSHYDROGENIUSFriction test under Friction test under highly controlled highly controlled environmentenvironmentHYDROGENIUSHYDROGENIUS
the world unique the world unique research center for research center for hydrogen materials hydrogen materials
40MPa40MPaTribology Tribology TestersTesters
environmentenvironment
Thermophysical Thermophysical 120MPa Fatigue Test Facilities120MPa Fatigue Test Facilities(3 systems)(3 systems)
Our OriginalOur OriginalInstrumentsInstruments
p yp yDatabase of HydrogenDatabase of Hydrogenup to 100MPaup to 100MPa--773K773K
(3 systems)(3 systems)
Compression Compression depression depression
t ft f
U iU i
apparatus for apparatus for elastomerselastomers(95MPa,100℃)
Unique Unique ObservationObservationTechniqueTechniqueCollaboration Collaboration
with with
Fatigue Test under AirFatigue Test under AirPVT measurementPVT measurement(100MPa,500℃)
organizationsorganizations
Fatigue TestFatigue TestFatigue Test Fatigue Test under 1 MPaunder 1 MPaHydrogenHydrogen
Viscosity measurementViscosity measurement(100MPa,500℃)
8
HYDROGENIUS in Phase II (2013-2017)
HYDROGENIUS was reborn in April 2013 as a research center of Kyushu University in collaboration with NEDOcenter of Kyushu University in collaboration with NEDO, AIST and other organizations and industries.
HYDROGENIUS contributes to development of safe and economical hydrogen systems through establishment of d i d l ti th d i i f d t fdesign and evaluation methods, provision of data for standards and regulations, and data for risk assessment.
9
HYDROGENIUS in phase II (2013-2017)HYDROGENIUS in phase II (2013-2017)
NEDONEDO“Research Project for Hydrogen Utilization Technologies”
to explore introduction of various steel materials to reduce cost, and toto explore introduction of various steel materials to reduce cost, and to develop new hydrogen resistant materials
to establish componentsealing and hose materials technologies for high p g g gpressure hydrogen
to establish standard test methods and design principles for high pressure hydrogen
to improve database of hydrogen thermophysical properties for design
to explore safety evaluation methods for hydrogen systems
10
Basics to Practice
Research Sections
Universities, Private companies
AIST Research Units
11
Hydrogen Fatigue and Fracture
Leader Prof. Saburo Matsuoka
Fatigue and Fracture Analysis for safe design
Inspection and AnalysisInspection and AnalysisImportant Findings on Hydrogen Embrittlement
of Hydrogen Refueling Stationsafter DemonstrationAccident Analysis
of Hydrogen Refueling Stationsafter DemonstrationAccident Analysis
1. Hydrogen-enhanced localized plasticity2. Frequency effects of crack growth rate3. Influence of Trace Amount of Hydrogen in Austenitic Stainless SteelsAustenitic Stainless Steels
Design book
Technical information for R&DISO t d d SAE t d d
Technical information for R&DISO t d d SAE t d d
12
ISO-standard、SAE-standardISO-standard、SAE-standardIndustries
HHMechanism of Hydrogen Embrittlement:Frequency effect and the Upper bound
Hydrogen Fatigue and Fracture
10-6
10-5
ycle
)
H:0.49ppmH:0.49ppm
H
H HH
H
H H
H
H HH
H
H HJIS-SCM435
10-7
,da
/dN(
m/c
y
H:0.49ppmH:0.49ppm
da
H
HH HH
H
a da
H
HH HH
H
a
Schematic image of the mechanism of effect ofX30
10 9
10-8
k gr
owth
rate
H:0.47ppmH:0.3ppmH:0.47ppmH:0.3ppm
(f 2H ) 0 58 0 49
Hydrogen-charged
(f=20Hz):0.49→0.24ppm(f=20Hz):0.53→0.27ppm
(f 2H ) 0 58 0 49
Hydrogen-charged
(f=20Hz):0.49→0.24ppm(f=20Hz):0.53→0.27ppm
Schematic image of the mechanism of effect of hydrogen and test frequency on fatigue crack growth.
Hydrogen-charged(0.56ppm)(0.56ppm)
10 10020 30 40 50 60 70809010-10
10-9
Crac
k
(f=0.2Hz):0.58→0.49ppm(f=2Hz):0.58→0.49ppm
Uncharged:0.01ppm
(f=0.2Hz):0.58→0.49ppm(f=2Hz):0.58→0.49ppm
Uncharged:0.01ppm
mMPa17≅ΔK120MPaH2 Fatigue
Test system
Stress intensity factor range,ΔK(MPa√m)
Uncharged specimen
(0.54ppm)Relationship between crack growth rateand stress intensity factor of SCM435 steel for a high-pressure cylinder. (R = -1)
・Slow stress cycles in H2 environment accelerates crack growth rate
13
Slow stress cycles in H2 environment accelerates crack growth rate.・Acceleration of fatigue crack growth rate shows an upper limit factor of ca. 30.
Basic mechanism ofHydrogen Embrittlement
Data collection of structural materials
Contribution to regulations
Hydrogen Fatigue and Fracture
10-6
10-5
/dN
[m/c
ycle
]
Type 316 (over 12 mass % Ni), 0 % cold rolling115 MPa H2, RTR = 0.1, ΔK = 20 MPa m1/2
Hydrogen Embrittlement structural materials
1
1.2SUS316 (12% Ni)
(115MPa)
φ H2/φ
Air
: Data Base : JRCM : Austenitic stainless steel1)×
: Data Base : JRCM : Austenitic stainless steel1)×
9
10-8
10-7
k gr
owth
rate
, da/
0.4
0.6
0.8
SUS316(82MPa)at
ive
redu
ctio
n of
are
a, φ
SUS316L(78MPa)
SUS310S(94MPa)
<In 115 MPa H2 (5N) >SUS316 ( over 12% Ni )
<In air, f = 20 Hz >SUS316 ( over 12% Ni )
<In 115 MPa H2 (7N) >SUS316 ( over 12% Ni )
10-4 10-3 10-2 10-1 100 10110-9
Frequency, f [Hz]
Cra
ck
Increase in FCG resistance by supersaturated hydrogen Strength data
Fatigue property of SUS316(>12%Ni)120MPaH2 Fatigue
Test system6 8 10 12 14 16 18 200
0.2
(82MPa)
Rel
aNi content (mass ppm)
SUS304(PH2=82MPa)
supersaturated hydrogen Strength data Construction of hydrogen structural materials DS for hydrogen infrastructure
y
Case studies of hydrogen stationsSGP Steel
y g
Hydrogen diffusion coefficient data
35MPa CylindersSCM435 Steel
EBSD像
14
蓄圧器a 蓄圧器b 蓄圧器c 蓄圧器d Discovery of test frequency effect and upper limit in acceleration of fatigue crack growth rate of the
steel SGP with hydrogen
EBSD像
Case study of 35 MPa hydrogen cylinder
Leader Prof. Shin Nishimura
Hydrogen Polymer Material
EmergencyRelease couplingHydrogen
V l
Hydrogen dispenserHose
Vessel Accumulator
Rubber O-ring
Plug of hydrogen Receptacle on Receptacle Plugdispenservehicles Receptacle Plug
15
Sealing high pressure hydrogen gas
Hydrogen Polymer Material
Sealing high pressure hydrogen gasRubber materials for O-ring (Ethylene propylene rubber strengthened by carbon black)
1 h afterDegassing
4 h 8 h 11 h
O-ring (NBR resin)f ℃ l
10mm
after 100MPa, 30℃×25 Cycles
Seal failureSeal failure
BlisterBlister140mm
断面
→ Improvement of performance by changing filler from Carbon black→ Improvement of performance by changing filler from Carbon black
5.5mm
16
Improvement of performance by changing filler from Carbon black to Silica which does not absorb hydrogen
Improvement of performance by changing filler from Carbon black to Silica which does not absorb hydrogen
Development and test methods for rubber materials and polymeric
Hydrogen Polymer Material
m)
1400 Model Compound Fracture Mechanicsli
Development and test methods for rubber materials and polymeric materials for hydrogen gas seal and hose under 82 MPa
O-ring squeeze ratio=1ーH/d1・・・10~20%Filli ti A /A 60 80%
Cont
ent
at 1
0 M
Pa(p
pm
EPDM–CB25phr
EPDM–CB50phr
NBR–CB50phr
Blister
NBR–CB25部
U fill d
600
800
1000
1200
1400 Model Compound Data Collection
Defect Origin
M i
Time
Grow of Blister
Grow of Blister
Molecular ChainBlisterCrosslink
Defect
H d1AOR
Filling ratio=AOR/AG・・・60~80%
Critical Pressure of Blister Fracture, ΠF, MPa
Hyd
roge
n C
No BlisterEPDM–SC60phr
NBR–SC60phrEPDM–WC95Unfilled
EPDMUnfilledNBR
0 2 4 6 8 100
200
400 Matrix Origin
Time AG=H × LLd1:O-ring Diameter,H: Gland hight,L: Gland widthCross section area: AOR:O-ring ,Gland
Development of Material Prototype Evaluation Product Evaluation Material Design Model Compound Data Fracture Modeling Design Guideline
O-rings
m)
Chemical Analyses Properties in Hydrogen Damage/Lifetime Analyses
Hydrogen Content
Solid State NMR Hoses
Product
c )c )
c )
Two types of dissolved hydrogenCB filled EPDM
10MPa, 30℃,24hours
●:Experimental Value−:Calculated Value
n Co
nten
t (m
ass.
pp
Solid State NMR
100℃
80℃ 30℃
Pres
sure
(MPa
)
100
Pressure Cycle Test of O-ring
Product Testing:Collaboration with Hydrogen Testing & Research
178 7 6 5 4 3 2 1 0C h e m ica l sh ift (δ in p p m )
U n e xp o
3 5 H2 3 H
1 4 H1 H
C ru d e N B R
g )b )
f)
a )
e )
g )
d ) h )
c )
5 5 H
Chemical Shift(ppm) Elapsed Time(sec)
Hyd
roge
n
Hyd
roge
n P
10101 100 1000 10000
Cycle Number of Failure
Center
17
Hydrogen Tribology
Leader Prof. Joichi Sugimura
F i ti d l b i ti fFriction, wear and lubrication of materials in hydrogen systems
18
Unique and comprehensive hydrogen tribology researches
Hydrogen Tribology
Surface analysis for investigating mechanisms of processes at tribo-interface
Experimental techniques
q p y g gy
Tribotests under controlled gas trace impurities,
p ocesses at t bo te ace
気体g p ,tribotests in 40 MPa hydrogen, cyclic contact tests, rolling contact fatigue tests, tec.
表面層Tribotests for various materials
○Adsorption, reaction, permeation of hydrogen and 1.0E-08
1.0E-07
1.0E-06
量, m
m^2
/N
0.50.60.70.8
0.91
摩擦係数
30405060708090
損確率
, %
水素アルゴン空気
固体
表面層
1.0E-06
1.0E-05
1.0E-04
ear r
ate,
mm
3 /Nm
1.0x10-4
1.0x10-5
1.0x10-6
PTFE
PTFE + Graphite
p y gtrace impurities○Changes in properties of surface and subsurface○Transfer and wear of materials
1.0E-10
1.0E-09
0.1 1 10 100水分濃度, ppm
比摩耗
00.1
0.20.30.4 摩
ピン+ディスク
摩擦係数58
101520
10 100 1000 10000 100000
累積破損
寿命, ×104サイクル
Rolling contact fatigue life ofVariation of friction and wear of Friction and wear of PTFE
1.0E-08
1.0E-07
0.1 0.2 0.3 0.4
Spec
ific
we
Coefficient of friction
1.0x10-8
1.0x10-7
PTFE + Bronzein Hydrogen
PTFE + Bronzein Helium
Rolling contact fatigue life of 52100 steel (SUJ2, PAO10, 4.8GPa, 90℃, Λ=1.69)
Variation of friction and wear of 316L steel in hydrogen with trace of water (10N, 6.3mm/s)
Friction and wear of PTFE composites slid against 316L steel in 40MPa hydrogen●and helium●
19
Contribution to industries with tribology data and design principles
Friction and wear of sealing materials for high pressure hydrogen
Friction and wear properties of polymeric materials for dynamic sealsp y y
Contact and friction behaviors of elastomeric materials for static seals
O ring
Pressure
Hydrogen Thermo-physical Property
Leader Prof. Yasuyuki Takata
Start of measurement of hydrogen thermo-physical property for low temperature and low pressure by NASA for rocket fuel.p p yHydrogen property at high temperature and high pressure is necessary for design of fuel cell systems.
Accurate fueling system
Rapid fueling systemfueling system
Database of thermophysical properties of hydrogenDatabase of thermophysical properties of hydrogen
21
Database of thermophysical properties of hydrogenDatabase of thermophysical properties of hydrogen
PVT(E ti f St t )PVT(E ti f St t ) Th l C d ti itTh l C d ti it
Thermophysical properties necessary in design
H Generator
PVT(Equation of State)PVT(Equation of State) Thermal ConductivityThermal Conductivity
Heat Heat TransferTransfer
DewDewSpecific Specific
H tH tViscosityViscosityH2 Generator Dew Dew
PointPointHeatHeat
yy
Precooler
Compressor Accumulator -60℃
Sound VelocitySound Velocity• Measurement of refueling mass flow rate by PVT data
Dispenser
Sound VelocitySound Velocity
• Estimation of H2 leak rate from a crack・・・・・Sound velocity
• Estimation of pressure drop・・・・・・・Viscosity
70MPa H2 Tank• H2 Purity monitor・・・・・・・Dew point
• Estimation of H2 leak rate from a crack・・・・・Sound velocity
f f
22
Thermophysical property data for hydrogen is a basis of hydrogen society and therefore, the database including accurate PVT, thermal conductivity, viscosity, sound velocity and specific heat is essential. 22
Development of apparauts for thermophysical property measurement Outcome 2006-2012
Hydrogen Thermo-physical Property
measurementMeasurements of H2 thermophysical properties
○PVT data and virial Equation Of State up to 100MPa, 500℃○Measurement and prediction equation for viscosity up to 100MPa and 500℃220 - 350 K
Isochoric PVT apparatus
○Measurement and prediction equation for thermal conductivity up to 100MPa and 500℃○Development of H2 thermophysical property database
C ill i t
1 5 10 50 100-0.4-0.2
00.20.4
220 350 K
300 K250 K
0.20.4
350 - 400 K
393 15 K
353.15 K
OS)
/ ρ v
irial
EO
S
Isochoric PVT apparatus(∼100MPa, 500°C)
Capillary viscometer(∼100MPa, 250°C)
0 4-0.2
00.20.4
400 - 500 K
433.15 K
473.15 K
1 5 10 50 100-0.4-0.2
0 393.15 K
100(
ρ - ρ
viria
l EO
PVT data and EOS
1 5 10 50 100-0.4
P , MPa
Burnett type PVT(∼100MPa 200°C)
Thermal conductivity(∼100MPa 500°C) 0 25
0.30
0.35
0.40
0.45
熱伝導率
[W/(m
·K)]
ノーマル水素
300°C
200°C
100°C150°C
50°C0°C
-50°C
400°C
500°C
14
16
18
20
sity
, η μ
Pa·s
HYDROGEN ExperimentalT:296.15K
Nabizadeh (1999)T:298.15K
Michels (1953) Gracki (1969) Barua (1964) Golubev (1953) Kuss(1952)
T:299.15K Rudenko (1968) Present correlation
FPROP
Michels
(195
3)
(∼100MPa, 200 C) (∼100MPa, 500 C)
0 20 40 60 80 1000.10
0.15
0.20
0.25熱
圧力 [MPa]
-100°C
Roder's correlation
Vi itHighly ingenious
0 50 100 150 2008
10
12
Pressure, P MPa
Vis
cos
REFPR
McCarty (1972)
Diler (1965) Hanley (1972)
23
Viscosityg y g
measurement apparatus Contribution to industry by supplying a reliable database
Thermal conductivity
Hydrogen Safety
Leader Prof. Nobuhiro Kuriyama
Hydrogen safety analysis
Failure in systems and componentsFailure in systems and componentsHuman error
Analysis of “Near miss incidents reports”Analysis of Near miss incidents reportsRisk assessment - from high pressure research facilities to practical systems
24
to practical systems
Cooperation with Industry and Government
FundamentalsN M th d
Hydrogen Energy Test &Research Center (HyTReC)
Education Programfor Engineers and Students
New MethodsMaterials Data etc.
Research Center (HyTReC)
H d S tHydrogen SystemSafe, Reliable, and Low Cost
Policy Making Development of
International Forum
Policy MakingCodes & Standards
Development ofHydrogen Systems
METI, NEDO, KHK INDUSTRIES
25
Local Governments(Fukuoka Pref. etc.)
Automobile, EnergyEngineering etc.
Thank you for your attention !
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