CN108469447A - Probe-type vacuum spin detection method based on microwave phase modulation spectroscopy technique - Google Patents
Probe-type vacuum spin detection method based on microwave phase modulation spectroscopy technique Download PDFInfo
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- CN108469447A CN108469447A CN201810227009.4A CN201810227009A CN108469447A CN 108469447 A CN108469447 A CN 108469447A CN 201810227009 A CN201810227009 A CN 201810227009A CN 108469447 A CN108469447 A CN 108469447A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/10—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using electron paramagnetic resonance
Abstract
The probe-type vacuum spin detection method based on microwave phase modulation spectroscopy technique that the invention discloses a kind of bases, includes the following steps：（1）, by microwave generator signal output end access microwave resonator, signal is then accessed into nano-probe by cantilever beam；（2）, open microwave source, probe tip emits microwave sweep signal, and microwave field frequency range is arranged, when not being put into sample scanning sample is placed on objective table by after data initialization；（3）, start to scan after setting Sample Scan region and accuracy, probe carries out high-speed mobile in scanning area, and microwave signal penetrates sample interior, and transition occurs for the Electron absorption energy of sample interior, and signal returns to probe and feedback signal is simultaneously sent to data collection terminal；（4）, data are analyzed according to the signal of collection terminal acquisition, generate microwave absorption and be distributed collection of illustrative plates, to which the position of electron spin resonance occur in judgement sample, may further obtain sample interior structure.
Description
Technical field
The invention belongs to quantum informations to resolve field, specially a kind of micro- based on microwave phase modulation spectroscopy technique application high-resolution
The method of wave probe test sample interior electron spin information.
Background technology
With unmatched electron magnetic moment from the unpaired spin of outer-shell electron or communization electronics（Such as semiconductor and
Free radical, the crystal defect of conduction electrons, organic matter in metal（Such as dislocation）And irradiation damage（Such as colour center）Deng）It generates not
Sharing electron generates magnetic resonance in certain stationary magnetic field and high frequency magnetic field while under acting on and is known as electron spin resonance（ESR）.
If adding the electromagnetic wave of suitable frequency in vertical outer magnetic field direction, the Electron absorption electromagnetic wave energy in low spin energy level can be made
And transit to high level.Using this principle, this system uses high-resolution Nano grade probe, by carrying out layer to sample
Analysis type micro-wave scanning come study the type at paramagnetism foreign ion and electron-hole related with point defect center in mineral,
Concentration, property.
To read the distributed intelligence of sample interior atom, existing method, which has, utilizes mobile STM probes and material surface
Interaction, the tunnelling current between surface and needle point feeds back the transition of electronics between some atom of surface, and thereby determines that out object
The monatomic ordered state of list on matter surface is long, but it has higher requirements to STM probes, in order to make atomic spin resonate, needs
There is high frequency lead that the signal of gigahertz frequencies is transmitted to probe, meanwhile, it needs to be guaranteed at ultra-high vacuum environment, and can only
Detect sample surfaces.
Invention content
The present invention is directed to existing electron spin detection method, improves the width and depth of detection range, and connect using non-
Touch probe detects the frequency of microwave come the microwave absorption situation of depth level different in test sample by change, utilizes
Sample interior characteristic electron is reflected to the absorption of microwave signal when electron spin resonance in sample, conventional method is breached and is only capable of
The limitation of test sample surface characteristic.
The present invention adopts the following technical scheme that realization：
A kind of probe-type vacuum spin detection method based on microwave phase modulation spectroscopy technique, includes the following steps：
（1）, by microwave generator signal output end access microwave resonator, then by signal pass through cantilever beam access nanometer visit
Needle, nano-probe are provided simultaneously with Microwave emission and receive capabilities by electronic circuit, on the one hand which emits from micro-
The microwave of wave resonator, on the one hand receive in Sample Scan region by the microwave of absorption back reflection；The microwave of nano-probe is defeated
Outlet connects oscillograph by wave detector with low-frequency amplifier；
One steady magnetic field generated by permanent magnet is set at objective table, tune field coil, the tune field are provided with outside permanent magnet
Coil connects regulated power supply by phase shifter；
Objective table center is fixed with the sample with electron spin property, and nano-probe is fixed on a cantilever beam, by adjusting two
Operating platform is tieed up, nano-probe needle point is made to be placed in above sample；
（2）, open microwave generator, nano-probe tip emit microwave sweep signal, pass through adjust field coil generate a low frequency
Alternating magnetic field is superimposed to steady magnetic field up, and observation and adjusting covibration determine the microwave field frequencies range model corresponding to the sample
It encloses；
（3）, set microwave field frequencies range, when not being put into sample scanning sample is placed on objective table by after data initialization；
After microwave generator exports microwave, sample position is first manually adjusted, then probe is scanned in platform surface, to determine sample side
Boundary；Start to scan after setting Sample Scan region and accuracy, probe is moved in scanning area, and microwave signal penetrates sample
Inside product, transition occurs for the Electron absorption energy of sample interior, and signal returns to probe and feedback signal is sent to oscillograph；
（4）, setting Sample Scan region and accuracy after start to scan, nano-probe is moved in scanning area, microwave
Signal penetrates sample interior, and transition occurs for the Electron absorption energy of sample interior, and signal returns to probe and transmits feedback signal
To oscillograph；
（5）, oscillograph enter data into FPGA, carry out processing analysis after carrying out digital filtering to the signal of acquisition, resolve and draw
Figure is demodulated, the signal after output adjustment is distributed collection of illustrative plates in graphical display window display waveform microwave absorption；
（6）, by observe microwave absorption peak, thus intuitively find out in sample occur electron spin resonance position, that is, obtain
In sample specific level can spinning electron distributed intelligence, and then obtain sample interior structure.
In the method for the present invention, microwave generator（VNA）Signal output end accesses microwave resonator, obtains with same stable
Signal is then accessed nano-probe, probe one by the signal for the frequency or frequency range that degree and Low phase noise require by cantilever beam
Aspect provides a microwave signal by electronic circuit, is on the other hand changed to Sample Scan region self-energy by electronic circuit
It is detected.At objective table be arranged a steady magnetic field, generated by permanent magnet, so i.e. ensure that magnetic field degree stability height with
Uniformity is good, and eliminates voltage stabilizing, current stabilization field power supply.Microwave source is opened, probe tip emits microwave sweep signal, adjusts field wire
Circle be used for generate a weak low frequency alternating magnetic field, be superimposed to stationary magnetic field up, achieve the purpose that field sweep, in conjunction with oscillograph with
Convenient for observing and adjusting covibration, the corresponding specific microwave field frequency range of the sample is determined.Then microwave frequency is set,
Sample is placed on objective table by scanning by after data initialization when not being put into sample.After microwave generator exports microwave, probe
High-speed mobile is carried out in scanning area, microwave signal penetrates sample interior, and transition occurs for the Electron absorption energy of sample interior,
Signal returns to probe and feedback signal is sent to data collection terminal（Oscillograph）.When sample has de minimis energy absorption, make into
The amplitude for penetrating microwave becomes smaller, and can sensitively detect the variation that amplitude occurs using high-resolution nano-probe, improve
Detect the sensitivity of electron spin resonance signal.Therefore the envelope of microwave signal becomes by the amplitude modulation of RESONANCE ABSORPTION signal modulation
Wave, after detection is amplified, so that it may the RESONANCE ABSORPTION signal detection of this reflection oscillator oscillation amplitude size variation is come out.
Data are analyzed according to the signal input FPGA of collection terminal acquisition, microwave absorption is generated and is distributed collection of illustrative plates（Electron resonance Spectral structure figure）,
To which the position of electron spin resonance occur in judgement sample, sample interior structure may further be obtained.
The present invention is directly by probe emission microwave signal, and when scanning sample predeterminable area, sample absorbs microwave energy volume production
Raw electron spin resonance, analysis microwave enter the information of microwave energy before and after sample, draw and absorb collection of illustrative plates, realize to resonance signal
Detection, eliminate probe contacted with sample generate loss.
The method of the present invention combines the detection that microwave phase modulation spectroscopy technique carries out electron spin resonance signal, with microwave by electronics
Energy level excites, using the variation for detecting microwave signal when electron transition to the absorption of microwave, for reading electronics in sample
Spin resonance is distributed, that is, reaches the object of the invention.
Reasonable design of the present invention, detection method is easy, and precision is high, and solves the problems, such as detection sample interior structure.
Description of the drawings
Fig. 1 shows probe-type ESR system structures.
Fig. 2 indicates probe structure figure.
Fig. 3 indicates the workflow of spin information detecting system.
Fig. 4 indicates that signal analyzes demodulating process.
In figure：1- samples, 2- microwave generators, 3- microwave resonators, 4- cantilever beams, 5- nano-probes, 6- objective tables, 7-
Permanent magnet, 8- tune field coils, 9- phase shifters, 10- regulated power supplies.
Specific implementation mode
Specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings.
A kind of probe-type vacuum spin detection method based on microwave phase modulation spectroscopy technique, detecting system is as shown in Figure 1, include
Nano-probe 5, nano-probe 5 are provided simultaneously with Microwave emission and receive capabilities, 4 one end linking probe 5 of cantilever beam, other end connection
Microwave resonator 3, microwave resonator 3 connect microwave generator 2；6 center of objective table is fixed with sample 1, and probe 5 is fixed on cantilever
On beam 4, by adjusting two-dimensional operation platform, making probe tip just can be placed in above sample.Objective table 6 is in right permanent magnet
In 7 high-intensity magnetic fields provided, it is provided with tune field coil outside permanent magnet 7, field coil is adjusted to be used for generating a weak low frequency alternating magnetic field,
It is superimposed to stationary magnetic field up, achievees the purpose that field sweep, in conjunction with oscillograph in order to observe and adjust covibration, determine the sample
The corresponding specific microwave field frequency range of product.
When it is implemented, after microwave generator output microwave, sample position is first manually adjusted, then probe is in platform surface
Scanning, to determine sample boundaries.Nano-probe 1 uses Pt material preparations, improves probe measurement accuracy.
The detection method applied microwave phase modulation spectroscopy technique carries out spin information detection to sample, need to only be collected in receiving terminal micro-
Wave signal can free electron spin information in sample.It is as follows：
（1）, by 2 signal output end of microwave generator access microwave resonator 3, then by signal pass through cantilever beam 4 access nanometer
Probe 5, nano-probe 5 are provided simultaneously with Microwave emission and receive capabilities by electronic circuit, on the one hand which emits
From the microwave of microwave resonator, on the one hand receive in Sample Scan region by the microwave of absorption back reflection；Nano-probe 5 it is micro-
Wave output terminal connects oscillograph by wave detector with low-frequency amplifier, as shown in Figure 2.
One steady magnetic field generated by permanent magnet 7 is set at objective table 6, is provided with outside permanent magnet and adjusts field coil 9, is adjusted
Field coil 9 connects regulated power supply 10 by phase shifter 8.
6 center of objective table is fixed with the sample 1 with electron spin property, and nano-probe 5 is fixed on cantilever beam 4, leads to
Two-dimensional operation platform is overregulated, nano-probe needle point is made to be placed in above sample.
（2）, open microwave generator 2, nano-probe tip emit microwave sweep signal, pass through adjust field coil generate one
Low frequency alternating magnetic field is superimposed to steady magnetic field up, and observation and adjusting covibration determine the microwave field frequency corresponding to the sample
Rate range.
（3）, set microwave field frequencies range（Different microwave frequencies corresponds to microwave and enters the different depth of sample）, it is not put into
Sample is placed on objective table by scanning by after data initialization when sample；After microwave generator exports microwave, first manually adjust
Sample position, then probe is in platform surface scanning, to determine sample boundaries；Start after setting Sample Scan region and accuracy
Scanning, probe are moved in scanning area, and microwave signal penetrates sample interior, and the Electron absorption energy of sample interior occurs
Transition, signal return to probe and feedback signal are sent to data collection terminal.
（4）, setting Sample Scan region and accuracy after start to scan, nano-probe is moved in scanning area,
Microwave signal penetrates sample interior, and transition occurs for the Electron absorption energy of sample interior, and signal returns to probe and by feedback signal
It is sent to oscillograph.
（5）, oscillograph enter data into FPGA, carry out processing analysis after carrying out digital filtering to the signal of acquisition, resolve
Demodulation figure is drawn, the signal after output adjustment is distributed collection of illustrative plates, such as Fig. 3 institutes in graphical display window display waveform microwave absorption
Show.
（6）, by observe microwave absorption peak, thus intuitively find out in sample occur electron spin resonance position, i.e.,
Obtain specific level in sample（Sample level in the case of different microwave frequencies）Can spinning electron distributed intelligence, and then
Go out sample interior structure.
Detection method is easy, and precision is high, and eliminates the complexity and unstability when atom measures, and improves
The signal-to-noise ratio of electron magnetic resonance.The detection to resonance signal is realized, to reach the detection of positioning spinning electron position, to really
The structure of random sample product eliminates probe and contacts the loss generated with sample.
It these are only specific embodiments of the present invention, however, it is not limited to this.It is any to be solved substantially based on the present invention
Identical technical problem, or realize essentially identical technique effect, made ground simple change, equivalent replacement or modification etc.,
In all belonging to the scope of protection of the present invention.
Claims (2)
- The detection method 1. a kind of probe-type vacuum based on microwave phase modulation spectroscopy technique spins, it is characterised in that：Include the following steps：（1）, by microwave generator（2）Signal output end accesses microwave resonator（3）, signal is then passed through into cantilever beam（4）It connects Enter nano-probe（5）, nano-probe（5）It is provided simultaneously with Microwave emission and receive capabilities by electronic circuit, the nano-probe one Microwave of the aspect transmitting from microwave resonator, on the one hand receive in Sample Scan region by the microwave of absorption back reflection；It receives Rice probe（5）Microwave output end oscillograph is connected with low-frequency amplifier by wave detector；Objective table（6）Place's setting one is by permanent magnet（7）The steady magnetic field of generation is provided with tune field coil outside permanent magnet（9）, The tune field coil（9）Pass through phase shifter（8）Connect regulated power supply（10）；Objective table（6）Center is fixed with the sample with electron spin property（1）, nano-probe（5）It is fixed on cantilever beam（4） On, by adjusting two-dimensional operation platform, nano-probe needle point is made to be placed in above sample；（2）, open microwave generator（2）, nano-probe tip emits microwave sweep signal, by adjusting field coil generation one low Frequency alternating magnetic field is superimposed to steady magnetic field up, and observation and adjusting covibration determine the microwave field frequencies range corresponding to the sample Range；（3）, set microwave field frequencies range, when not being put into sample scanning sample is placed on objective table by after data initialization； After microwave generator exports microwave, sample position is first manually adjusted, then probe is scanned in platform surface, to determine sample side Boundary；Start to scan after setting Sample Scan region and accuracy, probe is moved in scanning area, and microwave signal penetrates sample Inside product, transition occurs for the Electron absorption energy of sample interior, and signal returns to probe and feedback signal is sent to data acquisition End；（4）, setting Sample Scan region and accuracy after start to scan, nano-probe is moved in scanning area, microwave Signal penetrates sample interior, and transition occurs for the Electron absorption energy of sample interior, and signal returns to probe and transmits feedback signal To oscillograph；（5）, oscillograph enter data into FPGA, carry out processing analysis after carrying out digital filtering to the signal of acquisition, resolve and draw Figure is demodulated, the signal after output adjustment is distributed collection of illustrative plates in graphical display window display waveform microwave absorption；（6）, by observe microwave absorption peak, thus intuitively find out in sample occur electron spin resonance position, that is, obtain In sample specific level can spinning electron distributed intelligence, and then obtain sample interior structure.
- The detection method 2. probe-type vacuum according to claim 1 based on microwave phase modulation spectroscopy technique spins, feature exist In：The nano-probe（5）Using Pt material preparations.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113433348A (en) * | 2021-06-03 | 2021-09-24 | 中北大学 | Probe for microwave test |
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