CN109387799A - Pulsating electronic paramagnetic resonance spectrometer - Google Patents

Pulsating electronic paramagnetic resonance spectrometer Download PDF

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Publication number
CN109387799A
CN109387799A CN201810192503.1A CN201810192503A CN109387799A CN 109387799 A CN109387799 A CN 109387799A CN 201810192503 A CN201810192503 A CN 201810192503A CN 109387799 A CN109387799 A CN 109387799A
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China
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microwave
refrigeration machine
transmission line
magnet
resonance spectrometer
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周宗权
李佩耘
刘超
刘肖
李传锋
郭光灿
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University of Science and Technology of China USTC
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University of Science and Technology of China USTC
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00Arrangements or instruments for measuring magnetic variables
    • G01R33/20Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/60Arrangements or instruments for measuring magnetic variables involving magnetic resonance using electron paramagnetic resonance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/10Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using electron paramagnetic resonance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01RMEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00Arrangements or instruments for measuring magnetic variables
    • G01R33/20Arrangements or instruments for measuring magnetic variables involving magnetic resonance
    • G01R33/28Details of apparatus provided for in groups G01R33/44 - G01R33/64
    • G01R33/30Sample handling arrangements, e.g. sample cells, spinning mechanisms
    • G01R33/31Temperature control thereof

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

A kind of pulsating electronic paramagnetic resonance spectrometer, comprising: the microwave excitation for generating at least one microwave pulse generates unit;Microwave transmission unit, the microwave transmission line including resonant cavity and transmission microwave, the microwave transmission line are connected to microwave excitation and generate between unit resonant cavity, and the cavity configurations are to put sample;Refrigeration machine and magnet unit, including realizing that the cooling refrigeration machine of ultralow temperature, institute's microwave transmission line are arranged through the refrigeration machine and connect the resonant cavity to microwave cavity;Refrigeration machine and magnet unit further include the magnet for providing up magnetic resonance test magnetic field, and the resonant cavity is set in the room temperature gap of magnet.The device of the disclosure has the characteristics that ultralow sample temperature (0.1 Kelvin's magnitude), and instrumental function is complete, easily operated.

Description

Pulsating electronic paramagnetic resonance spectrometer
Technical field
This disclosure relates to nuclear magnetic resonance spectrometer field, more particularly to a kind of pulsating electronic that can be worked under ultra low temperature Paramagnetic resonance spectrometer.
Background technique
Electron paramagnetic resonance spectrometer (electron paramagnetic resonance, EPR) is in a kind of research substance The device of unpaired electron.Its basic principle is the Zeemen effect for sharing electron spin: Single Electron has s=1/2 Spin quantum number, therefore may be at ms=+1/2 or ms=-1/2 spin quantum state, when there are external magnetic field, both spins The energy of state will generate splitting.Further apply the resonance signal that microwave field detects the engery level cracking, substance system can be obtained The internal information of system, including nuclear species class, magnetic field environment, the electron spin spacing etc. around electronics.
EPR is a kind of highly sensitive, non-intrusion type detection method, a variety of in physics, chemistry, biology, medicine, engineering etc. Field has a wide range of applications.Some typical purposes include impurity or the defect inspection of engineering and security fields for material For being used for dose of radiation for imaging of tissue, medical domain in element-specific quantitative analysis, biological field in surveying, chemically reacting Quantitative analysis, in Condensed Matter Physics in the association of more bodies, the research of Phase-change Problems and quantum information field for realizing The functions such as quantum calculation and quantum storage.
Standard EPR system mainly comprises the following modules: microwave source, microwave pulse modulation and demodulation module, microwave amplifier, Microwave bridge, specimen holder, three-dimensional microwave resonant cavity, super uniform magnet.When the impinging microwave of EPR system is continuous wave, this company Continuous wave EPR system is only used for the detection of transition resonance signal.The impinging microwave of EPR system may be set to be complicated microwave pulse Sequence, this pulsed EPR system function can more horn of plenty, can be used for Spin population number service life and relevant service life etc. it is other from Spin dynamics analysis.By taking the application in quantum information field as an example, the prior art often generally requires pulsed EPR system, thus Realize spin quantum state manipulation, the storage of controlled Quantum logic gates, microwave quantum state etc. function.
Mainly there is the BRUKER company of Germany in the producer for being able to produce pulsed EPR system in the world at present.Consider solid The EPR of material is analyzed, and for cooling material internal electron-phonon interaction, is typically necessary low temperature environment.It is commercial at present The minimum sample temperature that EPR system can reach is about 3K.But this temperature is unable to satisfy quantum information field to solid appearance The demand in dry service life.For a typical example, rare earth ion doped crystal is realized to single photon quantum state in recent years High fidelity storage is the quantum storage system with practical potentiality.Its storage life finally limit be ion electronics The relevant service life of spin and nuclear spin.A kind of pulsed EPR system of the prior art, analyzes it as the result is shown with temperature Decline, sample Electron Spin and nuclear spin are concerned with the service life as temperature declines, significantly rise.When reaching, the system is minimum When temperature 5K, the sample Electron Spin core nuclear spin relevant service life respectively reaches 0.1ms and 1ms magnitude [Phys.Rev.Lett.114.170503(2015)].However practical quantum memory generally requires the storage longevity of second-time Life.The longer relevant service life can be obtained by continuing to reduce the sample temperature in the experiment obviously, however the study group has no idea Further data are done, reason is exactly that current all commercialization EPR systems can not reach 3K or less warm area.International academic community is even deposited In a kind of universal view, it is believed that the EPR system of three-dimensional resonance device can not reach 3K or less sample temperature.Such as document [Appl.Phys.Lett.106.193505 (2015)] have explicitly pointed out this point in first page second segment.If using passing The then cooling easy to accomplish of the resonant cavity of defeated line style, but the alternating current magnetic field that this resonant cavity generates only is distributed in tens near transmission line To the range scale of several hundred micron dimensions, which acutely decays with distance change, the disadvantage is that sample scale it is limited and Uniformity of magnetic field is very poor.
Summary of the invention
In view of this, the purpose of the disclosure is to be to provide a kind of electron paramagnetic resonance spectrometer, sample temperature reaches 0.1K Magnitude and the various test functions for having conventional electrical paramagnetic resonance spectrometer.
The disclosure provides a kind of pulsating electronic paramagnetic resonance spectrometer, comprising:
The microwave excitation for generating at least one microwave pulse generates unit;
Microwave transmission unit, the microwave transmission line including resonant cavity and transmission microwave, the microwave transmission line is connected to micro- Wave excitation generates between unit resonant cavity, and the cavity configurations are to put sample;
Refrigeration machine and magnet unit, including realizing the cooling refrigeration machine of 0.1 Kelvin's magnitude ultralow temperature to microwave cavity, The resonant cavity is set in the refrigeration machine, and institute's microwave transmission line is set as penetrating the refrigeration machine and is connected to the resonance Chamber;Refrigeration machine and magnet unit further include the magnet for providing up magnetic resonance test magnetic field, the resonant cavity setting In the room temperature gap of magnet.
In a further embodiment, the microwave transmission unit includes sample inserted link, sample inserted link one end peace Equipped with the resonant cavity, the other end is fixed with the refrigeration machine.
In a further embodiment, the refrigeration machine includes cold across the multilayer of direction setting along microwave transmission line Disk, with cooled microwave transmission line step by step.
In a further embodiment, the microwave cavity be include L, more kinds of service bands of S, X and electronics with The microwave cavity of core double resonance.
In a further embodiment, the conducting medium of the microwave transmission line be silver-plated stainless steel, silver-plated CuNi with And NbTi superconductor.
In a further embodiment, the refrigeration machine and magnet unit further include:
Motorized rails, the guide rail is for carrying and positioning the magnet.
In a further embodiment, the refrigeration machine tail end is cylinder, and the compatible magnet gap of outer diameter is described The compatible resonant cavity of the machine tail end internal diameter that freezes.
In a further embodiment, the microwave transmission line installs heat sink and adapter at cold dishes at different levels with abundant The shell and inner core of cooled microwave transmission line cable.
In a further embodiment, the sample inserted link includes thermal conductive metallic material.
In a further embodiment, heat radiation screening housing is installed outside the cold dishes at different levels.
EPR system is cooperated into refrigeration machine and microwave transmission line it can be seen from above-mentioned technical solution provided by the present disclosure Set-up mode, can obtain the sample temperature of 0.1K magnitude, to realize the EPR detection of ultra-low temperature region.It can using motorized rails Operation is docked and assembled with conveniently realize EPR system and refrigeration system;Equipment used by the above process is easily operated And stability is high, the temperature of sample is low and the institute of compatible conventional EPR system is functional.
Detailed description of the invention
It, below will be to required use in embodiment description in order to illustrate more clearly of the technical solution of the embodiment of the present disclosure Attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description is only some embodiments of the present disclosure, for this For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other Attached drawing.
Fig. 1 is the pulsating electronic paramagnetic resonance spectrometer frame diagram that the embodiment of the present disclosure provides;
Fig. 2 is the pulsating electronic paramagnetic resonance spectrometer part assembling schematic diagram that the embodiment of the present disclosure provides;
Fig. 3 is the Nd in YSO crystal at a temperature of 6.5K of resonance spectrometer shown in the application drawing 2 that provides of the embodiment of the present disclosure3+From Field sweep electron spin echo (ESE) schematic diagram of son;
Resonance spectrometer YSO crystal under ultra-low temperature region shown in the application drawing 2 that Fig. 4 A and Fig. 4 B provide for the embodiment of the present disclosure Middle Nd3+The electron spin echo (ESE) and temperature dependence figure of ion.Wherein, Fig. 4 A is provided surveys under different sample temperatures The time-domain signal of electron spin echo;Fig. 4 B provides the relative size of electron spin echo and the relationship of sample temperature.
Specific embodiment
Below with reference to the attached drawing in the embodiment of the present disclosure, the technical solution in the embodiment of the present disclosure is carried out clear, complete Ground description, it is clear that described embodiment is only disclosure a part of the embodiment, instead of all the embodiments.Based on this Disclosed embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts Example, belongs to the protection scope of the disclosure.
" ultralow temperature " described in the disclosure refers to the temperature of 0.1K (Kelvin) magnitude.
As described above, the EPR spectrometer of ultra-low temperature region is the great basic instrument of quantum information, quantum field of storage urgent need. Such as consider under the ultralow temperature of 0.1K, 95% or more initialization may be implemented in the i on population of electron spin in X-band EPR spectrometer Level, this directly makes the signal-to-noise ratio (the namely signal-to-noise ratio of instrument) of electron spin echo compared to the test condition of 3K temperature, Enhance one to two magnitudes.The promotion of signal-to-noise ratio is the basic index of all measuring instruments, therefore ultralow temperature EPR system is also expected to Other field obtains more applications.
According to the basic conception of the disclosure, a kind of pulsating electronic paramagnetic resonance spectrometer is provided, comprising: generate at least one The microwave excitation of microwave pulse generates unit;Microwave transmission unit, the microwave transmission line including resonant cavity and transmission microwave are described Microwave transmission line is connected to microwave excitation and generates between unit resonant cavity, and the cavity configurations are to put sample;Refrigeration machine And magnet unit, including realizing that the cooling refrigeration machine of ultralow temperature, institute's microwave transmission line are arranged through described to microwave cavity Refrigeration machine simultaneously connects the microwave cavity;Refrigeration machine and magnet unit further include providing up the magnetic resonance test magnetic The magnet of field, the resonant cavity are set in the room temperature gap of magnet.It can also include acquiring and analyzing microwave transmission unit Emit the microwave sounding unit of microwave.By above-mentioned setting, EPR system is cooperated into refrigeration machine, the super of 0.1K magnitude can be obtained Low sample temperature.
Fig. 1 is the schematic diagram for the system framework that the embodiment of the present disclosure one provides.As shown in Figure 1, the device mainly includes:
Microwave excitation generates unit 11, microwave transmission unit 12, microwave sounding unit 13 and refrigeration machine and magnet unit 14。
Wherein, the microwave excitation generates unit 11, for generating various High-Power Microwave pulses;
The microwave transmission unit 12, for the directional transmissions of microwave pulse, install sample and realize microwave transmitting and It collects;
The microwave sounding unit 13, acquisition and analysis for microwave signal;
The microwave excitation generates unit 11, and microwave transmission unit 12 and microwave sounding unit 13 have field sweep paramagnetic resonance The complete test function such as detection, electron spin echo, electronics and core double resonance.
The refrigeration machine and magnet unit 14, for realizing that ultralow temperature is cooling and provides high evenness to microwave cavity Magnetic field reaches magnetic resonance test condition.
Further, it includes: microwave source 111, microwave modulation module 112 that the microwave excitation, which generates unit 11, and microwave becomes Frequency module 113, microwave amplifier 114;
Wherein, the microwave source 111, for generating the single-frequency microwave signal of specific frequency;
The microwave modulation module 112, for generating the microwave arteries and veins of all size, phase, frequency from single-frequency continuous microwave Punching;
The microwave frequency-variable module 113, for extending the test frequency range of microwave;
The microwave amplifier 114 reaches high-energy arteries and veins required for pulse EPR for executing amplification to microwave pulse Punching.
Further, the microwave transmission unit 12 includes: that microwave circulators 121, microwave transmission line 122 and microwave are humorous Shake chamber 123;
Wherein, the microwave circulators 121, for the directional transmissions of microwave, guide the microwave of microwave excitation unit 11 into Enter sample, and transmits sample signal and enter microwave sounding unit 13;
The microwave transmission line 122, for the microwave transmission between microwave circulators 121 and microwave cavity 123; It is different from conventional microwave transmission cable, it is contemplated that the ultralow temperature cooling requirement of the present apparatus, the material selection of the microwave transmission line Conductive and heat-insulated demand should be taken into account, typical conducting medium can be silver-plated stainless steel, silver-plated CuNi and NbTi superconductor.
The microwave cavity 123, for installing sample and realizing the transmitting and collection of microwave;The microwave resonance of the disclosure Chamber 123 is three-D resonant cavity, and the alternating current magnetic field which generates is evenly distributed and can test large scale sample, has Richer test function.
Further, the track microwave sounding unit 13 includes: protective door 131, and frequency mixer 132, low pass filtered, which involve, puts Big device 133 and oscillograph 134;
Wherein, the protective door 131, for closing detection system in High-Power Microwave pulse incidence;When signal detection, Open detection system;
The frequency mixer 132, microwave signal and local oscillator microwave mixer for arriving to microwave transmission module collection, which are extracted, to be believed Number;Its local oscillator microwave generates unit 11 from microwave excitation
The low pass filtered involves amplifier 133, and the mixed frequency signal execution low pass filtered for exporting frequency mixer 132, which involves, puts Greatly, pulse demodulation is realized;For the amplification to demodulation afterpulse signal;
The oscillograph 134, for the storage and display to signal.
Further, the refrigerator unit 14 includes: refrigeration machine 141, refrigeration machine cavity 142 and super uniform magnet 143, motorized rails 144;
Wherein, the refrigeration machine 141, for providing refrigerating capacity, cooling goal systems;Pass through instrument described in the refrigeration machine Sample temperature can reach 0.1K magnitude;
The refrigeration machine cavity 142, for the installation of microwave transmission line 122 and microwave cavity 123, and is isolated the external world Heat radiation;
The super uniform magnet 143, for generating the magnetic field of high evenness high stable;It can be room temperature electromagnet either Superconducting magnet.
The motorized rails 144, when executing sample replacement, for the carrying and positioning to magnet;The motorized rails Has the jack run up and down for carrying and positioning placement magnet, and horizontal direction stroke is more than magnet outer dimension.
The embodiment of the present disclosure combines refrigeration machine and routine EPR system, realizes the EPR test of ultralow temperature, and has Help significantly improve the signal-to-noise ratio of test;Equipment used by the above process is easily operated, system stability with higher And perfect test function.
In order to be further described the disclosure, the embodiment of the present disclosure will enumerate specific numerical value, join to the element in the device Number is introduced;It should be noted that cited numerical value of the elements only to facilitate the understanding of the present disclosure, is not construed as limiting; In practical applications, user can according to demand or experience use different parameters element.
Each section module in Fig. 1 both individually can be purchased and be assembled, and can also provide multimode group from the prior art Subsystem after dress is easier to build pulsating electronic paramagnetic resonance spectrometer based on such subsystem.Such as commercialization EPR spectrum Instrument can provide microwave excitation unit, the circulator in microwave transmission unit and microwave cavity, microwave sounding unit and refrigeration machine And the super uniform magnet in magnet unit.As shown in Fig. 2, a kind of system assembles of the EPR spectrometer provided for the embodiment of the present disclosure Schematic diagram.The mating compressor set etc. of the Multilayer radiation-proof housing in low temperature cavity and low temperature cavity is omitted in figure, only presents and is The material particular of system docking.
It is specifically included that
1) (EPR system herein contains microwave excitation and generates unit, microwave transmission list pulsed multiband EPR system The magnet in microwave circulators and microwave cavity, microwave sounding unit and refrigeration machine and magnet unit in member)
It specifically includes that L/S/X band microwave bridge, L/S/X band microwave amplifier, based on the micro- of arbitrary waveform generator Wave modulator, L/S/X band microwave resonant cavity, X-band microwave detection system, electronics and core double resonance (ENDOR) module and Super uniform magnet.
In the present embodiment, the parameter of X-band microwave bridge can be with are as follows: 9.0~10.0GHz of frequency range.The microwave of L/S wave band Bridge mainly realizes the function of frequency transformation, its frequency mixer based on fixed local frequency realizes X-band and two kinds of band signals of L/S Frequency transformation.The mode of this frequency conversion realizes band spreading, is a kind of most economical mode, and a variety of wave bands can share X-band Microwave sounding module.The all built-in microwave circulators of the microwave bridge of three kinds of wave bands, realize the directional transmissions of microwave.
In the present embodiment, X-band microwave amplifier is the solid amplifier of 300W, the output power of L/S band amplifier About 100W.
In the present embodiment, the parameter of the microwave modulator based on arbitrary waveform generator can be with are as follows: sample rate 5GS/s is adjusted Bandwidth 500MHz processed realizes random waveform modulation to frequency, phase, amplitude.
In the present embodiment, L/S/X band microwave resonator parameter can be with are as follows: each intracavitary portion effective aperture 5mm of band resonant, Outer diameter 20mm realizes that easily wave band is replaced using SMB or MMCX type fast joint.The Q value of each band resonant chamber can be 50 and arrive 500 or so, Q value required for determining according to specific experiments.
In the present embodiment, the parameter of the super uniform superconducting magnet of coil form can be with are as follows: uniformity of magnetic field 10ppm 40mm DSV, Maximum field strength 1.8T, the air gap 100mm.
2) dilution refrigeration machine system (the main improvement due to the part as the embodiment of the present disclosure, individually enumerate It is illustrated, the refrigeration machine in corresponding diagram 1)
In the present embodiment, the parameter of refrigeration machine can be with are as follows: the dilution refrigeration machine of no liquid helium consumption, minimum temperature 10mK, Refrigeration work consumption 1W under refrigeration work consumption 400uW under 100mK, 4K.
In the present embodiment, preferred 201 parameter of refrigeration machine cavity can be with are as follows: and it include 50K cold dish 2055,3K cold dish 2054, 1K cold dish 2053,100mK cold dish 2052 and 10mK cold dish 2051.Wherein 50K cold dish 2055,3K cold dish 2054,1K cold dish 2053 are both needed to mating installation heat radiation screening housing (not shown).Freeze drive end unit outer diameter 95mm, and tail portion sample space has Imitate internal diameter 40mm.
In magnet the air gap of the refrigeration system by top insertion electron paramagnetic resonance system.
3) special system convergence part
It mainly includes sample inserted link 207, microwave transmission line 208.
In the present embodiment, resonant cavity 203 is mounted on the sample inserted link 207 of a heat-conducting metal material, sample inserted link 207 The other end be fixed on the lowest temperature cold dish 2051 of 10mK, between other cold dishes (2052,2053,2054 and 2055) without even It connects.In the present embodiment, the parameter of microwave transmission line can be with are as follows: semirigid coaxial transmission line, line outer diameter can be 3.5mm;Line Shell and inner core can be the material that silver-plated stainless steel, superconductor etc. are not easy thermally conductive yet highly conduction.
To further increase cooling effect, multiple heat sink 206 are arranged on the route of microwave transmission line 208.
4) motorized rails 204
In the present embodiment, the parameters of motorized rails 204 can be with are as follows: and weight bearing ability is greater than 3 tons, and 1.5 meters of impulse stroke, positioning Precision 0.1mm.The size of working face of guide rail plate is 550mm*550mm.
Magnet 202 in the present embodiment, two sides feet height can be 230mm, and feet distance in two sides is 600mm.It leads Rail is equipped with the jack of 20mm height stroke, has been used to support or has put down magnet after positioning.After guide rail jack rises, working face Plate is apart from ground total height 240mm, and working face of guide rail plate has directly supported magnet 202 and carried positioning at this time.Guide rail jack After falling, magnet 202 is detached from guide pass, directly supports on the ground.
In figure, refrigeration machine tail end is cylindrical, the compatible magnet gap of outer diameter, and refrigeration machine tail end internal diameter compatibility is described humorous Shake chamber.
In the present embodiment, for the temperature performance of optimization system temperature-fall period, measurement real system, thermometer can be used Measure the means measurement system and sample actual work temperature of assisted spin polarization calibration.
When system installs S-band microwave cavity, a calibrated RuO is mounted in resonant cavity2Resistance thermometer, As temperature reduces, resistance value is stepped up.The results show that minimum temperature reaches under conditions of resonant cavity is without actual test sample 10mK or less.
Further, the horizontal Accurate Determining sample real work temperature of rare earth ion spin polarization can be used in the present embodiment Degree.System is mounted with X-band ENDOR resonant cavity, intracavitary to be loaded with 20ppm concentration143The YSO crystal of Nd isotope doping, crystal In also the even number mass number containing 1ppm or so isotope (including142Nd,164Nd,148Nd).External testing magnetic field and crystal D1 axis is parallel.At a temperature of Fig. 3 gives 6.5K, the test result of field sweep electron spin echo, it includes 16143The spectral line of Nd With the spectral line of 2 even number mass number Nd isotopes.
Fig. 4 A gives under the magnetic field 4581G, when changing different cold dish temperature, the spin echo signal of acquisition.The survey Nd isotope of the magnetic resonance signal obtained under examination magnetic field from even number mass number.A length of 2us when spin evolution is chosen in experiment, It is concerned with service life (20us~200us) far below the electron spin under all test temperatures.
The electron spin of the Nd isotope of even number mass number is 1/2, and nuclear spin zero is simple two energy level under magnetic field System.Its spin echo relative size is proportional to the Population difference of target transition, can strictly be calculated according to ANALOGY OF BOLTZMANN DISTRIBUTION Two ionic fractional abundances under different temperatures are poor:
Wherein h is Planck's constant, and v=9.56GHz is microwave frequency, and h*v is the energy of resonant microwave photon, and k is glass The graceful constant of Wurz, T are sample temperature.When T approaches absolute zero 0K, spin echo size reaches relative maximum 1.
Fig. 4 B can see as cold dish temperature declines, and sample echo-signal is stepped up, and equipment is in 0.1K operating temperature The commercialization instrument of 4.5K operating temperature is compared down, and signal-to-noise ratio can be lifted beyond 20 times.Experimental result complies fully with Boltzmann It is distributed predicted spin polarization horizontal, therefore Strict Proof sample operating temperature reaches 0.1K.
The pulsating electronic paramagnetic resonance spectrometer of original creation is had developed in the embodiment of the present disclosure, thermometer shows sample cavity without negative It carries temperature and reaches 10mK or less.Nd in YSO crystal is completed based on the device3+The ultralow temperature spin echo of ion is tested, according to The size of spin echo signal, which calibrates sample actual work temperature, can reach 0.1K.This is to report minimum temperature in the world Three-D resonant cavity pulsating electronic paramagnetic resonance spectrometer.Its each section component is all universal electricity device, and device is steady It is fixed and multiple functional, there is wide application prospect.
It is apparent to those skilled in the art that for convenience and simplicity of description, only with above-mentioned each function The division progress of module can according to need and for example, in practical application by above-mentioned function distribution by different function moulds Block is completed, i.e., the internal structure of device is divided into different functional modules, to complete all or part of function described above Energy.
Particular embodiments described above has carried out further in detail the purpose of the disclosure, technical scheme and beneficial effects Describe in detail bright, it should be understood that the foregoing is merely the specific embodiment of the disclosure, be not limited to the disclosure, it is all Within the spirit and principle of the disclosure, any modification, equivalent substitution, improvement and etc. done should be included in the protection of the disclosure Within the scope of.

Claims (10)

1. a kind of pulsating electronic paramagnetic resonance spectrometer, characterized by comprising:
The microwave excitation for generating at least one microwave pulse generates unit;
Microwave transmission unit, the microwave transmission line including resonant cavity and transmission microwave, the microwave transmission line are connected to microwave and swash It encourages and generates between unit resonant cavity, the cavity configurations are to put sample;
Refrigeration machine and magnet unit, it is described including realizing the cooling refrigeration machine of 0.1 Kelvin's magnitude ultralow temperature to microwave cavity Resonant cavity is set in the refrigeration machine, and institute's microwave transmission line is set as penetrating in the refrigeration machine and is connected to the resonance Chamber;Refrigeration machine and magnet unit further include the magnet for providing up magnetic resonance test magnetic field, the resonant cavity setting In the room temperature gap of magnet.
2. pulsating electronic paramagnetic resonance spectrometer according to claim 1, which is characterized in that the microwave transmission unit packet Sample inserted link is included, sample inserted link one end is equipped with the resonant cavity, and the other end is fixed with the refrigeration machine.
3. pulsating electronic paramagnetic resonance spectrometer according to claim 1, which is characterized in that the refrigeration machine includes along micro- Wave transmission line passes through the multilayer cold dish of direction setting, and with cooled microwave transmission line step by step, the microwave transmission line is set as layer-by-layer Across the cold dish.
4. pulsating electronic paramagnetic resonance spectrometer according to claim 1, which is characterized in that the microwave cavity is packet Include L, the microwave cavity of more kinds of service bands of S, X and electronics and core double resonance.
5. pulsating electronic paramagnetic resonance spectrometer according to claim 4, which is characterized in that the microwave transmission line is led Dielectric is silver-plated stainless steel, silver-plated CuNi and NbTi superconductor.
6. pulsating electronic paramagnetic resonance spectrometer according to claim 1, which is characterized in that the refrigeration machine and magnet list Member further include:
Motorized rails, the guide rail is for carrying and positioning the magnet.
7. pulsating electronic paramagnetic resonance spectrometer according to claim 6, which is characterized in that the refrigeration machine tail end is circle Cylindricality, the compatible magnet gap of outer diameter, the compatible resonant cavity of the refrigeration machine tail end internal diameter.
8. pulsating electronic paramagnetic resonance spectrometer according to claim 6, which is characterized in that the microwave transmission line is each Heat sink and adapter is installed to be fully cooled the shell and inner core of microwave transmission line cable at grade cold dish.
9. pulsating electronic paramagnetic resonance spectrometer according to claim 2, which is characterized in that the sample inserted link includes to lead Hot metallic material.
10. pulsating electronic paramagnetic resonance spectrometer according to claim 3, which is characterized in that pacify outside the cold dishes at different levels Equipped with heat radiation screening housing.
CN201810192503.1A 2017-08-10 2018-03-08 Pulsating electronic paramagnetic resonance spectrometer Pending CN109387799A (en)

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