Takashi Hase

HTS-NMR: Present Status and Future Plan

Using high-Tc superconductors (HTS) is considered to be the only solution to dramatically increase the highest fields of NMR magnets because of their high critical fields. However, it is not easy to apply HTS to an NMR spectrometer (HTS-NMR) because a persistent-mode operation with HTS cannot satisfy the field stability of 0.01 ppm/h at present. To overcome this problem, we are now developing an HTS-NMR spectrometer in a driven-mode operation. As the first step, a layer-wound coil was fabricated with bronze-reinforced Bi-2223 conductors. Instead of the Nb3Sn coil, the Bi-2223 coil was installed as the innermost part of an existing NMR magnet. The magnet operated at a field of 11.7 T with a highly stabilized power supply. NMR measurements were carried out, and it was demonstrated that the quality of the multi-dimensional NMR spectra on the protein was equivalent to that obtained with a persistent-mode system. The next step will be to demonstrate its usefulness as a high-field NMR system. The upgrade of the 920 MHz NMR system installed at the Tsukuba Magnet Laboratory is underway. Its innermost coil is scheduled to be replaced by a Bi-2223 layer-wound coil for 2010. Its target field is 24.2 T (1.03 GHz).

Persistent-mode operation of a 920 MHz high-resolution NMR magnet

Development of a high-field NMR magnet has been underway at the Tsukuba Magnet Laboratory of the National Institute for Materials Science. The magnet succeeded in a persistent-mode operation at 21.17 T in December 1999. A 283-day long-term operation was carried out from October 2000 to August 2001. It included a persistent operation at 21.6 T (920 MHz) for 108 days. This was the highest field that the superconducting magnets have ever achieved in a persistent operation. Field decay was less than 2 Hz/h. Field homogeneity after correcting with superconducting shim coils were less than 0.1 ppm in a sample volume. These results confirmed that this magnet had been successfully developed as a high-resolution NMR magnet.

Bi-2223 Innermost Coil for 1.03 GHz NMR Magnet

Because of their high critical fields, high-Tc superconductors (HTS) are considered to be the only solution to dramatically increase the highest fields of NMR magnets. We have successfully demonstrated that a 500 MHz HTS/LTS NMR system with a Bi-2223 innermost coil could be used for solution NMR in a driven-mode operation. As the next step, the upgrade of the 920 MHz NMR system installed at the Tsukuba Magnet Laboratory is underway. The innermost Nb3Sn coil has been replaced by a Bi-2223 coil. The coil was fabricated as a layer-wound coil using five Bi-2223 conductors reinforced with bronze tapes. It was connected in series with the outer Nb3Sn and NbTi coils. The magnet is expected to generate a field of 24.2 T (1.03 GHz of 1H resonance frequency) at an operating current of 244.4 A. The test using the Bi-2223 coil and the outer Nb3Sn coils in combination was successfully carried out. The coil has been installed in the 1.03 GHz NMR magnet. Its cooling and operation are scheduled to take place within Fiscal Year 2010.

NMR Upgrading Project Towards 1.05 GHz

An NMR spectrometer over 1 GHz requires the contribution of high-Tc superconductors(HTS). However, a persistent-mode operation with HTS cannot satisfy the field stability of 0.01 ppm/h at present. This is a great barrier for applying HTS to an NMR magnet. To overcome this problem, a new project was undertaken in Japan in October 2006. In the course of the project, we will develop a highly stabilized power supply, field-compensation methods, and measurement techniques that allow a certain field fluctuation. By integrating them, the feasibility of HTS to NMR will be demonstrated. We performed a long-term operation of a 600 MHz NMR magnet in the driven-mode. Allowable field fluctuation of the existing internal lock system for solution NMR was evaluated by a model experiment. As the next step, the innermost Nb3Sn coil of the 600 MHz NMR magnet will be replaced with a Bi-2223 coil, and the field homogeneity, as well as the field stability, will be evaluated. In the final step of the project, the replacement of the innermost coil of the existing 920 MHz NMR magnet will be planned. The targeting field is 24.7 T (1.05 GHz for 1H NMR resonance frequency). The solid-state NMR on 17O nuclei in a labeled peptide will be demonstrated using a magic angle spinning probe; the probe has a 1H decoupling frequency of 1.05 GHz.

Development and operation of superconducting NMR magnet beyond 900 MHz

As a milestone in the 1-GHz NMR magnet project being carried out at the Tsukuba Magnet Laboratory, a 900-MHz class NMR magnet was successfully manufactured and operated in December 1999. The developed magnet is made of 15%Sn-bronze-processed (Nb,Ti)/sub 3/Sn, Ta-reinforced (Nb,Ti)/sub 3/Sn, and NbTi conductors. The room temperature bore of the cryostat is 54 mm is diameter. All the coils are cooled with pressurized superfluid helium. The magnet generated a field of 21.20 T in a driven mode and then operated in a persistent mode at 21.17 T corresponding to a proton NMR frequency of 902 MHz. The field may be raised to the range of 21.6 T (920 MHz) in the near future.

Newly Designed 3 T MRI Magnet Wound With Bi-2223 Tape Conductors

We have designed and fabricated a 3T magnetic resonance imaging magnet system for the human brain, which was wound with Bi-2223 tape conductors. Cooled by a Gifford-McMahon cryocooler, it was operated at 20 K with a stored energy of 2.3 MJ. A magnetic-field homogeneity of 5 ppm was attained at 1.5 T, which was our target value. Using this Bi-2223 high-temperature superconducting magnet, we obtained magnetic resonance images in 1.5 T at 8.5 K. The system was successfully magnetized to 3 T, which is the final target field in our project. This work demonstrates the potential of the high-temperature superconducting magnet for use in human magnetic resonance imaging experiments.

Development of Nb/sub 3/Sn superconductors for a 1 GHz NMR magnet. Dependence of high-field characteristics on tin content in bronze matrix

To realize a 1 GHz NMR magnet, superconducting properties such as critical current density (J/sub c/) and n-value are fundamental for conductors. J/sub c/ improvements of 15% to 27% have been observed in the conductor with Cu-15wt.%Sn-0.3wt.%Ti matrix compared with J/sub c/ in a conductor with Cu-13.wt%Sn-0.3wt.%Ti matrix. In contrast to J/sub c/, differences in n-values between conductors have not appeared. In this study, systematic analysis for dependence of J/sub c/ and n-value in the high field region on Sn content over 13wt.% in bronze was examined based on the microstructures, i.e. the amount of reacted layer, grain size of Nb/sub 3/Sn, and upper critical field (H/sub c2/) supported with stoichiometric analyses.

Development of high Sn content bronze processed Nb/sub 3/Sn superconducting wire for high field magnets

Bronze processed Nb/sub 3/Sn superconducting wire with Cu-16wt%Sn-0.3wt%Ti (16%Sn bronze) matrix has been developed. For the development, two-step approach was taken. At the first step, two kinds of small size round wires, having a bronze to niobium ratio (bronze ratio) of 2.5 and 1.9, were prepared. Heat treatment was made on these wires at 650/spl deg/C or 700/spl deg/C and the effects of bronze ratio and heat treatment temperature on critical current density (J/sub c/) in magnetic field region from 18 to 25 T were examined. A sample with a bronze ratio of 2.5 and heated at 700/spl deg/C was found to show the highest J/sub c/ of all. In the second step, we manufactured commercial scale rectangular cross-sectioned wire using 16%Sn bronze. J/sub c/ n-value in high magnetic field region are estimated for this wire. As a result, the wire showed J/sub c/ and n-value of 115 A/mm/sub 2/ and 37, respectively, at 22 T, 2.1 K, demonstrating the possibility as a candidate superconducting wire for high field magnets such as over-920 MHz NMR magnet.

Bronze route conductors for 1 GHz NMR superconducting magnet

Bronze route Nb/sub 3/Sn conductors applied to 1 GHz nuclear magnetic resonance spectrometer have been manufactured. Cu-1Swt%Sn-0.3wt%Ti (15% Sn-bronze) Nb/sub 3/Sn conductors employed in inner coils have shown overall J/sub c/ over 100 A/mm/sup 2/ in 21 T at 1.8 K. Other conductors with a Ta-core as a reinforcement employed in outer coils have presented a 0.2% proof strength of 300 MPa at 4.2 K. It is also reported that J/sub c/ of 15%-bronze conductors is enhanced to match that of the tube-processed Nb/sub 3/Sn conductors in the middle magnetic field region of 12-16 T.

Improvement of J/sub c/ in Bi-2212-Ag composite superconductor by controlling Po/sub 2/ on the partial melt process

In a partial melt process for Bi-2212-Ag composite tapes, round and rectangular shape superconductors, the effects of oxygen partial pressure (Po/sub 2/) on the critical current density (J/sub c/) have been studied. It was found that the J/sub c/ of Bi-2212-Ag composite tapes increased from 4.5/spl times/10/sup 4/ A/cm/sup 2/ to 2.2/spl times/10/sup 5/ A/cm/sup 2/ at 4.2 K in zero magnetic field with increasing Po/sub 2/ from 0.1 bar to 1.0 bar. SEM observation for the cross sectional image and J/sub c/ measurement revealed that the partial melt process under higher Po/sub 2/ was effective in realizing well-aligned structure along the silver wall. These results were explained by the idea that crystallization of the Bi-2212 system starts at the interface between the liquid phase and the oxygen rich gas phase. In order to prove the potentiality of this process for the rectangular shape conductors, fabrication of a solenoid magnet has been attempted using rectangular shape conductors under high oxygen partial pressure. The typical results of this solenoid magnet, 2.7/spl times/10/sup 4/ A/cm/sup 2/ in J/sub c/ with generating magnetic field 0.70 T, and 4.3/spl times/10/sup 4/ A/cm/sup 2/ in quenching current density with generating magnetic field 1.13 T have been observed at 4.2 K in the self magnetic field.<<ETX>>