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.