Dynamic nuclear polarization at 9T using a novel 250 GHz gyrotron microwave source. 2003

In this communication, we report enhancements of nuclear spin polarization by dynamic nuclear polarization (DNP) in static and spinning solids at a magnetic field strength of 9 T (250 GHz for g = 2 electrons, 380 MHz for ¹H). In these experiments, ¹H enhancements of up to 170 ± 50 have been observed in 1-¹³C-glycine dispersed in a 60:40 glycerol/water matrix at temperatures of 20 K; in addition, we have observed significant enhancements in ¹⁵N spectra of unoriented pf1-bacteriophage. Finally, enhancements of ∼17 have been obtained in two-dimensional ¹³C–¹³C chemical shift correlation spectra of the amino acid U–¹³C, ¹⁵N-proline during magic angle spinning (MAS), demonstrating the stability of the DNP experiment for sustained acquisition and for quantitative experiments incorporating dipolar recoupling. In all cases, we have exploited the thermal mixing DNP mechanism with the nitroxide radical 4-amino-TEMPO as the paramagnetic dopant. These are the highest frequency DNP experiments performed to date and indicate that significant signal enhancements can be realized using the thermal mixing mechanism even at elevated magnetic fields. In large measure, this is due to the high microwave power output of the 250 GHz gyrotron oscillator used in these experiments.     

Dynamic nuclear polarization at 9T using a novel 250GHz gyrotron microwave source

In this communication, we report enhancements of nuclear spin polarization by dynamic nuclear polarization (DNP) in static and spinning solids at a magnetic field strength of 9T (250 GHz for g=2 electrons, 380 MHz for 1H). In these experiments, 1H enhancements of up to 170+/-50 have been observed in 1-13C-glycine dispersed in a 60:40 glycerol/water matrix at temperatures of 20K; in addition, we have observed significant enhancements in 15N spectra of unoriented pf1-bacteriophage. Finally, enhancements of approximately 17 have been obtained in two-dimensional 13C-13C chemical shift correlation spectra of the amino acid U-13C, 15N-proline during magic angle spinning (MAS), demonstrating the stability of the DNP experiment for sustained acquisition and for quantitative experiments incorporating dipolar recoupling. In all cases, we have exploited the thermal mixing DNP mechanism with the nitroxide radical 4-amino-TEMPO as the paramagnetic dopant. These are the highest frequency DNP experiments performed to date and indicate that significant signal enhancements can be realized using the thermal mixing mechanism even at elevated magnetic fields. In large measure, this is due to the high microwave power output of the 250 GHz gyrotron oscillator used in these experiments.     

Development of 394.6 GHz CW Gyrotron (Gyrotron FU CW II) for DNP/Proton-NMR at 600 MHz

Gyrotron FU CW II with an 8 T liquid He free superconducting magnet, the second gyrotron of the THz Gyrotron FU CW Series, has been constructed and the operation test was successfully carried out. It will be used for enhancing the sensitivity of 600 MHz proton-NMR by use of Dynamic Nuclear Polarization (DNP). The designed operation mode of the gyrotron is TE_2,6 at the second harmonic. The corresponding frequency is 394.6 GHz. The real operation frequency is 394.3 GHz at TE₀₆ mode, because of fabrication error of the diameter of the cavity. The operation is in complete CW at the output power of around 30 W or higher at the TE₀₆ cavity mode. There are many other operation modes at the fundamental and the second harmonic. Typical output power of the fundamental and the second harmonic are higher than 100 W and 20 W, respectively. The highest frequency observed up to the present is 443.5 GHz at the second harmonic operation of TE_6,5 mode. The measured results are compared with the theoretical consideration.     

Towards 0.99999 28Si

A new approach for producing high-purity silicon with isotopic enrichment of ²⁸Si isotope is reported. The methods of centrifugal enrichment were modified to obtain the initial gaseous silicon tetrafluoride with a record-breaking enrichment of 0.99999664(11) with respect to ²⁸Si. The effective conversion of silicon tetrafluoride into elementary silicon with minimal isotopic dilution was achieved in an electron cyclotron resonance discharge plasma, sustained by gyrotron microwave radiation with a frequency of 24 GHz. We have experimentally demonstrated the deposition of the layers of microcrystalline ²⁸Si with enrichment of 0.999986 ± 0.000003, which is the best result at the present time.     

H DNP at 1.4 T of Water Doped with a Triarylmethyl-Based Radical

Recently a triarylmethyl-based (TAM) radical has been developed for research in biological and other aqueous systems, and in low magnetic fields, 10 mT or less, large ¹H dynamic nuclear polarization (DNP) enhancements have been reported. In this paper the DNP properties of this radical have been investigated in a considerably larger field of 1.4 T, corresponding to proton and electron Larmor frequencies of 60 MHz and 40 GHz, respectively. To avoid excessive microwave heating of the sample, an existing DNP NMR probe was modified with a screening coil, wound around the sample capillary and with its axis perpendicular to the electric component of the microwave field. It was found that with this probe the temperature increase in the sample after 4 s of microwave irradiation with an incident power of 10 W was only 16°C. For the investigations, 10 mM of the TAM radical was dissolved in deionized, but not degassed, water and put into a 1-mm i.d. and 6-mm long capillary tube. At 26°C the following results were obtained: (I) The relaxivity of the radical is 0.07 (mMs)⁻¹, in accordance with the value extrapolated from low-field results; (II) The leakage factor is 0.63, the saturation factor at maximum power is 0.85, and the coupling factor is −0.0187. It is shown that these results agree very well with an analysis where the electron–dipolar interactions are the dominant DNP mechanism, and where the relaxation transitions resulting from these interactions are governed by translational diffusion of the water molecules. Finally, the possibilities of combining DNP with magnetic resonance microscopy (MRM) are discussed. It is shown that at 26°C the overall DNP-enhanced proton polarization should become maximal in an external field of 0.3 T and become comparable to the thermal equilibrium polarization in a field of 30 T, considerably larger than the largest high-resolution magnet available to date. It is concluded that DNP MRM in this field, which corresponds to a standard microwave frequency of 9 GHz, has the potential to significantly increase the sensitivity in NMR and MRI experiments of small aqueous samples doped with the TAM radical.     

INFLUENCE OF MAGNETIC FIELD INHOMOGENEITY ON OPERATION OF THE THz GYROTRON WITH A PULSE MAGNET

Influence of magnetic field tapering on operation of a gyrotron working in the TE _4,12 mode at the second harmonic frequency 1013.67 GHz is investigated. It is found that the existing inhomogeneity of the magnetic field of the order of 0.25%–0.50% in the cavity allows one to achieve higher efficiencies. It improves also mode competition scenario by suppressing oscillations of the two parasitic TE _3,6⁺ and TE _5,5⁻ modes at the fundamental frequencies 513.35 GHz and 503.64 GHz, respectively.     

Detailed Consideration of Experimental Results of Gyrotron FU CW II Developed as a Radiation Source for DNP-NMR Spectroscopy

A CW gyrotron for the sensitivity enhancement of NMR spectroscopy through dynamic nuclear polarization has been designed. The gyrotron operates at the second harmonic and frequency of 394.6 GHz with the main operating mode TE_0,6. Operating conditions of other neighboring cavity modes such as TE_2,6 at frequency of 392.6 GHz and TE_2,3 at frequency of 200.7 GHz were also considered. The experimental conditions of the gyrotron at low and high voltages are simulated. The output power of 56 watts corresponds to the efficiency of 2 percent at low voltage operation and frequency of 394.6 GHz is expected.     

Operational Characteristics of a 14-W 140-GHz Gyrotron for Dynamic Nuclear Polarization

The operating characteristics of a 140-GHz 14-W long pulse gyrotron are presented. The device is being used in dynamic nuclear polarization enhanced nuclear magnetic resonance (DNP/NMR) spectroscopy experiments. The gyrotron yields 14 W peak power at 139.65 GHz from the TE(0,3) operating mode using a 12.3-kV 25-mA electron beam. Additionally, up to 12 W peak has been observed in the TE(2,3) mode at 136.90 GHz. A series of mode converters transform the TE(0,3) operating mode to the TE(1,1) mode. Experimental results are compared with nonlinear simulations and show reasonable agreement. The millimeter-wave output beam was imaged in a single shot using a pyroelectric camera. The mode patterns matched reasonably well to theory for both the TE(0,1) mode and the TE(1,1) mode. Repeatable mode patterns were obtained at intervals ranging from 0.8 s apart to 11 min apart at the output of the final mode converter.     

Towards a 1 MW, 170 GHz gyrotron design for fusion application

The electrical design of different components of 1 MW, 170 GHz gyrotron such as, magnetron injection gun, cylindrical interaction cavity and collector and RF window is presented in this article. Recently, a new project related to the development of 170 GHz, 1 MW gyrotron has been started for the Indian Tokamak. TE_34,10 mode is selected as the operating mode after studied the problem of mode competition. The triode type geometry is selected for the design of magnetron injection gun (MIG) to achieve the required beam parameters. The maximum transverse velocity spread of 3.28% at the velocity ratio of 1.34 is obtained in simulations for a 40 A, 80 kV electron beam. The RF output power of more than 1 MW with 36.5% interaction efficiency without depressed collector is predicted by simulation in single-mode operation at 170 GHz frequency. The simulated single-stage depressed collector of the gyrotron predicted the overall device efficiencies >55%. Due to the very good thermal conductivity and very weak dependency of the dielectric parameters on temperature, PACVD diamond is selected for window design for the transmission of RF power. The in-house developed code MIGSYN and GCOMS are used for initial geometry design of MIG and mode selection respectively. Commercially available simulation tools MAGIC and ANSYS are used for beam–wave interaction and mechanical analysis respectively.     

D-band frequency step-tuning of A 1 MW gyrotron using a brewster output window

In order to demonstrate the usability of gyrotron oscillators as frequency step tunable high power millimeter-wave sources, experiments on a 1 MW, 140 GHz TE_22,6 gyrotron with a built-in quasi-optical (q. o.) mode converter have been performed. By varying the operating parameters of the tube, a series of oscillations in the frequency range from 114 GHz to 166 GHz were excited. To avoid reflections, caused by the required vacuum barrier window, the gyrotron was equipped with a Brewster window. The achieved output power levels between 0.85 and 1.05 MW are compared to measurements carried out with the same tube using a conventional single-disk window. These experiments showed that even by using a q. o. mode converter, the influence of window reflections on the gyrotron oscillatory behavior cannot be removed completely.     

Investigation of a Broadband Quasi-Optical Mode Converter for a Multi-Frequency 1 MW Gyrotron

A broadband quasi-optical (QO) mode converter for a multi-frequency gyrotron has been designed and tested at Forschungszentrum Karlsruhe (FZK). The launcher is optimized for the TE_22,8 mode at 140 GHz, but the radiated beams present an almost identically focused pattern for all 9 considered modes between 105 GHz (TE_17,6) and 143 GHz (TE_23,8). Combining with a beam-forming mirror system, which consists of a quasi-elliptical mirror and two phase-correcting mirrors with non-quadratic surface contour, further calculations show that efficiencies of more than 94% have been achieved for converting the rotating high-order cylindrical cavity modes into the usable fundamental Gaussian mode. Low power (cold) measurements show a good agreement with theoretical predictions. This QO mode converter can be used for the broadband operation of a multi-frequency 1 MW gyrotron.     

Design of a RF window for 170 GHz, 1 MW gyrotron for ECRH application

This paper describes the design of a large sized diamond window for 1 MW, 170 GHz gyrotron. The diameter and the thickness of the diamond window are 80 mm and 1.482 mm, respectively, whose edge is directly cooled by water. The CST microwave studio has been used for the S-parameter, and finite element analysis code ANSYS has been used for the thermal and the structural simulation. The return loss (S₁₁) and insertion loss (S₂₁) of the 170 GHz gyrotron window have been found −39.80 dB and −0.011 dB, respectively. The thermal and structural analysis of RF window the 397 K temperature at disk center and maximum displacement 0.01 mm has been found in the window disk during the thermal analysis.     

Temperature Dependence of the Proton Overhauser DNP Enhancements on Aqueous Solutions of Fremy’s Salt Measured in a Magnetic Field of 9.2?T

The temperature dependence of the water-proton dynamic nuclear polarization (DNP) enhancement from Fremy’s salt nitroxide radicals was measured in a magnetic field of 9.2?T (corresponding to 260?GHz microwave (MW) and 392?MHz NMR frequencies) in the temperature range of 15–65?°C. The temperature could be determined directly from the proton NMR line shift of the sample. Very high DNP enhancements of ?38 (signal integral) or ?81 (peak intensity) could be achieved with a high-power gyrotron MW source. The experimental findings are compared with classical Overhauser theory for liquids, which is based on the translational and rotational motion of the molecules and with molecular dynamics calculations of the coupling factor.     

Electron Gun for Powerful Short Pulse Gyrotron with Operating Magnetic Field 8 T

High power short pulse gyrotron with operating frequency 395 GHz operating on the second cyclotron harmonic is now under developing at FIR FU. The gyrotron is planned to use in future experiments for plasma diagnostics. For this purpose the output power about 100 kW and pulse duration 100 ns at least are needed. Preliminary estimations of parameters of some versions of the electron guns with accelerating potential U₀= 70-100 kV were performed. Possibilities of non-adiabatic as well as adiabatic guns were considered. It was shown that non-adiabatic system is not reliable for such rather low value of U₀, the adiabatic magnetron injection gun (MIG) is more preferable for the gyrotron design. Analytical estimations of the suitable MIG dimensions and operating regime to form good quality electron beam were fulfilled. Numerical optimization of the gun shape and position was performed. It was shown that in spite of the extremely big ratio of the operating current (I₀= 18 A) to the Langmuir current of the gun, close to 0.4-0.5, the suggested MIG can form the helical electron beam (HEB) which is suitable for gyrotron operation properties.     

A 100 kW, 140 GHz pulsed gyrotron

The design and operation of a 100 kW, 140 GHz pulsed gyrotron are reported. To our knowledge, this is the highest frequency at which high gyrotron output power (>-100 kW) has been achieved. Results are presented for gyrotron operation in the range of magnetic field from 4 to 7 T, voltage from 23 to 80 kV and current up to 7.5 A. Near a value of magnetic field of 5.4 T, and output power of 100 kW was obtained at 140.4 GHz in single mode operation in the TE₀₃₁ resonator mode.     

Low-Field, Time-Resolved Dynamic Nuclear Polarization with Field Cycling and High-Resolution NMR Detection

Dynamic nuclear polarization (DNP) effects in aqueous solutions of stable 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPOL) radicals were studied in a pulsed mode of pumping the electron paramagnetic resonance (EPR) transitions. Our fast field cycling setup allowed us to perform the EPR pumping at low magnetic fields and to detect the enhanced nuclear magnetic resonance signals at 7 T with high spectral resolution. Pumping was performed at two different frequencies, 300 MHz and 1.4 GHz, corresponding to magnetic fields around 10 and 48.6 mT, respectively. For both frequencies, the DNP enhancements were close to the limiting theoretical values of ?110 (¹⁴N TEMPOL) and ?165 (¹⁵N TEMPOL). Our pulsed experiments exploit coherent motion of the electronic spins in the radio-frequency field as seen by an oscillatory component in the dependence of the DNP effect on the radio-frequency pulse duration. The DNP enhancement was studied in detail as a function of the pulse length, duty cycle, delay between the pulses, and applied power. The analysis of the results shows that pulsed DNP experiments provide an opportunity to achieve enhancements of about ?110 with relatively low applied power as compared to the standard continuous-wave DNP experiments. An adequate theoretical approach to the problem under study is suggested.     

全三维110GHz和220GHz同轴腔双注回旋管数值模拟研究

为了打破传统单注回旋管只能产生较低功率的局限性, 本文基于自主研发的PIC粒子模拟软件CHIPIC 对110 GHz和220 GHz同轴腔双注回旋管进行全三维数值模拟研究. 在理论分析同轴双电子注电子枪设计模型和初始参数的基础上通过CHIPIC对其进行优化设计, 得到了具有横纵速度比为1.0, 最大速度零散约为5.4%的高性能电子束; 并将此优化后的双阳极双注电子枪取代传统回旋管数值模拟时采用的回旋 发射进行110 GHz和220 GHz双注回旋管整管的数值模拟, 并采用MPI四进程并行计算, 最终获得了具有双频分别为110 GHz和220 GHz、模式为TE₀₂模、平均输出功率约在70 kW、 效率达到8.75%的高性能双注回旋振荡管. 关键词： 同轴腔双注回旋管 同轴双电子注电子枪 横纵速度比 速度零散     

电子束注入简单磁镜中被电子迴旋共振加热捕获的实验研究

在简单磁镜MM-2中,在采用15GHz大功率迴旋管进行电子迴旋共振加热(ECRH)的同时,以不同的方式向磁镜中注入电子束,进行了ECRH捕获电子束的实验研究。结果表明:由于电子束的提前注入,等离子体的预电离时间被大大地缩短。由上ECRH对电子束的捕获,使得热电子环参数得到很大的改善,热电子环的反磁β值约增加62%,对应反磁增加的捕获效率约为(30—40)%。在迴旋管输出约30kW的条件下,适应建立热电环的气体压力窗为(4.67—21.3)×10^-4Pa。 关键词：     

High-power oscillator of continuous electromagnetic radiation with a frequency of 300 GHz

We consider a general concept of construction, the possible versions, and specific features of a gyrotron, whose output power in CW oscillation regime can reach a few kilowatts at a frequency of 300 GHz. The gyrotron is designed for work in a high-frequency facility in combination with a “dry” cryomagnet, which ensures a magnetic field of up to 12 T, required for the gyrotron operation. The basic results of numerical simulation and optimization of the electron gun, the resonant cavity, and other subsystems of the gyrotron are presented. The designs used for the gyrotron development are justified. Preliminary experiments showed the efficiency of the pilotproduction gyrotron with an output power of about 2 kW, which is record-breaking in this frequency range. __________ Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Radiofizika, Vol. 50, No. 6, pp. 461–470, June 2007.