Electron paramagnetic resonance spectrometre

FIELD: physics.

SUBSTANCE: electron paramagnetic resonance spectrometre has a microwave generator (1) in the 90-100 GHz range, a microwave bridge (20), a system for transmitting microwave power to a sample in form of series-arranged first 3 mm waveguide (2), first horn antenna (3), at least one dielectric lens (4), second horn antenna (5) whose horn faces the horn of the first horn antenna (3), and a second 3 mm waveguide (6). The spectrometre also has a resonator (7), having a piston (8) and sample holder (9), a microwave signal detector (10), a synchronous detector (11), a magnetic field modulation generator (12), modulation coils (13), a magnetic field scan unit (14), a superconducting magnet (15), a cryogenic system (16) for maintaining temperature of liquid helium, having an optical window (17) and a control unit (18). The superconducting magnet (15), modulation coils (13), second horn antenna (5), second 3 mm waveguide (6) and resonator (7) are placed in the cryogenic system (16). The second horn antenna (5) is placed opposite the optical window (17) of the cryogenic system and is connected through the second 3 mm waveguide (5) to the resonator through a coupling aperture. The first horn antenna (3) and at least one dielectric lens (4) are fitted outside the cryogenic system (16) opposite its optical window (17).

EFFECT: reduced heat losses in the cryostat and reduced amount of reflected microwave power.

3 cl, 2 dwg

 

The invention relates to techniques for spectroscopy electron paramagnetic resonance (EPR) and may find application in studies of condensed materials and nanostructures by the EPR method in physics, chemistry, biology and other fields.

Known spectrometer electron paramagnetic resonance (see US patent No. 6504367, IPC G01R 33/60 published 07.01.2003)containing a microwave bridge, comprising a source of microwave radiation, the attenuator and the element for phase-shifting the output of a source of microwave radiation is connected with one arm of the circulator or the T-bridge, the other arm of which is connected to the cavity through the diaphragm connection, the third shoulder is connected to the microwave detector. The output of the microwave detector connected to the input of the synchronous detector, the second input of the specified synchronous detector connected to the output of large amplitude modulator capable of producing a modulation of the field with a large amplitude, not less than 20 Gauss. The second output of the specified modulator connected to the modulation coils, adapted to create a high modulation amplitudes of the field and associated with the resonator. The output of the synchronous detector serves to analog-to-digital Converter (ADC), the output of which is connected to the computer, the resonator is placed in a magnetic field in the center between the poles of a magnet.

The disadvantage of this device is the lack of a cryogenic system and the intercept is aktivnogo solution supply microwave power in such a system, as well as the magnetic system in the form of superconducting solenoids that allow you to create a magnetic field more than 3 Tesla, which is necessary for the observation of EPR spectra in the 3 mm range with frequencies above 90 GHz. For observation of the EPR signal with a typical g-factor g=2 at a frequency of 95 GHz required magnetic field 3,3 TL. The absence of the cryogenic system and magnetic system in the form of superconducting solenoids is not possible to record the EPR signals of the most paramagnetic objects at frequencies above 90 GHz.

Known spectrometer electron paramagnetic resonance (see PCT application no WO 200809136, IPC G01R 33/60 published 31.07.2008), including tools for continuous irradiation of the sample of radio-frequency field, means for application to the sample varying sinusoidally with a rotating magnetic field gradients for spatial encoding means for direct detection of signals from a sample without using a field modulation with continuous irradiation of a sample of radio-frequency radiation. Direct detection tools include sweep sinusoidal varying magnetic field and means of signal processing, including digital signal processor.

A disadvantage of the known device is the absence of cryogenic systems and design solutions supply microwave power in such a system, as well as the magnetic system in the form of superconducting solenoids, allows you to create a magnetic field more than 3 Tesla, which is necessary for the 3 mm range with frequencies above 90 GHz. For observation of the EPR signal with a typical g-factor g=2 at a frequency of 95 GHz required magnetic field 3,3 TL. The absence of the cryogenic system and magnetic system in the form of superconducting solenoids is not possible to record the EPR signals of the most paramagnetic objects at frequencies above 90 GHz.

Known for an EPR spectrometer 3 mm range, manufactured by Bruker (see BRUKER ELEXSIS - Electron Paramagnetic resonance E 600/680 User's Manual, Version 1 26, Written by G.G.Maresch 02.11.2004, Bruker Analytic GmbH, Rheinstetten, Germany), containing the microwave generator channel UHF-band cryogenic system with liquid helium temperature and the superconducting magnet, single-mode resonator, in which is placed the sample and recording system EPR microwave channel.

A disadvantage of the known device is the lack of sensitivity, as it is used long microwave tract (over two meters), including a waveguide system dual-band (3 cm, 3 mm) with appropriate transitions between waveguides, leading to loss of the microwave power and the emergence of multiple reflections at the boundaries of the waveguide system.

Known spectrometer electron paramagnetic resonance (see .J.van der Meer, J.. J..Disselhorst, J.Allgeier, J.Schmidt and W.Th.Wenckebach, Meas. Sci. Technol., 1, p.396-400 (1990), J.A.J..Disselhorst, H.J.van der Meer, O.G.Poluektov, and J.Schmidt, J.Magn.Reson., Ser. A 115, pp.183-188, 1995), which coincides with the proposed technical solution for the greatest number of significant features and adopted for the prototype. The spectrometer prototype includes a generator of ultra-high frequency microwave radiation 3 mm range with a frequency of 94.9 GHz, the transport system of the microwave power to the sample as a combination of waveguides 3 mm, 8 mm and 3 cm bands, the cryogenic system with liquid helium temperature of 2 K, the superconducting magnet system of the optical excitation of the sample in the vertical direction through the bottom window of the cryostat. The device prototype EPR signal recorded on a signal electron spin echo in a microwave channel using the receiver of microwave radiation.

The disadvantage of the spectrometer prototype is a long microwave tract (over two meters), including a waveguide system of three ranges (3 cm, 8 mm, 3 mm) with appropriate transitions between waveguides, leading to loss of the microwave power and the emergence of multiple reflections at the boundaries of the waveguide system. The presence of a waveguide system inevitably leads to significant thermal losses and causes additional difficulties for the manufacture of a heat seal in the additional section of the waveguide from a material with a small teploprovodnost the Y.

The task of the invention was to develop such a spectrometer, electron paramagnetic resonance, which would have reduced heat loss in the cryostat and reduced the amount of reflection of the microwave power.

The problem is solved in that the spectrometer electron paramagnetic resonance comprises a generator of microwave (microwave) range 90-100 GHz, the transport system of the microwave power to the sample, the cavity is equipped with a piston and a holder for the sample, the detector microwave signal, the synchronous detector, the modulation generator magnetic field modulation coil, the scanner's magnetic field, a superconducting magnet cryogenic system to maintain the temperature of liquid helium equipped with an optical window, and the control unit. The transport system of the microwave power to the sample is made in the form of a series set of the first 3 mm of the waveguide, the first horn antenna, at least one dielectric lens, the second horn antenna facing the mouthpiece to the horn first horn antenna, and the second is 3 mm of the waveguide. The cryogenic system posted by the superconducting magnet, the drive coil, the second horn antenna, the second 3 mm waveguide and the resonator. The second horn antenna is installed against the optical window cryogen the first system and a second 3 mm waveguide connected to the resonator through hole connection. The first horn antenna and at least one dielectric lens mounted outside the cryogenic system against the optical window. Generator SHF band is connected to the input of the detector microwave signal, the output of which is connected to the first input of a synchronous detector. Input/output of a synchronous detector connected to the first input/output control unit, and the second input of synchronous detector connected to the first generator output modulation of the magnetic field, the second output of which is connected to the modulation coils. The output control unit connected to the input of the scanner's magnetic field, which is connected with the superconducting magnet.

The inventive spectrometer for measuring photo EPR or registration of optically detected magnetic resonance may contain a light source, optically coupled through a rotating prism or mirror with a communication hole in the resonator.

Dielectric lens in the spectrometer can be performed, for example, PTFE.

The use of high frequency 90-110 GHz can be used in the inventive spectrometer quasi-optical path instead of the waveguide and, thus, to apply a microwave power to the sample directly through the optical window of the cryostat. The use of quasi-optical path ensures the reduction of heat losses is the cryostat and reducing the number of reflections of the microwave power.

The claimed technical solution is illustrated in the drawing, where

figure 1 presents the scheme of the proposed EPR spectrometer,

figure 2 shows the spectrum EPR registered on claimed an EPR spectrometer.

Declare an EPR spectrometer (see figure 1) comprises a generator 1 superhigh-frequency (SHF) range 90-100 GHz (sstf) and transportation system of the microwave power to the sample, made in the form of sequentially installed the first 3 mm of the waveguide 2, the first horn antenna 3, at least one dielectric lens 4, a second horn antenna 5, facing the mouthpiece to the horn first horn antenna 3, and the second is 3 mm of the waveguide 6. The inventive spectrometer also includes a resonator 7, provided with a piston 8 and a holder 9 for the sample, the detector 10 of the microwave signal (LCA), a synchronous detector 11 (DM), the generator 12 modulation of the magnetic field (GMP), modulation coil 13, block 14 sweep of the magnetic field (BRM occupational), superconducting magnet 15, a cryogenic system 16 to maintain the temperature of liquid helium equipped with an optical window 17, and the control unit 13 (BOO). Dielectric lens 4 may be made of Teflon (or other material suitable for focusing microwave radiation). Superconducting magnet 15, the modulation coil 13, the second horn antenna 5, the second 3 mm waveguide 6 and the reason is Thor 7 is placed in the cryogenic system. The second horn antenna 5 is set against the optical window 17 of the cryogenic system and through the second 3 mm waveguide 6 is connected with the cavity 7 through the communication hole 19. The configuration of the cavity 7 to the frequency of the microwave power produced by the piston 6, which serves as the bottom wall of the cavity 7. The first horn antenna 3 and at least one dielectric lens 4 are installed on the outside of the cryogenic system against the optical window 17. Sstf 1 is connected with a microwave bridge 20 (MM), which is connected with the first horn antenna 3 through the first 3 mm of the waveguide 2, MM 20 is connected also to the input of LCA 10, the output of which is connected to the first input SD 11. Input/output SD 11 connected to the first input/output BU 18, and the second input of the MD 11 is connected to the first output GMP 12, the second output of which is connected with the drive coil 13. The output BU 18 connected to the input of BRM occupational 14, which is connected with the superconducting magnet 15.

Declare an EPR spectrometer works in the following way. The signal of the microwave power from the sstf 1 enters through 20 MM, through the first 3 mm of the waveguide 2, the first horn antenna 3, at least one dielectric lens 4, a second horn antenna 5 and the second 3 mm waveguide 6 to the sample mounted on the holder 9. Reflected from the resonator 7, the signal of the microwave power is fed in the reverse direction through the second 3 mm waveguide 6, and the other is the horn antenna 5, at least one dielectric lens 4, the first horn antenna 3 and the second 3 mm waveguide 2, 20 MM on the DMS 10. This second horn antenna 5 plays the role of a transmitting antenna, and the first horn antenna 3 plays the role of a receptionist. Then the signal is sent to DM 11 (which includes the amplifier). At the same time there signal from GMP 12, the supply modulation coil 13, and the signal is then fed to BU 13, typically a controller, including a processor, an analog-to-digital Converter (ADC) and digital-to-analogue Converter (DAC), which also manages BRM occupational 14 and may be connected to the computer 21 (K) via a USB port. In the 21 signal is processed and displayed on the interface 21 in the form of the EPR spectrum (see figure 2). To measure signal photo EPR or registration of optically detected magnetic resonance optical excitation from the light source 22 is supplied through the rotary prism 23 (or mirror) through the connection hole 19 in the cavity 7 in the sample.

Was made a prototype of the proposed EPR spectrometer operating at a frequency of 94 GHz, which was used for the plot of quasi-optical path, allows you to apply a microwave power in a single-mode resonator, the registration of the EPR spectrum was carried out at room temperature on a specially selected sample, allowing to observe ignal EPR at low magnetic fields, to create utilizing an electromagnet standard EPR spectrometer 3 cm range. For registration of EPR signal at a frequency of 94 GHz was used, the magnetic field modulation frequency of 100 kHz.

1. The spectrometer electron paramagnetic resonance, comprising a generator of microwave (microwave) range 90-100 GHz microwave bridge, the transport system of the microwave power to the sample in the form of a series set of the first 3 mm of the waveguide, the first horn antenna, at least one dielectric lens, the second horn antenna facing the mouthpiece to the horn first horn antenna, and the second 3 mm waveguide, a resonator, provided with a piston and a holder for the sample, the detector microwave signal, the synchronous detector, the modulation generator magnetic field modulation coil, the scanner's magnetic field, a superconducting magnet cryogenic system to maintain the temperature of the liquid helium equipped with an optical window, and a control unit, a cryogenic system posted by the superconducting magnet, the drive coil, the second horn antenna, the second 3 mm waveguide and the resonator, the second horn antenna is installed against the optical window of the cryogenic system and through the second 3 mm waveguide connected to the cavity through the opening, one of the horn antennas is a and at least one dielectric lens mounted outside the cryogenic system against its optical window, the generator of the microwave range is connected with the first horn antenna via a microwave bridge, which, in turn, is connected to the input of the detector microwave signal, the output of which is connected to the first input of the synchronous detector, the input/output of which is connected to the first input/output control unit, and the second input of synchronous detector connected to the first generator output modulation of the magnetic field, the second output of which is connected with the drive coil, the output control unit connected to the input of the scanner's magnetic field, which is connected with the superconducting magnet.

2. The spectrometer according to claim 1, characterized in that it contains a light source, optically coupled through a rotating prism or mirror with a communication hole in the resonator.

3. The spectrometer according to claim 1, wherein the dielectric lens is made of PTFE.



 

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