T. Idehara

A spectrometer designed for 6.7 and 14.1 T DNP-enhanced solid-state MAS NMR using quasi-optical microwave transmission

A Dynamic Nuclear Polarisation (DNP) enhanced solid-state Magic Angle Spinning (MAS) NMR spectrometer operating at 6.7 T is described and demonstrated. The 187 GHz TE(13) fundamental mode of the FU CW VII gyrotron is used as the microwave source for this magnetic field strength and 284 MHz (1)H DNP-NMR. The spectrometer is designed for use with microwave frequencies up to 395 GHz (the TE(16) second-harmonic mode of the gyrotron) for DNP at 14.1T (600 MHz (1)H NMR). The pulsed microwave output from the gyrotron is converted to a quasi-optical Gaussian beam using a Vlasov antenna and transmitted to the NMR probe via an optical bench, with beam splitters for monitoring and adjusting the microwave power, a ferrite rotator to isolate the gyrotron from the reflected power and a Martin-Puplett interferometer for adjusting the polarisation. The Gaussian beam is reflected by curved mirrors inside the DNP-MAS-NMR probe to be incident at the sample along the MAS rotation axis. The beam is focussed to a ~1 mm waist at the top of the rotor and then gradually diverges to give much more efficient coupling throughout the sample than designs using direct waveguide irradiation. The probe can be used in triple channel HXY mode for 600 MHz (1)H and double channel HX mode for 284 MHz (1)H, with MAS sample temperatures ≥85 K. Initial data at 6.7 T and ~1 W pulsed microwave power are presented with (13)C enhancements of 60 for a frozen urea solution ((1)H-(13)C CP), 16 for bacteriorhodopsin in purple membrane ((1)H-(13)C CP) and 22 for (15)N in a frozen glycine solution ((1)H-(15)N CP) being obtained. In comparison with designs which irradiate perpendicular to the rotation axis the approach used here provides a highly efficient use of the incident microwave beam and an NMR-optimised coil design.

Development of frequency tunable, medium power gyrotrons (Gyrotron FU series) as submillimeter wave radiation sources

High frequency, medium power gyrotrons (Gyrotron FU series) have been developed at Fukui University as radiation sources covering a broad band from millimeter to submillimeter wave region. They have already been applied to high frequency electron spin resonance and to submillimeter wave scattering in plasma. Many parameters of the gyrotron series could be useful for applications in several new areas. The development and some applications of the Gyrotron FU series are summarized in this paper.

Review of Subterahertz and Terahertz Gyrodevices at IAP RAS and FIR FU

The maximal frequency of radiation higher than 1 THz has been recently obtained in pulse gyrotrons both at IAP (Nizhny Novgorod, Russia) and FIR (Fukui, Japan). CW generation at a 2.2-kW power level is radiated from a 300-GHz gyrotron and used for technological applications. New gyrotrons demonstrate single-mode operation at the second cyclotron harmonic with a frequency of 395 GHz in the CW regime with a power of 100 W and at the third harmonic with frequencies of 371-414 GHz in 10-mus pulses with power of 10-20 kW. Methods of selective excitation of higher cyclotron harmonics, frequency multiplication, and smooth frequency tuning in terahertz gyrotrons are also discussed in the review.

Frequency tunable gyrotron using backward-wave components

We present a frequency tunable scheme for the gyrotron at millimeter/submillimeter regime. Unlike step-tunable type where oscillation jumps discretely in different transverse modes, this scheme allows a smooth tuning within a single transverse mode using its backward-wave component. The characteristics of backward-wave interaction will be shown. A proof of principle experiment was conducted with a sealed cavity. The result shows the oscillation frequency smoothly transitions over a wide range of 6 GHz from 134 to 140 GHz. The proposed mechanism is capable of producing medium output power with broad frequency tunability up to sub-terahertz region.

A 150–600 GHz step‐tunable gyrotron

An account of the operation of a step‐tunable, low‐power, continuous‐wave gyrotron, GYROTRON V, at the fundamental and second harmonic of the electron cyclotron frequency is presented. The design of this gyrotron was especially optimized for the second harmonic. The gyrotron operating frequency at the fundamental can be tuned from 150 to 300 GHz and extended by second‐harmonic operation to above 600 GHz. Under normal operating conditions where the accelerating voltage is 10 kV and the beam current is 50 mA, power levels in excess of 20 W are obtained at the fundamental and hundreds of milliwatts at the second harmonic. The paper includes observations of single mode operation at the second harmonic and mode competition between second harmonic and fundamental.

Development of a second cyclotron harmonic gyrotron operating at submillimeter wavelengths

The development of a high‐frequency, step‐tunable gyrotron operating at submillimeter wavelengths is described. The gyrotron design was optimized for operation at the second harmonic of the electron cyclotron frequency in the TE261 cavity mode, whose resonant frequency is 384 GHz. Experimental results show that second harmonic operation can occur without mode competition as long as the beam current is low (Ib ≲0.8 A), but as the current is increased, the fundamental TE231 cavity mode increases and eventually (Ib ≳1 A) suppresses the second harmonic. The competition between the two modes is studied in detail. The starting current for second harmonic operation is also studied experimentally and compared with calculated results. Other resonances have also been examined. With the present superconducting magnet, the maximum frequency achieved is 402 GHz (second harmonic operation in the TE551 cavity mode) at several kilowatts.

A high harmonic gyrotron with an axis-encircling electron beam and a permanent magnet

A gyrotron with an axis-encircling electron beam is capable of high-frequency operation, because the high-beam efficiency is kept even at high harmonics of the electron cyclotron frequency. We have designed and constructed such a gyrotron with a permanent magnet. The gyrotron has already operated successfully at the third, fourth, and fifth harmonics. The frequencies are 89.3, 112.7, and 138 GHz, respectively, and the corresponding cavity modes are TE/sub 311/, TE/sub 411/, and TE/sub 511/. The permanent magnet system is quite novel and consists of many magnet elements made of NbFeB and additional coils for controlling the field intensities in the cavity and electron gun regions. The magnetic field in the cavity region can be varied from 0.97 to 1.18 T. At the magnetic field intensities, the output powers at the third and the fourth harmonics are 1.7 and 0.5 kW, respectively. The gyrotron is pulsed, the pulse length is 1 ms and the repetition frequency is 1 Hz. The beam energy is 40 kV and the beam current is 1.2-1.3 A. Beam efficiencies and emission patterns have also been measured. In this paper, the experimental results of the gyrotron are described and compared with computer simulations.

Dynamic nuclear polarization experiments at 14.1 T for solid-state NMR.

Instrumentation for high-field dynamic nuclear polarization (DNP) at 14.1 T was developed to enhance the nuclear polarization for NMR of solids. The gyrotron generated 394.5 GHz submillimeter (sub-mm) wave with a power of 40 W in the second harmonic TE(0,6) mode. The sub-mm wave with a power of 0.5-3 W was transmitted to the sample in a low-temperature DNP-NMR probe with a smooth-wall circular waveguide system. The (1)H polarization enhancement factor of up to about 10 was observed for a (13)C-labeled compound with nitroxyl biradical TOTAPOL. The DNP enhancement was confirmed by the static magnetic field dependence of the NMR signal amplitude at 90 K. Improvements of the high-field DNP experiments are discussed.

Generation of high power sub-terahertz radiation from a gyrotron with second harmonic oscillation

New power records of second harmonic gyrotron oscillation have been demonstrated in the sub-THz band. The first step gyrotron of demountable type had succeeded in oscillation with power more than 50 kW at 350 GHz and nearly 40 kW at 390 GHz [T. Notake et al., Phys. Rev. Lett. 103, 225002 (2009)]. Then, the second step gyrotron of sealed-off type was manufactured. A cavity mode was carefully selected to avoid mode competition with a neighboring fundamental harmonic mode. Matching of the selected mode with the electron gun was also circumspectly considered. The second step gyrotron has attained higher power radiation than the first gyrotron. The maximum single mode power was 62 kW at 388 GHz. Then, the electron gun was modified for use of a different cavity mode with a higher coupling coefficient than that for the 62 kW mode. The new mode proved single mode oscillation power of 83 kW at about 389 GHz. These results are new second-harmonic-oscillation power records for sub-THz gyrotrons. The present study constitutes foundations of development of high power second harmonic sub-THz gyrotron for application to collective Thomson scattering measurement on fusion plasmas, especially on high-density plasmas such as those produced in LHD [N. Ohyabu et al., Phys. Rev. Lett. 97, 055002 (2006)]. This paper reports the design consideration to realize high power single mode gyrotron oscillation at second harmonic and the examination of oscillation characteristics of the gyrotron.

Helium-cooling and -spinning dynamic nuclear polarization for sensitivity-enhanced solid-state NMR at 14 T and 30 K.

We describe a (1)H polarization enhancement via dynamic nuclear polarization (DNP) at very low sample temperature T≈30 K under magic-angle spinning (MAS) conditions for sensitivity-enhanced solid-state NMR measurement. Experiments were conducted at a high external field strength of 14.1 T. For MAS DNP experiments at T<<90 K, a new probe system using cold helium gas for both sample-cooling and -spinning was developed. The novel system can sustain a low sample temperature between 30 and 90K for a period of time >10 h under MAS at ν(R)≈3 kHz with liquid He consumption of ≈6 L/h. As a microwave source, we employed a high-power, continuously frequency-tunable gyrotron. At T≈34 K, (1)H DNP enhancement factors of 47 and 23 were observed with and without MAS, respectively. On the basis of these observations, a discussion on the total NMR sensitivity that takes into account the effect of sample temperature and external field strength used in DNP experiments is presented. It was determined that the use of low sample temperature and high external field is generally rewarding for the total sensitivity, in spite of the slower polarization buildup at lower temperature and lower DNP efficiency at higher field. These findings highlight the potential of the current continuous-wave DNP technique also at very high field conditions suitable to analyze large and complex systems, such as biological macromolecules.