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Development of 1020 MHz NMR superconducting magnet
using Bi-2223 innermost coil
Mamoru Hamada, Japan Superconductor Technology, Inc. Hideaki Maeda, Yoshinori Yanagisawa, RIKEN
Tadashi Shimizu, Gen Nishijima, Shinji Matsumoto, National Institute for Materials Science
Yusuke Nishiyama, Hiroto Suematsu, JEOL RESONANCE Inc.
UHF workshop @ NIH, USA Nov. 12th – 13th 2015
This work is supported by the System Development Program for Advanced Measurement and Analysis
(SENTAN) (Program-S), JST.
2
Collaborators
NIMSS. Matsumoto, K. Hashi, S. Ohki, A. Goto, T. Noguchi, S. Sakai, G. Nishijima and T. Shimizu
RIKENS. Iguchi, Y. Yanagisawa, M. Takahashi and H. Maeda
JEOL RESONANCER. Tanaka, Y. Nishiyama, and H. Suematsu
Kobe SteelT. Miki and K. Saito
3
… and the founder of this project,
the late Dr. Tsukasa Kiyoshi.
Collaborators
4
Outline
n Bi-2223 innermost coil development n Damage by the huge earthquake n Restoration n Cool down n Ramp up and operation at 1020 MHz (24.0 T) n NMR data acquisition n Ramp up to 1030 MHz (24.2 T)
We succeeded in upgrading 920 MHz superconducting magnet to 1020 MHz
using Bi-2223 innermost coil.
5
Critical Current of superconducting materials
1GHz (23.5 T)
NbTiBi-2223
GdBCO
REBCO
RRP Nb3Sn
PIT Nb3Sn
Bronze Nb3Sn
3020100B [T]
J e(A
/mm
2 )
101
102
103
104
T = 4.2 KBronze Nb3Sn @ 2K
Y. Miyoshi et al., Physica C, 516 (2015) 31
6
Concept of upgrading 920 MHz magnet to 1030 MHz
Nb3Sn coil Bi-2223 coil
920 MHz 1030 MHz
7
920 MHz 1020 MHz1995 Start R&D of 1 GHz project1996 Design1997 Wire development1998 Magnet manufacturing
Magnet manufacturingTo give up to use Bi-2212
900 MHz achieved 2008 Start 1020 MHz R&D2000 Performance check @ 900 MHz 2009 NMR at 500MHz driven mode2001 920 MHz achieved 2010 1020 MHz coil assembly2002 NMR measurement 2011 Earthquake2003 NMR measurement 2012 Restoration2004 930 MHz achieved by 2nd magnet 2013 Restoration2005 NMR measurement 2014 1020 MHz achieved2006 NMR measurement NMR measurement2007 NMR measurement 1030 MHz achieved
1999
2015
Progress of 1020 MHz development
8
Feasibility of HTS by PS-driven mode
WATERGATE NOESY (2mM lysozyme in 90%H2O and 10%D2O)
LTS-NMR / Persistent mode HTS/LTS-NMR / Driven mode
HTS/LTS PS-driven mode is feasible for NMR
500 MHz Bi-2223/LTS driven mode NMR magnet
T. Kiyoshi et al., IEEE Trans. Appl. Supercond. 20, 714-717, 2010
1H Chemical shift (ppm) 10 0
1H Chemical shift (ppm) 10 0
10
0
1 H C
hem
ical
shif
t (p
pm)
10
0
1 H C
hem
ical
shif
t (p
pm)
9
Coil configuration of 1030 MHz NMR magnet
High-Jc Nb3Sn(15%Sn bronze)
High-strength Nb3Sn(Ta reinforced)
High-strength Nb-Ti(Cold-worked)
Nb-Ti
Cu-Sn laminatedBi-2223Sumitomo Electric, Ltd.
0.8 25
20
15
-0.6 0.60.40.20.0-0.2-0.4(m)
(m)(T)
0.6
0.4
0.2
0.0
-0.2
-0.4
-0.6
-0.8
10
Bi-2223 innermost coil parameters
840
mm 4.
45 m
m
0.36 mm920 MHz 1030 MHzSuperconductor Nb3Sn Bi-2223Lamination material n/a Cu-SnConductor size [mm] 3.5×1.75 4.45×0.36
Insulation material Glass yarnPolyimide
tapesInsulated conductor size [mm]
3.65×1.90 4.50×0.41
Inner diameter [mm] 78.4 78.4Outer diameter [mm] 124.3 124.0Height [mm] 599.1 840.0Number of layers 12 54Number of turns 1,953 10,094Conductor length [m] 622 3,209Operating current [A] 244.2 242.8Contribution field [T] 0.989 3.66
Bi-2223 coil Bi-2223 wire by Sumitomo
11
Bi-2223 innermost coil manufacturing
Including 5 joints
840
mm 4.
45 m
m
0.36 mm
Bi-2223 coil Bi-2223 wire by Sumitomo
12
Design confirmation test of Bi-2223 coil
Bi-2223 + outer Nb3Sn coils
0 5 10 15 20 25 300
100
200
300
400
500
600
Nb3Sn+Bi-2223
255 A
HM
Current (A)
Magnetic Field (T)
18 T SCM B//
0 2000 4000 6000 8000 100000
50
100
150
200
250
300
-50
0
50
100
150
200
250
Current (A)
Time (s)
Coil Voltage (mV)
Tested at 4.2 K, 11.2 T
no significant voltage increase up to 255 A
R=3.2 µΩ
13
The Great East Japan Earthquake
n 14:46 JST March 11th 2011n The biggest earthquake
ever recorded in Japann Seismic intensity
n Lower-6 in Tsukuban (upper-6 in Sendai)
n Status of the magnet n Cooled down to 4.2 K,
waiting for pumping. n No current, no field.
Tsukuba
epicenter
250mi
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Major damages
LN2 bore
RT bore
15
cut by a pipe cutter
OVC LN2 shieldGCS
４K shieldHe II chamber
Support rods for LN2 chamber were brokenLN2 bore RT bore
Major damages
16
Restoration activity (2011-2013)
Resistance check Helium can assembly
Thermal shield assembly
Restoration completion
17
Cool down
300
250
200
150
100
50
0
Tem
per
ature
[K]
Jun 20 Jul 4 Jul 18 Aug 1Date (CY2014)
5
4
3
2
1
0
Tem
per
ature
[K]
Jul 18Jul 25 Aug 1 Aug 8
Date
He II Bath Magnet top
LHe cooling
Pumping
λ point
Cryogen consumption
LN2 (290-80 K): 10,000 L
LHe (80K-2 K): 6,500 L80K-4 K : 2,500 LStorage : 3,000 L4 K-2 K : 1,000 L
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l Power (commercial power or emergency generator) was supplied to a DC power supply (3 KVA input, 1.2ppm/8hr) through a momentary voltage drop compensator.
l Emergency generator takes 10 seconds to run after the power outage.
l Momentary voltage drop compensator (a kind of UPS) supplies 4 KVA for 15 seconds.
l In case of power supply shuts down, safety switch closes.
Diagram of power supply system
S. Matsumoto, to be published
19
5
4
3
2
1
0
Vcoil [
mV]
250200150100500
Icoil [A]
Bi-2223
Sec #4
Sec #1 (LTS)
Coils Resistance
Section #1 (Nb3Sn)• 21.5 µΩ at 240.5 A (1.24 W)• Possible degradation in
superconducting joint(s)
Section #4 (Nb3Sn)• 4.16 µΩ at 240.5 A (267 mW)• Degraded joint generated
voltage at I>140 A
Final decision: Target field 1030 MHz à 1020 MHz
Bi-2223 innermost coil• 5.28 µΩ at 240.5 A (305 mW)• 1.6 times larger than the
design confirmation test• 5 joints including the coil
Heat load from coil= 1.8 W
Sec #1 (Nb3Sn)
20
During ramp up
21
25
20
15
10
5
0
B [
T]
Aug 15 Sep 12 Oct 10 Nov 7 Dec 5 Jan 2 Jan 30 Feb 27 Mar 27 Apr 24
Date (2014/2015)
250
200
150
100
50
0
I [A]
Ramp up and operation
StartedAug 25
Sep 1722.3 T
(950 MHz)
Oct 123.5 T
(1001 MHz)Oct 2Normal [email protected] T
Oct [email protected] T
Oct 1724.0 T (1020 MHz)
21
2.0
1.8
1.6
1.4Bat
h Te
mpe
ratu
re [
K]
Aug 15 Sep 12 Oct 10 Nov 7 Dec 5 Jan 2 Jan 30 Feb 27 Mar 27 Apr 24
Date (2014/2015)
22
Stability and homogeneity evaluation by NMR
Internal 2H lock operation
Stability < ±0.6 ppm for 70 hrs• w/o NMR lock operation• RT controlled• ripples < ± 0.15 ppm
1 ppb for 10 hFWHM0.7 Hz (0.7 ppb)
K. Hashi et al., JMR, 256 (2015) 30
23
-10 0 10
-10
0
10
20
30
Axial position, z (mm)
Norm
aliz
ed m
agn
etic
field
diffe
rence,
(Bz(
z)-B
z(0))
/B
z(0) (p
pm
)
17.4 ppm
-10 0 10 -10 0 10
Cryoshim Ferroshim
13.2 ppm 2.6 ppm
-10 0 10 -10 0 10
Cryoshim RT shim
0.8 ppm 0.5 ppm
-10 0 10
-2
0
2
-10 0 10
-2
0
2
Higherharmonics
Very large inhomogeneity
50 mm
xy
58.1
mm
44.5
mm
Ironwires Nickel
wires
Ironsheets
x y
Ferroshim RT shim
Y. Yanagisawa et al., Submitted to IEEE Trans. Appl. Supercond.
Shimming
24
NMR data ( 2D-DARR AquaporinZ )
1) H. Maeda et al., Submitted to eMagRes.2) K. Hashi et al., Submitted to Chemistry Letters
7 hr, MAS=10.3 KHz, 3.2 mm rotor, 70 KHz Spinal64 Decoupling
7 hr, external lock MAS=15 KHz, 2.5 mm rotor 70 KHz Spinal64 Decoupling
25
L-Tryptophanyl-glycyl-glycine dihydrate
NMR data ( 17O WGG peptide )
T. Shimuzu et al., 8pA-3, 39th Annual Conf. on Mag. 2015
26
500MHz at 20kHzMAS
1020MHz at 15kHzMAS
２次摂動による分裂がなくなっている。
11B of Na-Borax HydrateNa2B4O5(OH)4.8H2O
NMR data ( 11B in borax )
T. Shimuzu et al., 8pA-3, 39th Annual Conf. on Mag. 2015
27
NMR data ( L-Histidine・HCl・H2O, L-Tyrosine )
L-Histidine,1D ultrafast MAS proton spectra
2D CSA/CS correlation at 60 KHz
L-Tyrosine
1H CSA lineshapes
70KHz 600MHz
60KHz 1020MHz
Y. Nishiyama et al., JMR, 261 (2015) 1
28
Spectral projection
3D SQ/DQ/SQ spectrum60 KHz, 16t1, t2, 8 scans, 6s recycle delay,BABA-XY16 sequence with 133.3µs excitation
SQ1/SQ2
DQ/SQ2
DQ/SQ1
600 MHz 1020 MHz
NMR data ( L-Histidine・HCl・H2O )
Y. Nishiyama et al., JMR, 261 (2015) 1
29
25
20
15
10
5
0
B [
T]
Aug 15 Sep 12 Oct 10 Nov 7 Dec 5 Jan 2 Jan 30 Feb 27 Mar 27 Apr 24
Date (2014/2015)
250
200
150
100
50
0
I [A]
StartedAug 25
Sep 1722.3 T
(950 MHz)
Oct 123.5 T
(1001 MHz)Oct 2Normal [email protected] T
Oct [email protected] T
Oct 1724.0 T (1020 MHz)
Operated for 6 months (1020 MHz)
Apr 14 Ramped up to 1030 MHz (24.2 T)
Ramp up to 1030 MHz ( 24.2 T )
2.0
1.8
1.6
1.4Bat
h Te
mpe
ratu
re [
K]
Aug 15 Sep 12 Oct 10 Nov 7 Dec 5 Jan 2 Jan 30 Feb 27 Mar 27 Apr 24
Date (2014/2015)
24.5
24.0
23.5
23.0
B [T
]
00:00Apr 13
12:00Apr 15
Date (2014/2015)
245
240
235
230
I [A]
24.2 T (1030 MHz) Confirmed by 2D NMR
29
30
Summary We succeeded in upgrading 920 MHz NMR superconducting magnet to 1020 MHz using Bi-2223 innermost coil.
nBi-2223 innermost coil was developed. n Seriously damaged by the huge earthquake. nAfter >2 year restoration, cooled down to ~1.6 K and
operated at ~1.7 K. nGenerated 1020 MHz.nOperated at 1020 MHz NMR for 6 months by power
supply driven mode. n Stability : 1 ppb/10 hr nHomogeneity : 0.7 ppb
with internal 2H lock system operation nGenerated 1030 MHz (24.2 T).
Reference[1] K. Hashi et al., “Achievement of 1020 MHz NMR,” J. Mag. Res., 256, 30, 2015.[2] G. Nishijima et al., to be published.; MT24 2PoBD-‐‑‒08.[3] Y. Nishiyama et al., J. Mag. Res., 261, 1, 2015.[4] G. Nishijima et al., EUCAS 2015 1A-‐‑‒LS-‐‑‒O2.1.[5] T. Kiyoshi et al., “NMR upgrading project towards 1.05 GHz,” IEEE TAS, 18, 860, 2008.[6] T. Kiyoshi et al., “Bi-‐‑‒2223 Innermost Coil for 1.03 GHz NMR Magnet,” IEEE TAS, 21, 2110, 2011.[7] T. Shimizu et al., The 39th Annual Conference on Magnetics in Japan, 2015.
31
Short Summary
1970 1980 1990 2000 2010 20200
10
20
30
40
0.0
0.5
1.0
1.5
NMR magnetic field (T)
Time (year)
1GHz, 23.5T
1GHzNMR920MHzNMR
Super-high-field NMR
This is one small step for an NMR magnet, but one great leap for super high field NMR ( N. A. Armstrong of Apollo 11)
32
Thank you for your attention
