CN102945786B - Flat-plate type high-field asymmetric waveform ion mobility spectrometer with noise reduction function - Google Patents

Flat-plate type high-field asymmetric waveform ion mobility spectrometer with noise reduction function Download PDF

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CN102945786B
CN102945786B CN201210448596.2A CN201210448596A CN102945786B CN 102945786 B CN102945786 B CN 102945786B CN 201210448596 A CN201210448596 A CN 201210448596A CN 102945786 B CN102945786 B CN 102945786B
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electrode
migration area
asymmetric waveform
current detection
current
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CN102945786A (en
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唐飞
王晓浩
徐初隆
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Tsinghua University
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Abstract

The invention discloses a flat-plate type high-field asymmetric waveform ion mobility spectrometer with a noise reduction function, which comprises an ion source, a migration area and a detection unit, wherein an upper substrate and a lower substrate are arranged in the migration area in parallel; the upper substrate and the lower substrate are respectively provided with an upper migration area electrode and a lower migration area electrode; the upper migration area electrode is connected with an asymmetric waveform radio-frequency power supply and a direct-current scanning compensation power supply; and the detection unit consists of a current detection electrode and a current detection deflection electrode which are respectively arranged on the upper substrate and the lower substrate. The flat-plate type high-field asymmetric waveform ion mobility spectrometer with the noise reduction function is characterized in that one circle of migration area shielding electrode is additionally arranged on the periphery of the upper migration area electrode; meanwhile, one circle of current detection shielding electrode is additionally arranged around the current detection electrode; the two circles of shielding electrodes are respectively earthed; and the upper migration area electrode and the migration area shielding electrode as well as the current detection electrode and the current detection shielding electrode are insulated by air or insulating materials.

Description

There is the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function
Technical field
The present invention relates to and biochemical substances is measured, belong to field assay detection field, be specially one and around migration area electrode and current detection electrode, increase by a circle bucking electrode respectively and ground connection, reduce the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of input noise.
Background technology
High-Field asymmetric waveform ion mobility spectrometry (FAIMS, High-field Asymmetric Waveform Ion MobilitySpectrometry) is a kind of biochemical substances detection technique that the nineties progressively grows up last century.It mainly utilizes the mobility of ion under high electric field the characteristic different with the change of electric field strength can be separated and detect different types of material.Its general principle is as follows: under low current field condition, and the mobility coefficients of ion and electric field strength have nothing to do; After electric field strength height to certain value (E/N>40Td), the mobility coefficients K of ion will change with electric field strength in the nonlinear mode of one.The relation of the mobility of ion under High-Field and electric field strength is available as shown in the formula subrepresentation:
K=K 0[1+α 1(E/N) 22(E/N) 4+…]
Wherein K is the mobility of ion under high electric field, K 0for the mobility of ion under low electric field, E is electric field strength, and N is gas density, α 1, α 2for ionic mobility decomposition coefficient.Make α (E)=[α 1(E/N) 2+ α 2(E/N) 4+ ... ], then K=K 0[1+ α (E)].As α (E) >0, K>K 0, then K increases with E and increases; As α (E) <0, K<K 0, then K reduces along with the increase of E; As α (E) ≈ 0, K ≈ K 0.As seen from the above analysis, under the effect of high electric field, the mobility of ion can present nonlinear trends different separately, and this just makes the ion that ionic mobility is identical or close under low electric field strength condition separatedly under high electric field strength condition to open.
At present, High-Field asymmetric waveform ion mobility spectrometry mainly contains plate and cylinder type two kinds of structures, compared to cylinder type, plate High-Field Asymmetric Waveform Ion Mobility Spectrometer is easier to micro electro mechanical system (MEMS) technology (MEMS, Micro ElectroMechanical System) carry out process, be convenient to microminiaturization, therefore in portable biochemical detecting instrument device, there is larger advantage.
That furthers investigate plate High-Field Asymmetric Waveform Ion Mobility Spectrometer mainly contains Sionex company and Tsing-Hua University.Wherein the structure of the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of Sionex company as shown in Figure 1.The Chinese patent " the ion focusing method of slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer " (application number 201010619966.5) that Tsing-Hua University proposes adds a direct voltage at lower migration area electrode, ion is assembled to center, migration area while separation, the losses of ions that minimizing brings because of factors such as diffusion, carrier gas disturbances, increase signal strength signal intensity, its structure as shown in Figure 2.In addition, Chinese patent " aggregation apparatus of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer and method " (application number 20120211272.7) of Tsing-Hua University's application arranges at least one focal zone in front end, migration area, the upper substrate and subtegulum of each focal zone arrange at least one pair and focuses on pole plate pair, and just right up and down, its structure is as shown in Figure 3.Simultaneously every secondary focus on pole plate on apply specific voltage, the voltage of applying has two kinds of patterns, direct current focusing mode be focusing pole plate on interval apply identical direct voltage, as shown in Figure 4; Radio frequency focusing pattern for every secondary focus on pole plate on apply sinusoidal rf potential, adjacent focus pole plate radio frequency voltage-phase differs 180 °, as shown in Figure 5.The voltage applied makes ion retrain the width of ion beam before entering migration area, reduces the broadening of spectral lines caused because ion disperses in migration area, improves the resolution of system.But these structures above all also exist deficiency: because the asymmetric waveform radio-frequency voltage applied on migration area electrode is a high voltage high frequency voltage, can produce electromagnetic interference in whole space; And the electric current that current detection electrode detects is the small-signal of a skin peace magnitude, this signal is very easy to the interference being subject to asymmetric waveform radio-frequency voltage, causes the last signal noise detected very large, departs from actual value.
Summary of the invention
The object of the invention is the deficiency overcoming existing plate High-Field Asymmetric Waveform Ion Mobility Spectrometer, a kind of structural design reducing noise is provided, make current detecting be not easy to be subject to the interference of asymmetric waveform radio-frequency voltage, improve the performance of system.
Technical scheme of the present invention is as follows:
Have a plate High-Field Asymmetric Waveform Ion Mobility Spectrometer for noise reduction function, described plate High-Field Asymmetric Waveform Ion Mobility Spectrometer comprises ion source, migration area and detecting unit; Substrate and subtegulum in parallel placement in migration area, migration area electrode and lower migration area electrode on upper substrate and subtegulum are arranged respectively, upper migration area electrode is connected with dc sweeps offset supply with asymmetric waveform radio-frequency power supply respectively; Described detecting unit is made up of current detection electrode and current detecting deflecting electrode, current detection electrode is placed on substrate, current detecting deflecting electrode is arranged on subtegulum, it is characterized in that: at upper migration area surrounding them, one circle migration area bucking electrode is set, one loop current is set around current detection electrode and detects bucking electrode, two circle bucking electrodes ground connection respectively; Between upper migration area electrode and migration area bucking electrode, and insulate with air or insulating material between current detection electrode and current detecting bucking electrode.
The present invention has the following advantages and high-lighting effect: 1., the structure of bucking electrode of the present invention effectively can reduce the interference of asymmetric waveform radio-frequency voltage for current detecting, improves sensitivity and the stability of system; 2., the present invention can work in atmospheric conditions, do not need the pumped vacuum systems of assisting; 3., the present invention totally based on slab construction, the structure of migration area, detecting unit, migration area bucking electrode and current detecting bucking electrode is all convenient to adopt MEMS process technology to process, and is easy to integrated, is convenient to FAIMS system microminiaturized.
Accompanying drawing explanation
The plate High-Field Asymmetric Waveform Ion Mobility Spectrometer structural principle schematic diagram of Tu1Shi Sionex company.
The plate High-Field Asymmetric Waveform Ion Mobility Spectrometer structural principle schematic diagram of the Chinese patent " the ion focusing method of slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer " (application number 201010619966.5) that Tu2Shi Tsing-Hua University proposes.
The plate High-Field Asymmetric Waveform Ion Mobility Spectrometer structural principle schematic diagram of Chinese patent " aggregation apparatus of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer and method " (application number 20120211272.7) of the application of Tu3Shi Tsing-Hua University.
Pole plate is focused on to applied V diagram under Chinese patent " aggregation apparatus of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer and method " (application number 20120211272.7) direct current focusing mode of Tu4Shi Tsing-Hua University application.
Pole plate is focused on to applied V diagram under Chinese patent " aggregation apparatus of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer and method " (application number 20120211272.7) radio frequency focusing pattern of Tu5Shi Tsing-Hua University application.
Fig. 6 is the structural principle schematic diagram with the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function provided by the invention.
Fig. 7 is the A-A generalized section of Fig. 6.
Fig. 8 is asymmetric waveform radio-frequency voltage schematic diagram.
Fig. 9 is dc sweeps bucking voltage schematic diagram.
Figure 10 is the structural principle schematic diagram that the present invention adds the embodiment of a direct voltage on lower migration area electrode.
Figure 11 is the present invention arranges the embodiment of focal zone structural principle schematic diagram in front end, migration area.
In figure: 1-carrier gas; 2-ion source; 3-migration area; The upper substrate of 4-; 5-subtegulum; 6-upper migration area electrode; Migration area electrode under 7-; 8-dc sweeps offset supply; 9-asymmetric waveform radio-frequency power supply; 10-detecting unit; 11-current detecting deflecting electrode; 12-current detection electrode; 13-migration area bucking electrode; 14-current detecting bucking electrode; 15-direct voltage; 16-focal zone; 17-first focuses on pole plate pair; 18-second focuses on pole plate pair; 19-the 3rd focuses on pole plate pair; 20-the 4th focuses on pole plate pair; 21-the 5th focuses on pole plate pair.
Embodiment
Be described further below in conjunction with the noise-decreasing device of the drawings and specific embodiments to a kind of plate High-Field asymmetric waveform ion mobility spectrometry provided by the invention.
Fig. 6 is the structural representation with the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function of the present invention.Described plate High-Field Asymmetric Waveform Ion Mobility Spectrometer comprises ion source 2, migration area 3 and detecting unit 10, and wherein migration area 3 comprises substrate 4, subtegulum 5, upper migration area electrode 6 and lower migration area electrode 7; The placement parallel with subtegulum 5 of upper substrate 4, form the gas channels of migration area 3, upper migration area electrode 6 and lower migration area electrode 7 lay respectively on substrate 4 and subtegulum 5; At the rear portion of migration area 3, the end of gas channels is the detecting unit 10 that can detect faint ion current, and detecting unit 10 is made up of current detecting deflecting electrode 11 and current detection electrode 12, lays respectively on subtegulum 5 and upper substrate 4; Upper migration area electrode 6 is connected with dc sweeps offset supply 8 with asymmetric waveform radio-frequency power supply 9 respectively.The circle migration area bucking electrode 13 increased around upper migration area electrode 6, the loop current increased around current detection electrode 12 detects bucking electrode 14, and difference ground connection.Between upper migration area electrode 6 and migration area bucking electrode 13, and insulate with air or insulating material between current detection electrode 12 and current detecting bucking electrode 14.The shape of migration area bucking electrode 13 and the shape of upper migration area electrode 6 identical or different; The shape of current detecting bucking electrode 14 and the shape of current detection electrode 12 identical or different.The A-A generalized section of Fig. 6 as shown in Figure 7.
Figure 10 is the structural principle schematic diagram that the present invention adds the embodiment of a direct voltage on lower migration area electrode, namely adds a direct voltage 15 at lower migration area electrode 7; The circle migration area bucking electrode 13 increased around upper migration area electrode 6, the loop current increased around current detection electrode 12 detects bucking electrode 14, and difference ground connection.
Figure 11 is the present invention arranges the embodiment of focal zone structural principle schematic diagram in front end, migration area, namely at least one focal zone 16 is set in front end, migration area 3, the upper substrate 4 and subtegulum 5 of each focal zone 16 at least arrange a secondary focusing pole plate pair, and it is just right up and down, simultaneously every secondary focus on pole plate on apply voltage, the voltage applied has two kinds of patterns, and one is direct current focusing mode, and another kind is radio frequency focusing pattern; Direct current focusing mode be focusing pole plate on interval apply identical direct voltage; Radio frequency focusing pattern for every secondary focus on pole plate on apply sinusoidal rf potential, the sinusoidal rf potential phase 180 ° that adjacent focus pole plate is right.The circle migration area bucking electrode 13 increased around upper migration area electrode 6, the loop current increased around current detection electrode 12 detects bucking electrode 14, and difference ground connection.
The illustrated action principle with the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function is as follows:
Carrier gas 1 carries sample and passes in ionic migration spectrometer, and sample ionization occurs under ion source 2 acts on and forms sample ions.
Upper migration area electrode 6 is connected with asymmetric waveform radio-frequency power supply 9 with dc sweeps offset supply 8 respectively, lower migration area electrode 7 ground connection.The voltage that wherein asymmetric waveform radio-frequency power supply 9 produces is the High-Field asymmetric waveform (as shown in Figure 8) of upper and lower area equation; The voltage that dc sweeps offset supply 8 produces carries out scanning (as shown in Figure 9) between the interval CV1 ~ CV2 of certain dc sweeps bucking voltage with specific scanning frequency and scanning step.For ion not of the same race, under the effect of asymmetric waveform radio-frequency voltage, certain ion upwards migration area electrode 6 or lower migration area electrode 7 produces a clean displacement and (depends on the kinetic characteristic of ion under high field action, the clean displacement of different ions is different), if do not have the effect of dc sweeps bucking voltage, generation deflection strikes on upper migration area electrode 6 or lower migration area electrode 7 and is neutralized by ion.If load a suitable dc sweeps offset supply, the clean displacement energy that ion is produced under the effect of asymmetric waveform radio-frequency voltage accesses compensation, then ion is by migration area.The ion of certain dc sweeps bucking voltage so corresponding can pass through migration area, and other ion then strikes on metal electrode and is neutralized.Then the corresponding different types of ion of the dc sweeps bucking voltage of different size, therefore just can determine the kind of sample according to the value of dc sweeps bucking voltage.
Filter through migration area 3 under the effect of the ion after selecting in carrier gas and continue to move right, enter detecting unit 10, current detecting deflecting electrode 11 applies a direct voltage, by ion deflecting on current detection electrode 12, ion signal is converted into current signal, measures the value of current signal.Due to upper migration area electrode 6 surround by migration area bucking electrode 13, current detection electrode 12 surround by current detecting bucking electrode 14, and migration area bucking electrode 13 and current detecting bucking electrode 14 ground connection respectively, so around upper migration area electrode 6 and current detection electrode 12, form respectively zero potential district, and electric field line cannot pass through zero potential district.Thus, the asymmetric waveform radio-frequency voltage that the asymmetric waveform radio-frequency power supply 9 be connected with upper migration area electrode 6 produces can not interfere with current detection electrode 12, and the interference that current detection electrode 12 accepts will reduce greatly, the current signal detected by current detection electrode 12 truly can reflect actual signal.By recording the related data of the electric current that the corresponding moment detecting unit of each dc sweeps bucking voltage detects, and drawn both corresponding relation curves in real time by software.Through noise and the image procossing of microprocessor, determine the dc sweeps bucking voltage value that in each waveform, current signal maximum is corresponding.Data in the flow velocity of the size (length, width, spacing) of the relevant parameter (voltage max, frequency, duty ratio, waveform etc.) of High-Field asymmetric waveform radio-frequency voltage now and dc sweeps bucking voltage, migration area, air pressure, pure carrier gas, temperature and kind (High Purity Nitrogen, cleaned air, carbon dioxide etc.) and dc sweeps bucking voltage value and database are compared, thus determines sample material kind entrained in sample carrier gas.
Embodiment 1:
Utilization has the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function and has carried out unloaded contrast experiment without the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function.Obstructed carrier gas in experiment, obstructed sample, just observe the impact of asymmetric waveform radio-frequency voltage for current detecting.Asymmetric waveform radio-frequency power supply 9 produces frequency 1MHz, and duty ratio is the asymmetric waveform radio-frequency voltage of 30%, is carried on migration area electrode 6.The peak-to-peak value of asymmetric waveform radio-frequency voltage is started from scratch and is increased gradually, the current value recorded under simultaneously recording corresponding voltage.From the experimental results, the detection electric current without the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function sharply increases along with the increase of asymmetric waveform radio-frequency voltage, cannot measure; And the detection electric current with the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function changes little along with the increase of asymmetric waveform radio-frequency voltage, affect very little on actual measurement.
Without the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function
Radio-frequency voltage Vpp/V 0 100 200 300 400
Electric current/pA 1.5 1.3 1.5 1.4 -0.3
Radio-frequency voltage Vpp/V 450 500 550 600 650
Electric current/pA -5 -21 -62 -84 -96
There is the plate High-Field Asymmetric Waveform Ion Mobility Spectrometer of noise reduction function
Radio-frequency voltage Vpp/V 0 100 200 300 400 450
Electric current/pA -4.4 -4.0 -3.5 -3.1 -3.4 -4.1
Radio-frequency voltage Vpp/V 500 550 600 650 700 750
Electric current/pA -4.6 -5.1 -5.6 -6.2 -6.8 -7.4
Radio-frequency voltage Vpp/V 800 850 900 950 1000
Electric current/pA -8.0 -8.4 -9.1 -9.2 -9.3
Embodiment 2:
The upper employing of Chinese patent " the ion focusing method of slab construction High-Field Asymmetric Waveform Ion Mobility Spectrometer " (application number 201010619966.5) proposed in Tsing-Hua University has the design of noise reduction function, as shown in Figure 10.The circle migration area bucking electrode 13 increased around upper migration area electrode 6, the loop current increased around current detection electrode 12 detects bucking electrode 14, and difference ground connection.Due to upper migration area electrode 6 surround by migration area bucking electrode 13, current detection electrode 12 surround by current detecting bucking electrode 14, and migration area bucking electrode 13 and current detecting bucking electrode 14 ground connection respectively, so around upper migration area electrode 6 and current detection electrode 12, form respectively zero potential district, and electric field line cannot pass through zero potential district.Thus, the asymmetric waveform radio-frequency voltage that the asymmetric waveform radio-frequency power supply 9 be connected with upper migration area electrode 6 produces can not interfere with current detection electrode 12, and the interference that current detection electrode 12 accepts will reduce greatly, the current signal detected by current detection electrode 12 truly can reflect actual signal.Simultaneously add a direct voltage 15 at lower migration area electrode 7, ion is assembled to center, migration area while separation, reduce the losses of ions brought because of factors such as diffusion, carrier gas disturbances, increase signal strength signal intensity.
Embodiment 3:
The design with noise reduction function is adopted, as shown in figure 11 at Chinese patent " aggregation apparatus of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer and method " (application number 20120211272.7) of Tsing-Hua University's application.The circle migration area bucking electrode 13 increased around upper migration area electrode 6, the loop current increased around current detection electrode 12 detects bucking electrode 14, and difference ground connection.Due to upper migration area electrode 6 surround by migration area bucking electrode 13, current detection electrode 12 surround by current detecting bucking electrode 14, and migration area bucking electrode 13 and current detecting bucking electrode 14 ground connection respectively, so around upper migration area electrode 6 and current detection electrode 12, form respectively zero potential district, and electric field line cannot pass through zero potential district.Thus, the asymmetric waveform radio-frequency voltage that the asymmetric waveform radio-frequency power supply 9 be connected with upper migration area electrode 6 produces can not interfere with current detection electrode 12, and the interference that current detection electrode 12 accepts will reduce greatly, the current signal detected by current detection electrode 12 truly can reflect actual signal.At least one focal zone is set in front end, migration area simultaneously, the upper substrate and subtegulum of each focal zone arranges at least one pair and focuses on pole plate pair, and just right up and down.Simultaneously every secondary focus on pole plate on apply specific voltage, ion was retrained the width of ion beam before entering migration area, reduces the broadening of spectral lines caused because ion disperses in migration area, the resolution of raising system.
Embodiment 4:
MEMS technology is adopted to carry out the system integration to ion focusing type High-Field Asymmetric Waveform Ion Mobility Spectrometer.Ion source 2 adopts the corona discharge ion source of cylinder type, forms by ICP technique etching conductive silicon chip.Upper substrate 4 and subtegulum 5 adopt Pyrex.On-chip upper migration area electrode 6, lower migration area electrode 7, current detecting deflecting electrode 11, current detection electrode 12, migration area bucking electrode 13, current detecting bucking electrode 14 forms (thickness Ti:400 by sputtered with Ti/Pt/Au metal on borosilicate glass pt:300 au:900 ).Substrate is assembled by bonding technology.Adopt the discharge mode of negative corona during experiment, acetic acid sample entrained in carrier gas is ionized.According to the operating characteristic of cylinder type corona discharge ion source, the gas flow rate of carrier gas is adjusted to 100ml/min.Under certain High-Field asymmetric waveform radio-frequency voltage parameter, by dc sweeps bucking voltage, obtain corresponding signal curve, by the substance classes of the comparison determination acetic acid to acetic acid dc sweeps bucking voltage.

Claims (4)

1. have a plate High-Field Asymmetric Waveform Ion Mobility Spectrometer for noise reduction function, described plate High-Field Asymmetric Waveform Ion Mobility Spectrometer comprises ion source (2), migration area (3) and detecting unit (10); Substrate (4) and subtegulum (5) in parallel placement in migration area (3), upper substrate (4) and subtegulum (5) arrange upper migration area electrode (6) and lower migration area electrode (7) respectively, and upper migration area electrode (6) is connected with dc sweeps offset supply (8) with asymmetric waveform radio-frequency power supply (9) respectively; Described detecting unit is made up of current detection electrode (12) and current detecting deflecting electrode (11), current detection electrode (12) is placed on substrate (4), current detecting deflecting electrode (11) is placed on subtegulum (5), it is characterized in that: circle migration area bucking electrode (13) is set around upper migration area electrode (6), one loop current is set around current detection electrode (12) and detects bucking electrode (14), two circle bucking electrodes ground connection respectively; Between upper migration area electrode (6) and migration area bucking electrode (13), and insulate with air or insulating material between current detection electrode (12) and current detecting bucking electrode (14).
2. according to a kind of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer with noise reduction function according to claim 1, it is characterized in that: add a direct voltage (15) in lower migration area electrode (7).
3. according to a kind of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer with noise reduction function according to claim 1, it is characterized in that: in migration area (3) front end, at least one focal zone (16) is set, the upper substrate (4) and subtegulum (5) of each focal zone (16) at least arrange a secondary focusing pole plate pair, and it is just right up and down, simultaneously every secondary focus on pole plate on apply voltage, the voltage applied has two kinds of patterns, and one is direct current focusing mode, and another kind is radio frequency focusing pattern; Direct current focusing mode be focusing pole plate on interval apply identical direct voltage; Radio frequency focusing pattern for every secondary focus on pole plate on apply sinusoidal rf potential, the sinusoidal rf potential phase 180 ° that adjacent focus pole plate is right.
4., according to a kind of plate High-Field Asymmetric Waveform Ion Mobility Spectrometer with noise reduction function described in claim 1,2 or 3, it is characterized in that: the shape of described migration area bucking electrode (13) and the shape of upper migration area electrode (6) identical or different; The shape of described current detecting bucking electrode (14) and the shape of current detection electrode (12) identical or different.
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