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A 110 GHz quasi-optical ring resonator, designed for use with a 1 MW pulsed gyrotron, has been built and successfully tested using a 100 mW solid-state source. A low reflectance (2.4%) input coupler and a low-loss, four-mirror ring demonstrated a compression ratio, defined as the ratio of output to input power, of 36. The 6 ns output pulses were generated from the 2 m length ring using a silicon laser-driven semiconductor switch (LDSS). The quasi-optical ring resonator was designed with large waist sizes so that input pulses of up to 1 MW will stay under the 35 kV/cm electric field limit for ionization in ambient air. Maximum compression gain was achieved by matching the input coupling fraction to the round trip loss in the ring, achieving close to critical coupling. The experimental output pulse shape obtained after firing the LDSS was modeled using the reflectance, transmittance, and absorptance of the switch vs. time and vs. laser pulse fluence, with good agreement found with theory. The timing for the peak energy efficiency of 32% was found and the main loss mechanism limiting that efficiency was found to be the absorptance in the silicon wafer., Competing Interests: Conflict of Interest The authors declare no competing interests.

We present 3D electromagnetic simulations of the coupling of a 250 GHz beam to the sample in a 380 MHz DNP NMR spectrometer. To obtain accurate results for magic angle spinning (MAS) geometries, we first measured the complex dielectric constants of zirconia, sapphire, and the sample matrix material (DNP juice) from room temperature down to cryogenic temperatures and from 220 to 325 GHz with a VNA and up to 1 THz with a THz TDS system. Simulations of the coupling to the sample were carried out with the ANSYS HFSS code as a function of the rotor wall material (zirconia or sapphire), the rotor wall thickness, and the THz beam focusing (lens or no lens). For a zirconia rotor, the B 1 field in the sample was found to be strongly dependent on the rotor wall thickness, which is attributed to the high refractive index of zirconia. The optimum thickness of the wall is likely due to a transmission maximum but is offset from the thickness predicted by a simple calculation for a flat slab of the wall material. The B 1 value was found to be larger for a sapphire rotor than for a zirconia rotor for all cases studied. The results found in this work provide new insights into the coupling of THz radiation to the sample and should lead to improved designs of future DNP NMR instrumentation., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Inc. All rights reserved.)

Dynamic nuclear polarization (DNP) improves the sensitivity of NMR spectroscopy by the transfer of electron polarization to nuclei via irradiation of electron-nuclear transitions with microwaves at the appropriate frequency. For fields > 5 T and using g ∼ 2 electrons as polarizing agents, this requires the availability of microwave sources operating at >140 GHz. Therefore, microwave sources for DNP have generally been continuous-wave (CW) gyrotrons, and more recently solid state, oscillators operating at a fixed frequency and power. This constraint has limited the DNP mechanisms which can be exploited, and stymied the development of new time domain mechanisms. We report here the incorporation of a microwave source enabling facile modulation of frequency, amplitude, and phase at 9 T (250 GHz microwave frequency), and we have used the source for magic-angle spinning (MAS) NMR experiments. The experiments include investigations of CW DNP mechanisms, the advantage of frequency-chirped irradiation, and a demonstration of an Overhauser enhancement of ∼25 with a recently reported water-soluble BDPA radical, highlighting the potential for affordable and compact microwave sources to achieve significant enhancement in aqueous samples, including biological macromolecules. With the development of suitable microwave amplifiers, it should permit exploration of multiple new avenues involving time domain experiments., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Inc. All rights reserved.)

The reflectance ( R ) and transmittance ( T ) of Si and GaAs wafers irradiated by a 6 ns pulsed, 532 nm laser have been studied for s- and p-polarized 250 GHz radiation as a function of laser fluence and time. The measurements were carried out using precision timing of the R and T signals, allowing an accurate determination of the absorptance ( A ) where A = 1 - R - T . Both wafers had a maximum reflectance above 90% for a laser fluence ≥ 8  mJ / cm 2 . Both also showed an absorptance peak of ~50% lasting ~2 ns during the risetime of the laser pulse. Experimental results were compared with a stratified medium theory using the Vogel model for the carrier lifetime and the Drude model for permittivity. Modeling showed that the large absorptance at the early part of the rise of the laser pulse was due to the creation of a lossy, low carrier density layer. For Si, the measured R ,   T and A were in very good agreement with theory on both the nanosecond time scale and the microsecond scale. For GaAs, the agreement was very good on the nanosecond scale but only qualitatively correct on the microsecond scale. These results may be useful for planning applications of laser driven semiconductor switches.

The application of radio frequency (RF) vacuum electronics for the betterment of the human condition began soon after the invention of the first vacuum tubes in the 1920s and has not stopped since. Today, microwave vacuum devices are powering important applications in health treatment, material and biological science, wireless communication-terrestrial and space, Earth environment remote sensing, and the promise of safe, reliable, and inexhaustible energy. This article highlights some of the exciting application frontiers of vacuum electronics.

The effect of reflection is studied experimentally and theoretically on a high-power 110 GHz gyrotron operating in the TE 22,6 mode in 3 μ s pulses at 96 kV, 40 A. The experimental setup allows variation of the reflected power from 0 to 33 % over a range of gyrotron operating conditions. The phase of the reflection is varied by translating the reflector along the axis. Operating at a higher efficiency point, at 4:40 T with 940 kW of output power, reflected power exceeding 11% causes a switch from operation in the TE 22,6 to simultaneous operation in the TE 22,6 and TE 21,6 modes with a large decrease of the total gyrotron output power. This switching effect is in good agreement with simulations using the MAGY code. Operating at a more stable point, 4:44 T with 580 kW of output power, when the reflection is increased, the output power remains in the TE 22,6 mode but it decreases monotonically with increasing reflection, dropping to 200 kW at 33% reflection. Furthermore, at a reflection above 22%, a power modulation at 25 to 30 MHz is observed, independent of the phase of the reflected wave. Such a modulated signal may be useful in spectroscopic and other applications.

The phase stability of a 140GHz, 1kW pulsed gyro-amplifier system and the phase dependence on the cathode voltage were experimentally measured. To optimize the measurement precision, the amplifier was operated at 47 kV and 1 A, where the output power was ∼ 30W. The phase was determined to be stable both pulse-to-pulse and during each pulse, so far as the cathode voltage and electron beam current are constant. The phase variation with voltage was measured and found to be 130±30°/kV, in excellent agreement with simulations. The electron gun used in this device is non-adiabatic, resulting in a steep slope of the beam pitch factor with respect to cathode voltage. This was discovered to be the dominant factor in the phase dependence on voltage. The use of an adiabatic electron gun is predicted to yield a significantly smaller phase sensitivity to voltage, and thus a more phase-stable performance. To our knowledge, these are the first phase measurements reported for a gyro-amplifier operating at a frequency above W-band., Competing Interests: Conflict of Interest The authors declare that they have no conflict of interest.

We report the design and experimental demonstration of a frequency tunable terahertz gyrotron at 527 GHz built for an 800 MHz Dynamic Nuclear Polarization enhanced Nuclear Magnetic Resonance (DNP-NMR) spectrometer. The gyrotron is designed at the second harmonic ( ω = 2 ω c ) of the electron cyclotron frequency. It produces up to 9.3 W continuous microwave (CW) power at 527.2 GHz frequency using a diode type electron gun operating at V = 16.65 kV, I b = 110 mA in a TE 11,2,1 mode, corresponding to an efficiency of ~0.5%. The gyrotron is tunable within ~ 0.4 GHz by combining voltage and magnetic field tuning. The gyrotron has an internal mode converter that produces a Gaussian-like beam that couples to the HE 11 mode of an internal 12 mm i.d. corrugated waveguide periscope assembly leading up to the output window. An external corrugated waveguide transmission line system is built including a corrugated taper from 12 mm to 16 mm i.d. waveguide followed by 3 m of the 16 mm i.d. waveguide The microwave beam profile is measured using a pyroelectric camera showing ~ 84% HE 11 mode content.

This Letter reports the successful experimental demonstration of amplification of subterahertz radiation in a klystron with photonic crystal cavities. The klystron has six cavities, with each cavity having a series of oversized photonic crystal cells made up of a 5×3 array of square posts. The center post is removed from each cell to form a highly oversized (0.8  mm∼λ/4) beam tunnel, with power coupling from cell to cell through the tunnel. The pulsed electron beam is operated at 23.5 kV, 330 mA in a 0.5 T solenoidal field. At 93.7 GHz, a small-signal gain of 26 dB and a saturated output power of 30 W are obtained. Experimental results are in very good agreement with the predictions of a particle-in-cell code. The successful achievement of high gain operation of a photonic crystal klystron amplifier is promising for the future extension of klystron operation well into the terahertz frequency region.

We report experimental measurements of the threshold for multipactor discharges on dielectric surfaces at 110 GHz. Multipactor was studied in two geometries: electric field polarized parallel to or perpendicular to the sample surface. Measured multipactor thresholds ranged from 15 to 34  MV/m, more than 10 times higher than those found at conventional microwave frequencies. Measured thresholds were compared with prior data at lower frequencies, showing agreement with theoretical predictions that thresholds increase linearly with frequency. Measurements of the rf power dissipated in the multipactor show low dissipation (≤1%) for the parallel electric field case, but very strong dissipation for the perpendicular case, also in agreement with theoretical predictions. The agreement between experiment and theory over a wide range of frequencies provides a strong basis for the understanding of dielectric multipactor discharges.

We describe the design and construction of a modular, triple-resonance, fully balanced, DNP-MAS probe based on transmission line technology and its integration into a 500 MHz/330 GHz DNP-NMR spectrometer. A novel quantitative probe design and characterization strategy is developed and employed to achieve optimal sensitivity, RF homogeneity and excellent isolation between channels. The resulting three channel HCN probe has a modular design with each individual, swappable module being equipped with connectorized, transmission line ports. This strategy permits attachment of a mating connector that facilitates accurate impedance measurements at these ports and allows characterization and adjustment (e.g. for balancing or tuning/matching) of each component individually. The RF performance of the probe is excellent; for example, the 13 C channel attains a Rabi frequency of 280 kHz for a 3.2 mm rotor. In addition, a frequency tunable 330 GHz gyrotron operating at the second harmonic of the electron cyclotron frequency was developed for DNP applications. Careful alignment of the corrugated waveguide led to minimal loss of the microwave power, and an enhancement factor ε = 180 was achieved for U- 13 C urea in the glassy matrix at 80 K. We demonstrated the operation of the system with acquisition of multidimensional spectra of cross-linked lysozyme crystals which are insoluble in glycerol-water mixtures used for DNP and samples of RNA., (Copyright © 2019 Elsevier Inc. All rights reserved.)

A laser-driven semiconductor switch (LDSS) employing silicon (Si) and gallium arsenide (GaAs) wafers has been used to produce nanosecond-scale pulses from a 3 μ s, 110 GHz gyrotron at the megawatt power level. Photoconductivity was induced in the wafers using a 532 nm laser, which produced 6 ns, 230 mJ pulses. Irradiation of a single Si wafer by the laser produced 110 GHz RF pulses with a 9 ns width and >70% reflectance. Under the same conditions, a single GaAs wafer yielded 24 ns 110 GHz RF pulses with >78% reflectance. For both semiconductor materials, a higher value of reflectance was observed with increasing 110 GHz beam intensity. Using two active wafers, pulses of variable length down to 3 ns duration were created. The switch was tested at incident 110 GHz RF power levels up to 600 kW. A 1-D model is presented that agrees well with the experimentally observed temporal pulse shapes obtained with a single Si wafer. The LDSS has many potential uses in high power millimeter-wave research, including testing of high-gradient accelerator structures., (Copyright © 2019 Author(s).)

We present the first demonstration of high-power, reversed-Cherenkov wakefield radiation by electron bunches passing through a metamaterial structure. The structure supports a fundamental transverse magnetic mode with a negative group velocity leading to reversed-Cherenkov radiation, which was clearly verified in the experiments. Single 45 nC electron bunches of 65 MeV traversing the structure generated up to 25 MW in 2 ns pulses at 11.4 GHz, in excellent agreement with theory. Two bunches of 85 nC with appropriate temporal spacing generated up to 80 MW by coherent wakefield superposition, the highest rf power that metamaterial structures ever experienced without damage. These results demonstrate the unique features of metamaterial structures that are very attractive for future high-gradient wakefield accelerators, including two-beam and collinear accelerators. Advantages include the high shunt impedance for high-power generation and high-gradient acceleration, the simple and rugged structure, and a large parameter space for optimization.

We report the amplification of 250 GHz pulses as short as 260 ps without observation of pulse broadening using a photonic-band-gap circuit gyrotron traveling-wave-amplifier. The gyrotron amplifier operates with a device gain of 38 dB and an instantaneous bandwidth of 8 GHz. The operational bandwidth of the amplifier can be tuned over 16 GHz by adjusting the operating voltage of the electron beam and the magnetic field. The amplifier uses a 30 cm long photonic-band-gap interaction circuit to confine the desired TE 03 -like operating mode while suppressing lower order modes which can result in undesired oscillations. The circuit gain is >55 dB for a beam voltage of 23 kV and a current of 700 mA. These results demonstrate the wide bandwidths and a high gain achievable with gyrotron amplifiers. The amplification of picosecond pulses of variable lengths, 260-800 ps, shows good agreement with the theory using the coupled dispersion relation and the gain-spectrum of the amplifier as measured with quasi-CW input pulses.

The design and experimental results of a 140 GHz gyro-amplifier that uses a dielectric-loaded, sever-less confocal waveguide are presented. The gyro-traveling wave amplifier uses the HE 06 mode of a confocal geometry with power coupled in and out of the structure with Vlasov-type, quasi-optical couplers. Dielectric loading attached to the side of the confocal structure suppresses unwanted modes allowing zero-drive stable operation at 48 kV and 3A of beam current. The confocal gyro-amplifier demonstrated a peak circuit gain of 35 dB, a bandwidth of 1.2 GHz and a peak output power of 550 W at 140.0 GHz.

The linear and nonlinear theory of a gyroamplifier using a confocal waveguide is presented. A quasi-optical approach to describing the modes of a confocal waveguide is derived. Both the equations of motion and the mode excitation equation are derived in detail. The confocal waveguide circuit has the advantage of reducing mode competition but the lack of azimuthal symmetry presents challenges in calculating the gain. In the linear regime, the gain calculated using the exact form factor for the confocal waveguide agrees with an azimuthally averaged form factor. A beamlet code including velocity spread effects has been written to calculate the linear and nonlinear (saturated) gain. It has been successfully benchmarked against the MAGY code for azimuthally symmetric cases. For the confocal waveguide, the beamlet code shows that the saturated gain is reduced when compared with results obtained using an azimuthally averaged form factor. The beamlet code derived here extends the capabilities of nonlinear gyroamplifier theory to configurations that lack azimuthal symmetry.

An electron beam passing through a metamaterial structure is predicted to generate reversed Cherenkov radiation, an unusual and potentially very useful property. We present an experimental test of this phenomenon using an intense electron beam passing through a metamaterial loaded waveguide. Power levels of up to 5 MW are observed in backward wave modes at a frequency of 2.40 GHz using a one microsecond pulsed electron beam of 490 keV, 84 A in a 400 G magnetic field. Contrary to expectations, the output power is not generated in the Cherenkov mode. Instead, the presence of the magnetic field, which is required to transport the electron beam, induces a Cherenkov-cyclotron (or anomalous Doppler) instability at a frequency equal to the Cherenkov frequency minus the cyclotron frequency. Nonlinear simulations indicate that the Cherenkov-cyclotron mode should dominate over the Cherenkov instability at a lower magnetic field where the highest output power is obtained.

Simple analytical formulae are presented for the design of linear tapers with very low mode conversion loss in overmoded corrugated waveguides. For tapers from waveguide radius a 2 to a 1 , with a 1 < a 2 , the optimal length of the taper is 3.198 a 1 a 2 /λ. Here, λ is the wavelength of radiation. The fractional loss of the HE 11 mode in an optimized taper is [Formula: see text]. These formulae are accurate when a 2 ≲ 2 a 1 . Slightly more complex formulae, accurate for a 2 ≤ 4 a 1 , are also presented in this paper. The loss in an overmoded corrugated linear taper is less than 1 % when a 2 ≤ 2.12 a 1 and less than 0.1 % when a 2 ≤ 1.53 a 1 . The present analytic results have been benchmarked against a rigorous mode matching code and have been found to be very accurate. The results for linear tapers are compared with the analogous expressions for parabolic tapers. Parabolic tapers may provide lower loss, but linear tapers with moderate values of a 2 / a 1 may be attractive because of their simplicity of fabrication.

We present results for the successful fabrication of low-loss THz metallic waveguide components using direct machining with a CNC end mill. The approach uses a split-block machining process with the addition of an RF choke running parallel to the waveguide. The choke greatly reduces coupling to the parasitic mode of the parallel-plate waveguide produced by the split-block. This method has demonstrated loss as low as 0.2 dB/cm at 280 GHz for a copper WR-3 waveguide. It has also been used in the fabrication of 3 and 10 dB directional couplers in brass, demonstrating excellent agreement with design simulations from 240-260 GHz. The method may be adapted to structures with features on the order of 200 μm.

We present a novel, relatively simple method for determining the mode content of the linearly polarized modes of a corrugated waveguide using the moments of the intensity pattern of the field radiated from the end of the waveguide. This irradiance moment method is based on calculating the low-order irradiance moments, using measured intensity profiles only, of the radiated field from the waveguide aperture. Unlike the phase retrieval method, this method does not use or determine the phase distribution at the waveguide aperture. The new method was benchmarked numerically by comparison with sample mode mixtures. The results predict less than ±0.7% error bar in the retrieval of the mode content. The method was also tested using high-resolution experimental data from beams radiated from 63.5 mm and 19 mm corrugated waveguides at 170 and 250 GHz, respectively. The results showed a very good agreement of the mode content retrieved using the irradiance moment method versus the phase retrieval technique. The irradiance moment method is most suitable for cases where the modal power is primarily in the fundamental HE 11 mode, with <8% of the power in high-order modes.

When using overmoded corrugated waveguide transmission lines for high power applications, it is necessary to control the mode content of the system. Ideally, overmoded corrugated transmission lines operate in the fundamental HE 11 mode and provide low losses for long distances. Unwanted higher order modes (HOMs), particularly LP 11 and HE 12 , are often excited in the experimental systems due to practical misalignments in the transmission line system. This paper discusses how the unwanted modes propagate along with the fundamental mode in the transmission line system by formulating an equation that relates the center of power offset and angle of propagation of a beam (for the HE 11 and LP 11 modes) or the waist size and phase front radius of curvature of a beam (for the HE 11 and HE 12 modes). By introducing two miter bend correctors into the transmission system-miter bends that have slightly angled or ellipsoidal mirrors-the HOMs can be precisely manipulated in the system. This technique can be used to eliminate small quantities of unwanted modes, thereby creating a nearly pure fundamental mode beam with minimal losses. Examples of these applications are calculated and show the theoretical conversion of up to 10% HOM content into the fundamental HE 11 mode with minimal losses.

We report the experimental demonstration of a gyrotron traveling-wave-tube amplifier at 250 GHz that uses a photonic band gap (PBG) interaction circuit. The gyrotron amplifier achieved a peak small signal gain of 38 dB and 45 W output power at 247.7 GHz with an instantaneous -3  dB bandwidth of 0.4 GHz. The amplifier can be tuned for operation from 245-256 GHz. The widest instantaneous -3  dB bandwidth of 4.5 GHz centered at 253.25 GHz was observed with a gain of 24 dB. The PBG circuit provides stability from oscillations by supporting the propagation of transverse electric (TE) modes in a narrow range of frequencies, allowing for the confinement of the operating TE03-like mode while rejecting the excitation of oscillations at nearby frequencies. This experiment achieved the highest frequency of operation for a gyrotron amplifier; at present, there are no other amplifiers in this frequency range that are capable of producing either high gain or high output power. This result represents the highest gain observed above 94 GHz and the highest output power achieved above 140 GHz by any conventional-voltage vacuum electron device based amplifier.

During the three decades 1980-2010, magic angle spinning (MAS) NMR developed into the method of choice to examine many chemical, physical, and biological problems. In particular, a variety of dipolar recoupling methods to measure distances and torsion angles can now constrain molecular structures to high resolution. However, applications are often limited by the low sensitivity of the experiments, due in large part to the necessity of observing spectra of low-γ nuclei such as the I = 1/2 species (13)C or (15)N. The difficulty is still greater when quadrupolar nuclei, such as (17)O or (27)Al, are involved. This problem has stimulated efforts to increase the sensitivity of MAS experiments. A particularly powerful approach is dynamic nuclear polarization (DNP) which takes advantage of the higher equilibrium polarization of electrons (which conventionally manifests in the great sensitivity advantage of EPR over NMR). In DNP, the sample is doped with a stable paramagnetic polarizing agent and irradiated with microwaves to transfer the high polarization in the electron spin reservoir to the nuclei of interest. The idea was first explored by Overhauser and Slichter in 1953. However, these experiments were carried out on static samples, at magnetic fields that are low by current standards. To be implemented in contemporary MAS NMR experiments, DNP requires microwave sources operating in the subterahertz regime, roughly 150-660 GHz, and cryogenic MAS probes. In addition, improvements were required in the polarizing agents, because the high concentrations of conventional radicals that are required to produce significant enhancements compromise spectral resolution. In the last two decades, scientific and technical advances have addressed these problems and brought DNP to the point where it is achieving wide applicability. These advances include the development of high frequency gyrotron microwave sources operating in the subterahertz frequency range. In addition, low temperature MAS probes were developed that permit in situ microwave irradiation of the samples. And, finally, biradical polarizing agents were developed that increased the efficiency of DNP experiments by factors of ∼4 at considerably lower paramagnet concentrations. Collectively, these developments have made it possible to apply DNP on a routine basis to a number of different scientific endeavors, most prominently in the biological and material sciences. This Account reviews these developments, including the primary mechanisms used to transfer polarization in high frequency DNP, and the current choice of microwave sources and biradical polarizing agents. In addition, we illustrate the utility of the technique with a description of applications to membrane and amyloid proteins that emphasizes the unique structural information that is available in these two cases.

We describe the design and implementation of the instrumentation required to perform DNP-NMR at higher field strengths than previously demonstrated, and report the first magic-angle spinning (MAS) DNP-NMR experiments performed at (1)H/e(-) frequencies of 700 MHz/460 GHz. The extension of DNP-NMR to 16.4 T has required the development of probe technology, cryogenics, gyrotrons, and microwave transmission lines. The probe contains a 460 GHz microwave channel, with corrugated waveguide, tapers, and miter-bends that couple microwave power to the sample. Experimental efficiency is increased by a cryogenic exchange system for 3.2 mm rotors within the 89 mm bore. Sample temperatures ≤85 K, resulting in improved DNP enhancements, are achieved by a novel heat exchanger design, stainless steel and brass vacuum jacketed transfer lines, and a bronze probe dewar. In addition, the heat exchanger is preceded with a nitrogen drying and generation system in series with a pre-cooling refrigerator. This reduces liquid nitrogen usage from >700 l per day to <200 l per day and allows for continuous (>7 days) cryogenic spinning without detrimental frost or ice formation. Initial enhancements, ε=-40, and a strong microwave power dependence suggests the possibility for considerable improvement. Finally, two-dimensional spectra of a model system demonstrate that the higher field provides excellent resolution, even in a glassy, cryoprotecting matrix., (Copyright © 2012 Elsevier Inc. All rights reserved.)

We described a versatile spectrometer designed for the study of dynamic nuclear polarization (DNP) at low temperatures and high fields. The instrument functions both as an NMR spectrometer operating at 212 MHz ((1)H frequency) with DNP capabilities, and as a pulsed-EPR operating at 140 GHz. A coiled TE(011) resonator acts as both an NMR coil and microwave resonator, and a double balanced ((1)H, (13)C) radio frequency circuit greatly stabilizes the NMR performance. A new 140 GHz microwave bridge has also been developed, which utilizes a four-phase network and ELDOR channel at 8.75 GHz, that is then multiplied and mixed to obtain 140 GHz microwave pulses with an output power of 120 mW. Nutation frequencies obtained are as follows: 6 MHz on S=1/2 electron spins, 100 kHz on (1)H, and 50 kHz on (13)C. We demonstrate basic EPR, ELDOR, ENDOR, and DNP experiments here. Our solid effect DNP results demonstrate an enhancement of 144 and sensitivity gain of 310 using OX063 trityl at 80 K and an enhancement of 157 and maximum sensitivity gain of 234 using Gd-DOTA at 20 K, which is significantly better performance than previously reported at high fields (≥3 T)., (Copyright © 2012 Elsevier Inc. All rights reserved.)

We describe the design and implementation of a novel tunable 250 GHz gyrotron oscillator with >10 W output power over most of a 3 GHz band and >35 W peak power. The tuning bandwidth and power are sufficient to generate a >1 MHz nutation frequency across the entire nitroxide EPR lineshape for cross effect DNP, as well as to excite solid effect transitions utilizing other radicals, without the need for sweeping the NMR magnetic field. Substantially improved tunability is achieved by implementing a long (23 mm) interaction cavity that can excite higher order axial modes by changing either the magnetic field of the gyrotron or the cathode potential. This interaction cavity excites the rotating TE(₅,₂,q) mode, and an internal mode converter outputs a high-quality microwave beam with >94% Gaussian content. The gyrotron was integrated into a DNP spectrometer, resulting in a measured DNP enhancement of 54 on the membrane protein bacteriorhodopsin., (Copyright © 2012 Elsevier Inc. All rights reserved.)

Applications of high-power Terahertz (THz) sources require low-loss transmission lines to minimize loss, prevent overheating and preserve the purity of the transmission mode. Concepts for THz transmission lines are reviewed with special emphasis on overmoded, metallic, corrugated transmission lines. Using the fundamental HE(11) mode, these transmission lines have been successfully implemented with very low-loss at high average power levels on plasma heating experiments and THz dynamic nuclear polarization (DNP) nuclear magnetic resonance (NMR) experiments. Loss in these lines occurs directly, due to ohmic loss in the fundamental mode, and indirectly, due to mode conversion into high order modes whose ohmic loss increases as the square of the mode index. An analytic expression is derived for ohmic loss in the modes of a corrugated, metallic waveguide, including loss on both the waveguide inner surfaces and grooves. Simulations of loss with the numerical code HFSS are in good agreement with the analytic expression. Experimental tests were conducted to determine the loss of the HE(11) mode in a 19 mm diameter, helically-tapped, three meter long brass waveguide with a design frequency of 330 GHz. The measured loss at 250 GHz was 0.029 ± 0.009 dB/m using a vector network analyzer approach and 0.047 ± 0.01 dB/m using a radiometer. The experimental results are in reasonable agreement with theory. These values of loss, amounting to about 1% or less per meter, are acceptable for the DNP NMR application. Loss in a practical transmission line may be much higher than the loss calculated for the HE(11) mode due to mode conversion to higher order modes caused by waveguide imperfections or miter bends.

This work focuses on the accuracy of the mode content measurements in an overmoded corrugated waveguide using measured radiated field patterns. Experimental results were obtained at 250 GHz using a vector network analyzer with over 70 dB of dynamic range. The intensity and phase profiles of the fields radiated from the end of the 19 mm diameter helically tapped brass waveguide were measured on planes at 7, 10, and 13 cm from the waveguide end. The measured fields were back propagated to the waveguide aperture to provide three independent estimates of the field at the waveguide exit aperture. Projecting that field onto the modes of the guide determined the waveguide mode content. The three independent mode content estimates were found to agree with one another to an accuracy of better than ±0.3%. These direct determinations of the mode content were compared with indirect measurements using the experimentally measured amplitude in three planes, with the phase determined by a phase retrieval algorithm. The phase retrieval technique using the planes at 7, 10, and 13 cm yielded a mode content estimate in excellent agreement, within 0.3%, of the direct measurements. Phase retrieval results using planes at 10, 20, and 30 cm were less accurate due to truncation of the measurement in the transverse plane. The reported measurements benefited greatly from a precise mechanical alignment of the scanner with respect to the waveguide axis. These results will help to understand the accuracy of mode content measurements made directly in cold test and indirectly in hot test using the phase retrieval technique.

Dynamic nuclear polarization (DNP) increases the sensitivity of nuclear magnetic resonance (NMR) spectroscopy by using high frequency microwaves to transfer the polarization of the electrons to the nuclear spins. The enhancement in NMR sensitivity can amount to a factor of well above 100, enabling faster data acquisition and greatly improved NMR measurements. With the increasing magnetic fields (up to 23 T) used in NMR research, the required frequency for DNP falls into the THz band (140-600 GHz). Gyrotrons have been developed to meet the demanding specifications for DNP NMR, including power levels of tens of watts; frequency stability of a few megahertz; and power stability of 1% over runs that last for several days to weeks. Continuous gyrotron frequency tuning of over 1 GHz has also been demonstrated. The complete DNP NMR system must include a low loss transmission line; an optimized antenna; and a holder for efficient coupling of the THz radiation to the sample. This paper describes the DNP NMR process and illustrates the THz systems needed for this demanding spectroscopic application. THz DNP NMR is a rapidly developing, exciting area of THz science and technology.

We present a calculation of the microwave field distribution in a magic angle spinning (MAS) probe utilized in dynamic nuclear polarization (DNP) experiments. The microwave magnetic field (B(1S)) profile was obtained from simulations performed with the High Frequency Structure Simulator (HFSS) software suite, using a model that includes the launching antenna, the outer Kel-F stator housing coated with Ag, the RF coil, and the 4mm diameter sapphire rotor containing the sample. The predicted average B(1S) field is 13μT/W(1/2), where S denotes the electron spin. For a routinely achievable input power of 5W the corresponding value is γ(S)B(1S)=0.84MHz. The calculations provide insights into the coupling of the microwave power to the sample, including reflections from the RF coil and diffraction of the power transmitted through the coil. The variation of enhancement with rotor wall thickness was also successfully simulated. A second, simplified calculation was performed using a single pass model based on Gaussian beam propagation and Fresnel diffraction. This model provided additional physical insight and was in good agreement with the full HFSS simulation. These calculations indicate approaches to increasing the coupling of the microwave power to the sample, including the use of a converging lens and fine adjustment of the spacing of the windings of the RF coil. The present results should prove useful in optimizing the coupling of microwave power to the sample in future DNP experiments. Finally, the results of the simulation were used to predict the cross effect DNP enhancement (ϵ) vs. ω(1S)/(2π) for a sample of (13)C-urea dissolved in a 60:40 glycerol/water mixture containing the polarizing agent TOTAPOL; very good agreement was obtained between theory and experiment., (Copyright © 2011 Elsevier Inc. All rights reserved.)

An experimental study of picosecond pulse amplification in a gyrotron-traveling wave tube (gyro-TWT) has been carried out. The gyro-TWT operates with 30 dB of small signal gain near 140 GHz in the HE₀₆ mode of a confocal waveguide. Picosecond pulses show broadening and transit time delay due to two distinct effects: the frequency dependence of the group velocity near cutoff and gain narrowing by the finite gain bandwidth of 1.2 GHz. Experimental results taken over a wide range of parameters show good agreement with a theoretical model in the small signal gain regime. These results show that in order to limit the pulse broadening effect in gyrotron amplifiers, it is crucial to both choose an operating frequency at least several percent above the cutoff of the waveguide circuit and operate at the center of the gain spectrum with sufficient gain bandwidth.

This contribution addresses four potential misconceptions associated with high-resolution dynamic nuclear polarization/magic angle spinning (DNP/MAS) experiments. First, spectral resolution is not generally compromised at the cryogenic temperatures at which DNP experiments are performed. As we demonstrate at a modest field of 9 T (380 MHz (1)H), 1 ppm linewidths are observed in DNP/MAS spectra of a membrane protein in its native lipid bilayer, and <0.4 ppm linewidths are reported in a crystalline peptide at 85 K. Second, we address the concerns about paramagnetic broadening in DNP/MAS spectra of proteins by demonstrating that the exogenous radical polarizing agents utilized for DNP are distributed in the sample in such a manner as to avoid paramagnetic broadening and thus maintain full spectral resolution. Third, the enhanced polarization is not localized around the polarizing agent, but rather is effectively and uniformly dispersed throughout the sample, even in the case of membrane proteins. Fourth, the distribution of polarization from the electron spins mediated via spin diffusion between (1)H-(1)H strongly dipolar coupled spins is so rapid that shorter magnetization recovery periods between signal averaging transients can be utilized in DNP/MAS experiments than in typical experiments performed at ambient temperature.

Dynamic Nuclear Polarization (DNP) experiments transfer polarization from electron spins to nuclear spins with microwave irradiation of the electron spins for enhanced sensitivity in nuclear magnetic resonance (NMR) spectroscopy. Design and testing of a spectrometer for magic angle spinning (MAS) DNP experiments at 263 GHz microwave frequency, 400 MHz (1)H frequency is described. Microwaves are generated by a novel continuous-wave gyrotron, transmitted to the NMR probe via a transmission line, and irradiated on a 3.2 mm rotor for MAS DNP experiments. DNP signal enhancements of up to 80 have been measured at 95 K on urea and proline in water-glycerol with the biradical polarizing agent TOTAPOL. We characterize the experimental parameters affecting the DNP efficiency: the magnetic field dependence, temperature dependence and polarization build-up times, microwave power dependence, sample heating effects, and spinning frequency dependence of the DNP signal enhancement. Stable system operation, including DNP performance, is also demonstrated over a 36 h period.

The design, operation, and characterization of a continuous-wave (CW) tunable second-harmonic 460-GHz gyrotron are reported. The gyrotron is intended to be used as a submillimeter-wave source for 700-MHz nuclear magnetic resonance experiments with sensitivity enhanced by dynamic nuclear polarization. The gyrotron operates in the whispering-gallery mode TE 11,2 and has generated 16 W of output power with a 13-kV 100-mA electron beam. The start oscillation current measured over a range of magnetic field values is in good agreement with theoretical start currents obtained from linear theory for successive high-order axial modes TE 11,2,q . The minimum start current is 27 mA. Power and frequency tuning measurements as a function of the electron cyclotron frequency have also been carried out. A smooth frequency tuning range of 1 GHz was obtained for the operating second-harmonic mode either by magnetic field tuning or beam voltage tuning. Long-term CW operation was evaluated during an uninterrupted period of 48 h, where the gyrotron output power and frequency were kept stable to within ±0.7% and ±6 ppm, respectively, by a computerized control system. Proper operation of an internal quasi-optical mode converter implemented to transform the operating whispering-gallery mode to a Gaussian-like beam was also verified. Based on the images of the gyrotron output beam taken with a pyroelectric camera, the Gaussian-like mode content of the output beam was computed to be 92% with an ellipticity of 12%.

We describe a cryogenic sample exchange system that dramatically improves the efficiency of magic angle spinning (MAS) dynamic nuclear polarization (DNP) experiments by reducing the time required to change samples and by improving long-term instrument stability. Changing samples in conventional cryogenic MAS DNP/NMR experiments involves warming the probe to room temperature, detaching all cryogenic, RF, and microwave connections, removing the probe from the magnet, replacing the sample, and reversing all the previous steps, with the entire cycle requiring a few hours. The sample exchange system described here-which relies on an eject pipe attached to the front of the MAS stator and a vacuum jacketed dewar with a bellowed hole-circumvents these procedures. To demonstrate the excellent sensitivity, resolution, and stability achieved with this quadruple resonance sample exchange probe, we have performed high precision distance measurements on the active site of the membrane protein bacteriorhodopsin. We also include a spectrum of the tripeptide N-f-MLF-OH at 100K which shows 30 Hz linewidths.

The theory, design, and experimental results of a wideband 140-GHz 1-kW pulsed gyro-traveling-wave amplifier (gyro-TWA) are presented. The gyro-TWA operates in the HE(06) mode of an overmoded quasi-optical waveguide using a gyrating electron beam. The electromagnetic theory, interaction theory, design processes, and experimental procedures are described in detail. At 37.7 kV and a 2.7-A beam current, the experiment has produced over 820 W of peak power with a -3-dB bandwidth of 0.8 GHz and a linear gain of 34 dB at 34.7 kV. In addition, the amplifier produced a -3-dB bandwidth of over 1.5 GHz (1.1%) with a peak power of 570 W from a 38.5-kV 2.5-A electron beam. The electron beam is estimated to have a pitch factor of 0.55-0.6, a radius of 1.9 mm, and a calculated perpendicular momentum spread of approximately 9%. The gyro-amplifier was nominally operated at a pulselength of 2 μs but was tested to amplify pulses as short as 4 ns with no noticeable pulse broadening. Internal reflections in the amplifier were identified using these short pulses by time-domain reflectometry. The demonstrated performance of this amplifier shows that it can be applied to dynamic nuclear polarization and electron paramagnetic resonance spectroscopy.

Millimeter-wave components were re-examined for high power (Mega-Watt) and steady-state (greater than one hour) operation. Some millimeter-wave components, including waveguide joints, vacuum pumping sections, power monitors, sliding waveguides, and injection windows, have been improved for high power CW (Continuous Waves) transmission. To improve transmission efficiency, information about the wave phase and mode content of high power millimeter-waves propagating in corrugated waveguides, which are difficult to measure directly, were obtained by a newly developed method based on retrieved phase information. To optimize the plasma heating efficiency, a proof-of-principle study of the injection polarization feedback control was performed in the low power test stand.

We report the measurement of small losses in transmission line (TL) components intended for high-power millimeter-wave applications. Measurements were made using two different low-power techniques: a coherent technique using a vector network analyzer (VNA) and an incoherent technique using a radiometer. The measured loss in a 140 GHz 12.7 mm diameter TL system, consisting of 1.7 m of circular corrugated waveguide and three miter bends, is dominated by the miter bend loss. The measured loss was 0.3±0.1 dB per miter bend using a VNA; and 0.22±0.1 dB per miter bend using a radiometer. Good agreement between the two measurement techniques implies that both are useful for measuring small losses. To verify the methodology, the VNA technique was employed to measure the extremely small transmission loss in a 170 GHz ITER prototype TL system consisting of three lengths of 1 m, 63.5 mm diameter, circular corrugated waveguide and two miter bends. The measured loss of 0.05±0.02 dB per miter bend may be compared with the theoretical loss of 0.027 dB per miter bend. These results suggest that low-power testing of TL losses, utilizing a small, simple TL system and a VNA, is a reliable method for evaluating performance of low-loss millimeter-wave TL components intended for use in high-power applications.

Dynamic nuclear polarization (DNP) results in a substantial nuclear polarization enhancement through a transfer of the magnetization from electrons to nuclei. Recent years have seen considerable progress in the development of DNP experiments directed towards enhancing sensitivity in biological nuclear magnetic resonance (NMR). This review covers the applications, hardware, polarizing agents, and theoretical descriptions that were developed at the Francis Bitter Magnet Laboratory at Massachusetts Institute of Technology for high-field DNP experiments. In frozen dielectrics, the enhanced nuclear polarization developed in the vicinity of the polarizing agent can be efficiently dispersed to the bulk of the sample via (1)H spin diffusion. This strategy has been proven effective in polarizing biologically interesting systems, such as nanocrystalline peptides and membrane proteins, without leading to paramagnetic broadening of the NMR signals. Gyrotrons have been used as a source of high-power (5-10 W) microwaves up to 460 GHz as required for the DNP experiments. Other hardware has also been developed allowing in situ microwave irradiation integrated with cryogenic magic-angle-spinning solid-state NMR. Advances in the quantum mechanical treatment are successful in describing the mechanism by which new biradical polarizing agents yield larger enhancements at higher magnetic fields. Finally, pulsed methods and solution experiments should play a prominent role in the future of DNP.

Dynamic nuclear polarization (DNP) is a method that permits NMR signal intensities of solids and liquids to be enhanced significantly, and is therefore potentially an important tool in structural and mechanistic studies of biologically relevant molecules. During a DNP experiment, the large polarization of an exogeneous or endogeneous unpaired electron is transferred to the nuclei of interest (I) by microwave (microw) irradiation of the sample. The maximum theoretical enhancement achievable is given by the gyromagnetic ratios (gamma(e)gamma(l)), being approximately 660 for protons. In the early 1950s, the DNP phenomenon was demonstrated experimentally, and intensively investigated in the following four decades, primarily at low magnetic fields. This review focuses on recent developments in the field of DNP with a special emphasis on work done at high magnetic fields (> or =5 T), the regime where contemporary NMR experiments are performed. After a brief historical survey, we present a review of the classical continuous wave (cw) DNP mechanisms-the Overhauser effect, the solid effect, the cross effect, and thermal mixing. A special section is devoted to the theory of coherent polarization transfer mechanisms, since they are potentially more efficient at high fields than classical polarization schemes. The implementation of DNP at high magnetic fields has required the development and improvement of new and existing instrumentation. Therefore, we also review some recent developments in microw and probe technology, followed by an overview of DNP applications in biological solids and liquids. Finally, we outline some possible areas for future developments.

We report the observation of two-dimensional plasma filamentary arrays with more than 100 elements generated during breakdown of air at atmospheric pressure by a focused Gaussian beam from a 1.5-MW, 110-GHz gyrotron operating in 3-micros pulses. Each element is a plasma filament elongated in the electric field direction and regularly spaced about one-quarter wavelength apart in the plane perpendicular to the electric field. The development of the array is explained as a result of diffraction of the beam around the filaments, leading to the sequential generation of high intensity spots, at which new filaments are created, about a quarter wavelength upstream from each existing filament. Electromagnetic wave simulations corroborate this explanation and show very good correlation to the observed pattern of filaments.

In this paper, we describe a 250 GHz gyrotron oscillator, a critical component of an integrated system for magic angle spinning (MAS) dynamic nuclear polarization (DNP) experiments at 9T, corresponding to 380 MHz (1)H frequency. The 250 GHz gyrotron is the first gyro-device designed with the goal of seamless integration with an NMR spectrometer for routine DNP enhanced NMR spectroscopy and has operated under computer control for periods of up to 21 days with a 100% duty cycle. Following a brief historical review of the field, we present studies of the membrane protein bacteriorhodopsin (bR) using DNP enhanced multidimensional NMR. These results include assignment of active site resonances in [U-(13)C, (15)N]-bR and demonstrate the utility of DNP for studies of membrane proteins. Next, we review the theory of gyro-devices from quantum mechanical and classical viewpoints and discuss the unique considerations that apply to gyrotron oscillators designed for DNP experiments. We then characterize the operation of the 250 GHz gyrotron in detail, including its long-term stability and controllability. We have measured the spectral purity of the gyrotron emission using both homodyne and heterodyne techniques. Radiation intensity patterns from the corrugated waveguide that delivers power to the NMR probe were measured using two new techniques to confirm pure mode content: a thermometric approach based on the temperature-dependent color of liquid crystalline media applied to a substrate and imaging with a pyroelectric camera. We next present a detailed study of the mode excitation characteristics of the gyrotron. Exploration of the operating characteristics of several fundamental modes reveals broadband continuous frequency tuning of up to 1.8 GHz as a function of the magnetic field alone, a feature that may be exploited in future tunable gyrotron designs. Oscillation of the 250 GHz gyrotron at the second harmonic of cyclotron resonance begins at extremely low beam currents (as low 12 mA) at frequencies between 320 and 365 GHz, suggesting an efficient route for the generation of even higher frequency radiation. The low starting currents were attributed to an elevated cavity Q, which is confirmed by cavity thermal load measurements. We conclude with an appendix containing a detailed description of the control system that safely automates all aspects of the gyrotron operation.

Gyrotrons operating in the millimeter and submillimeter wavelength ranges are the promising sources for applications that are requiring good spectral characteristics and a wide range of output power. We report the precise measurement results of gyrotron spectra. Experiments were conducted using a 140-GHz long-pulse gyrotron that is developed for the dynamic nuclear polarization/nuclear-magnetic-resonance spectroscopy at the Massachusetts Institute of Technology. Transient downshift of the frequency by 12 MHz with a time constant of 3 s was observed. After reaching equilibrium, the frequency was maintained within 1 ppm for over 20 s. The coefficient of the frequency change with cavity temperature was -2.0 MHz/K, which shows that fine tuning of the gyrotron frequency is plausible by cavity-temperature control. Frequency pulling by the beam current was observed, but it was shown to be masked by the downward shift of the gyrotron frequency with temperature. The linewidth was measured to be much less than 1 MHz at 60 dB relative to the carrier power [in decibels relative to carrier (dBc)] and 4.3 MHz at 75 dBc, which is the largest dynamic range to date for the measurement of gyrotron linewidth to our knowledge.

The gyrotron oscillator is a source of high average power millimeter-wave through terahertz radiation. In this paper, we report low beam power and high-efficiency operation of a tunable gyrotron oscillator at 233 GHz. The low-voltage operating mode provides a path to further miniaturization of the gyrotron through reduction in the size of the electron gun, power supply, collector, and cooling system, which will benefit industrial and scientific applications requiring portability. Detailed studies of low-voltage operation in the TE(2) (,) (3) (,) (1) mode reveal that the mode can be excited with less than 7 W of beam power at 3.5 kV. During CW operation with 3.5-kV beam voltage and 50-mA beam current, the gyrotron generates 12 W of RF power at 233.2 GHz. The EGUN electron optics code describes the low-voltage operation of the electron gun. Using gun-operating parameters derived from EGUN simulations, we show that a linear theory adequately predicts the low experimental starting currents.

The effect of spatial dispersion on the electromagnetic properties of a metamaterial consisting of a three-dimensional mesh of crossing metallic wires is reported. The effective dielectric permittivity tensor epsilon(ij)(omega, k) of the wire mesh is calculated in the limit of small wavenumbers. The procedure for extracting the spatial dispersion from the omega versus k dependence for electromagnetic waves propagating in the bulk of the metamaterial is developed. These propagating modes are identified as similar to the longitudinal (plasmon) and transverse (photon) waves in a plasma. Spatial dispersion is found to have the most dramatic effect on the surface waves that exist at the wire mesh-vacuum interface.