CN101067616B - Longitudinal High Field Asymmetric Waveform Ion Mobility Spectrometer - Google Patents
Longitudinal High Field Asymmetric Waveform Ion Mobility Spectrometer Download PDFInfo
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- CN101067616B CN101067616B CN2007100233228A CN200710023322A CN101067616B CN 101067616 B CN101067616 B CN 101067616B CN 2007100233228 A CN2007100233228 A CN 2007100233228A CN 200710023322 A CN200710023322 A CN 200710023322A CN 101067616 B CN101067616 B CN 101067616B
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Abstract
本发明公开了纵向高场不对称波形离子迁移谱装置，包括介质阻挡放电离化源、屏蔽电极、检测仪。介质阻挡放电离化源包括阻挡介质，即硼硅玻璃及镀于硼硅玻璃上的离化电极和离化电路，屏蔽电极置有分别平行镀于硼硅玻璃上的离化迁移内屏蔽电极、离化迁移外屏蔽电极和迁移检测屏蔽电极。进气样品通过介质阻挡放电离化源被离化、然后进入离子迁移管被分离、最后到达检测仪被检测到。本发明通过集成高离化率的离化源，通过改变装置结构以缩短离子复合时间，使得到达检测区的离子数大幅度增加，并比较容易地被检测到，提高了装置的灵敏度，另一方面通过使用屏蔽电极消除了介质阻挡放电离化源、离子迁移管、检测仪之间的相互影响，提高了装置的稳定性。
The invention discloses a longitudinal high-field asymmetric waveform ion migration spectrometer device, which comprises a dielectric barrier discharge ionization source, a shielding electrode and a detector. Dielectric barrier discharge ionization source includes barrier medium, namely borosilicate glass and ionization electrode and ionization circuit plated on borosilicate glass, the shielding electrode is equipped with ionization migration inner shielding electrode, Ionization migration outer shielding electrode and migration detection shielding electrode. The intake air sample is ionized by the dielectric barrier discharge ionization source, then enters the ion transfer tube to be separated, and finally reaches the detector to be detected. The present invention integrates an ionization source with a high ionization rate and shortens the ion recombination time by changing the structure of the device, so that the number of ions arriving at the detection area is greatly increased and can be detected relatively easily, thereby improving the sensitivity of the device. On the one hand, the mutual influence between the dielectric barrier discharge ionization source, the ion transfer tube and the detector is eliminated by using the shielding electrode, and the stability of the device is improved.
Description
Technical field the present invention relates to can integrated ionization source and the High-Field asymmetric waveform ion migration detection range of guarded electrode, particularly a kind of longitudinal high-field asymmetric waveform ion mobility spectrometry apparatus.
Background technology is along with terroristic wildness, and the air of materials such as explosive, drugs detects down and becomes more and more important.Detector in the past mainly contains mass spectrometer, fast ionic migration spectrometer.
Mass spectrometer is sensitivity and selectivity is good, the reflection time is short very, but that bulky, vacuum tightness requires is high, power consumption is big, cost an arm and a leg, and is not suitable for operating in public places.
Quick ionic migration spectrometer, thereby by the ownership of definite ion mobility judgement of the space flight time of measuring various different ions ion, but its sensitivity depends on the length of migration tube, and length is long more, resolution is easy more to be done highly, and this has directly caused the difficulty of its miniaturization.If must miniaturization, just very high to the requirement of detector so, this can cause the increase of cost.Moreover, there is a lot of materials very approaching, makes and detect the difficulty that becomes in low ion mobility after the match.
To be USSR (Union of Soviet Socialist Republics) the earliest begin to develop in eighties of last century the eighties High-Field asymmetric waveform example mobility spectrometer (FAIMS).Nonlinearities change can take place in its mobility under high electric field action of the ion in the gas, thereby can produce a difference with the mobility under the low electric field, and different ions is under different height electric field actions, the ion mobility difference can be different, therefore the height electric field that on plasma, adds an alternate, different ions just produces different displacements on the direction of electric field, thereby can be separated effectively.Selectivity that FAIMS is high and signal to noise ratio (S/N ratio) have received increasing attention, but it exists that volume is big, cost is high, Measuring Time is long, power is big, be inconvenient to the shortcoming of carrying and being difficult to produce in batches.
Be devoted to the FAIMS miniaturization and obtain effective achievement two companies are arranged, U.S. Sionex company and Canadian Ionalytics company.
Plate minitype ion migration tube is mainly studied by Sionex company, and has released its serial core product microDMx.This small product size is little, and is highly sensitive, detecting first when stupid with the logotype of thorium americium ionization source, and accuracy of detection can reach the 60ppb magnitude.This product can be used in above terminal user's the testing product, such as hand-held detectors and mass spectrometer etc., in March, 2004, Varian Inc company uses the product microDMx of Sionex company to release new product CP-4900 portable gas chromatography detecting device, and this product has entered Chinese market at present.People such as its main researchist La Anan A Miller have applied for related invention patent (CN 1390361A) in China.
Column type minitype ion migration tube is mainly studied by Ionalytics company, principle with plate be the same, just two electrode is respectively the solid cylinder of inside and the drum of outside, disturb less with plate its electric field that is subjected to the external world of comparing, thereby higher sensitivity is arranged, can reach 0.5-0.005ppb as detecting perchlorate with electron spray ionization source (ESI)-mass spectrometer (MS) logotype, be 0.5-1min detection time, but this transference tube column type top is easy to generate corona discharge, so require very high to manufacture craft.
No matter be Sionex company or Ionalytics company, its product all is to exist as the part of analytical instrument, all there are not integrated ionization source and detector, and external ionization source is understood the volume of aggrandizement apparatus on the one hand, can make that on the other hand the distance between ionization source and the migration tube is long, thereby increased plasma recombination time, and can reduce plasma density like this, thereby reduced detectable amount of ions, and this can reduce the sensitivity of device, and can improve the requirement to detector.
The ionization source that can be integrated in the midget plant commonly used has low energy β source, vacuum UV lamp, corona discharge, surface ionization source.
There is very big advantage in low energy β source as ionization source in the device of compactness, but has safety problem, and ionization efficient is low.
But vacuum UV lamp specific aim ionization, and volume is little, be easy to integrated, but its energy is low, therefore about 8-11eV has very big restriction to the species that detected.Vacuum UV lamp is frangible in addition, thus need protection, and As time goes on performance descend, and these have all limited its application.
Corona discharge can use in little space, and high energy can be provided, but is polluted easily.
Surface ionization is used for vacuum system mostly, uses in atmosphere that to have power consumption big, caducous shortcoming.And the device one-piece construction is bigger, is not suitable for integrated.
The patent (CN 1561532A) of " the small-sized capacitive discharge plasma ion source " that draw application such as the people that pacifies the A Miller of Sionex company provides a kind of miniaturization, can be integrated in the ionization source of midget plant, yet, have several significant disadvantages if be integrated in High-Field asymmetric waveform transference tube.One, the region of discharge of this ionization source is very little, thereby makes plasma concentrate on a very little zone, and this can cause the concentration of local plasma excessive, and the plasma recombination velocity is to follow the quadratic power of concentration to be directly proportional, and sensitivity is disadvantageous to Device Testing for this; They are two years old, the ionization district gas channel of this ionization source is much smaller than the gas channel of High-Field unsymmetric ion migration tube, thereby must there be vertically big projection in whole gas channel the inside, can have influence on the lengthwise movement of air-flow in the transference tube like this, and transference tube to work be exactly lengthwise movement by ion, obvious this ionization device can have influence on the stability and the sensitivity of transference tube; They are three years old, the ionization voltage of ionization source is generally more than several kilovolts, its induced voltage on the migration electrode can the motion of article on plasma body in transference tube cause very big influence, and this not only can have influence on the sensitivity of device, also can have influence on the stability of device; Its four, there is complicated microstructure in this ionization device, can give and make and the integrated difficulty of bringing.
Summary of the invention the objective of the invention is: at the deficiency of existing High-Field asymmetric waveform ion mobility spectrometer (FAIMS), propose a kind of longitudinal high-field asymmetric waveform ion mobility spectrometer.
Longitudinal high-field asymmetric waveform ion mobility spectrometer working medium barrier discharge ionization source, claim dielectric impedance corona discharge or voltolising again, be to have insulating medium to insert a kind of nonequilibrium state gas discharge of discharge space, can in hyperbar and very wide frequency range, work, ionization efficient height, discharge stability is even, can be integrated in the transference tube of miniaturization, shortcoming is that ionization voltage is very high, and the parts to other produce interference, the present invention's guarded electrode head it off easily.The present invention adds guarded electrode in different zones, and the electric field that can effectively reduce zones of different disturbs, and improves the stability and the sensitivity of device.
The longitudinal high-field asymmetric waveform ion mobility spectrometer is integrated in one dielectric barrier discharge ionization source, guarded electrode, transference tube, detecting electrode, and by reducing gap, migration area, ionization district and changing gas channel to reduce ion recombination time, High-Field asymmetric waveform ion mobility spectrometer after improving like this has the ability that can work independently, and higher sensitivity, resolution characteristic and stability are arranged.
Technical scheme of the present invention is: a kind of longitudinal high-field asymmetric waveform ion mobility spectrometry apparatus, comprise the dielectric barrier discharge ionization source, transference tube, guarded electrode, detector, extract system, transference tube is equipped with migration electrode and migration circuit, the migration electrode comprises that the first migration electrode and the second migration electrode are directly to be plated on the strip thin metal layer that Pyrex are first Pyrex and the second Pyrex inboard, first Pyrex and second Pyrex are how just the same gas outlet and the air intake opening except first Pyrex, and the position is relative, the migration area is i.e. first gas channel that moves between the electrode and the second migration electrode of migration electrode, and the migration circuit can move electrode a migration voltage is provided for the first migration electrode and second in the migration electrode;
Extract system is equipped with air pump, the gas outlet, air intake opening and by the i.e. rectangle gas channel formed of first Pyrex and second Pyrex and silicon strip of Pyrex, described gas channel comprises the migration area, the ionization district, detection zone and gap, migration area, ionization district, gap, migration area, described ionization district is between migration area and ionization district, described silicon strip comprises the end silicon strip, be the first end silicon strip and the second end silicon strip, the side silicon strip i.e. the first side silicon strip and the second side silicon strip, four rules and regulations bars be sandwiched between first Pyrex in the Pyrex and second Pyrex rectangularly and with Pyrex in first Pyrex and second Pyrex rectangular parallelepiped cavity that is bonded to a sealing;
Particularly: the dielectric barrier discharge ionization source comprises block media, be Pyrex and be plated on ionization electrode and ionization circuit on the Pyrex, Pyrex comprise first Pyrex and second Pyrex, the ionization electrode comprises the first ionization electrode and the second ionization electrode, gas channel between the first ionization electrode and the second ionization electrode is the ionization district, and the ionization circuit provides the high-frequency impulse high pressure for the ionization electrode;
Guarded electrode is equipped with the parallel respectively ionization migration inner screening electrode that is plated on the Pyrex on i.e. first Pyrex and second Pyrex, ionization migration external shield electrode and migration detect guarded electrode, the shape of ionization migration inner screening electrode is rectangle and comprises first ionization migration inner screening electrode and second ionization migration inner screening electrode, ionization migration external shield electrode comprises first ionization migration external shield electrode and second ionization migration external shield electrode, migration detects guarded electrode and comprises that first migration detects guarded electrode and second migration detects guarded electrode, wherein first ionization migration external shield electrode in the ionization migration external shield electrode and second ionization migration external shield electrode and migration detect first migration in the guarded electrode and detect guarded electrode and second migration and detect guarded electrode and be plated on the i.e. outside of first Pyrex and second Pyrex of Pyrex, and first ionization migration inner screening electrode in the ionization migration inner screening electrode and second ionization migration inner screening electrode are plated on the i.e. inboard of first Pyrex and second Pyrex of Pyrex;
Ionization migration inner screening electrode i.e. first ionization migration inner screening electrode and second ionization migration inner screening electrode have covered the major part in gap, migration area, ionization district on directions X; The external shield electrode is moved in i.e. first ionization of ionization migration external shield electrode and second ionization migration external shield electrode has covered gap, migration area, ionization district major part on directions X and the migration electrode is the fraction that the first migration electrode and second moves electrode; Migration detects i.e. first migration of guarded electrode and detects guarded electrode and second migration and detect guarded electrode covered the i.e. i.e. major part of first detecting electrode and second detecting electrode of the fraction of the first migration electrode and the second migration electrode and detecting electrode of migration electrode on directions X;
Detector is equipped with detecting electrode and testing circuit, detecting electrode comprises first detecting electrode and second detecting electrode, be to be plated on the rectangular metal thin layer that Pyrex are first Pyrex and second Pyrex outside, size on the Y direction is equal to or less than the migration electrode, detecting electrode is that the gas channel between first detecting electrode and second detecting electrode is a detection zone, and testing circuit is equipped with direct voltage source and Pi Anbiao;
The air inlet sample under the extract system effect successively by ionization district, migration area, detection zone, the air inlet sample earlier in the ionization district by ionization, become low temperature plasma, become plasma to enter the migration area then, non-determinand ion wherein is filtered under the effect of migration voltage, have only the determinand ion to enter detection zone with air-flow, flow to detecting electrode i.e. first detecting electrode and second detecting electrode formation electric current under the effect of detection voltage, the Pi Anbiao in the detected circuit detects.
As a further improvement of existing technologies, the block media Pyrex promptly first Pyrex and second Pyrex be in the ionization electrode promptly the part between the first ionization electrode and the second ionization electrode can be processed into column, tip-shape;
The ionization electrode is that the first ionization electrode and the second ionization electrode shape comprise pectination, latticed, square, circular, and the first ionization electrode and the interelectrode distance of second ionization and ionization district size can both change;
Ionization migration inner screening electrode, ionization migration external shield electrode, migration electrode, migration detect all ground connection of guarded electrode, and the electrode material that ionization electrode, ionization migration inner screening electrode, ionization migration external shield electrode, migration electrode, migration detect guarded electrode, detecting electrode is metal material titanium, gold or the platinum that chemical property is stable in air;
Ionization migration external shield electrode is that the external shield electrode is moved in first ionization and second ionization migration external shield electrode is that first migration detects guarded electrode and the second migration detection guarded electrode can be made an electrode with migration detection guarded electrode, i.e. first ionization migration external shield electrode and first migration detect guarded electrode and can make an electrode, and second ionization migration external shield electrode and second migration detect guarded electrode and can make an electrode;
Gap, migration area, ionization district, because of the effect of guarded electrode can do very little, the size on the Y direction can be dwindled five times.
Beneficial effect of the present invention: weak point in the prior art is: at first the very for a short time concentration of local plasma that causes of the region of discharge of ionization source is excessive, and the plasma recombination velocity is to follow the quadratic power of concentration to be directly proportional, and sensitivity is disadvantageous to Device Testing for this; Secondly the ionization district gas channel of this ionization source is much smaller than the gas channel of High-Field unsymmetric ion migration tube, can cause like this that there is lengthwise movement in air-flow in the transference tube, and transference tube to work be exactly lengthwise movement by ion, stability and sensitivity that obvious this ionization device can have influence on; The ionization voltage of ionization source is generally more than several kilovolts once more, and its induced voltage on the migration electrode can the motion of article on plasma body in transference tube cause very big influence, and this also can influence the sensitivity and the stability of transference tube; There is complicated microstructure in this in addition ionization device, can give and make and the integrated difficulty of bringing.
A kind of longitudinal high-field asymmetric waveform ion mobility spectrometry apparatus among the present invention, comprise dielectric barrier discharge ionization source, transference tube, guarded electrode, detector, extract system, the dielectric barrier discharge ionization source comprises block media, be Pyrex and be plated on ionization electrode and ionization circuit on the Pyrex that guarded electrode is equipped with parallel respectively ionization migration inner screening electrode, ionization migration external shield electrode and the migration that is plated on the Pyrex and detects guarded electrode.Ionization migration inner screening electrode, the effect of ionization migration external shield electrode is the phase mutual interference that reduces between ionization source and the migration tube, it is the interference that reduces to move the electrode pair detecting electrode that migration detects the guarded electrode effect. the air inlet sample under the extract system effect successively by the ionization district, the migration area, detection zone, earlier in the ionization district by ionization, become low temperature plasma, become plasma to enter the migration area then, non-determinand ion wherein is filtered under the effect of migration voltage, have only the determinand ion to enter detection zone with air-flow, flow to detecting electrode and form electric current under the effect of detection voltage, the Pi Anbiao in the detected circuit detects.
Hence one can see that, the invention has the beneficial effects as follows:
One, the present invention is integrated in ionization electrode, block media, guarded electrode, migration electrode, detecting electrode on two relative Pyrex, realized the integrated of ionization source, transference tube, detector, make longitudinal high-field asymmetric waveform ion mobility spectrometry apparatus have the ability that works alone, realized the miniaturization of longitudinal high-field asymmetric waveform ion mobility spectrometry apparatus and integrated.
Its two, ionization source of the present invention is the dielectric barrier discharge ionization source, ionization efficient height, ionization zone is big, and the plasma of high concentration can be provided; There is not big projection in the ionization district of ionization source on vertically, that is to say that air communication crosses the motion of ionization district on can not existing vertically, thereby the lengthwise movement in the migration area can not impact to ion.
They are three years old, guarded electrode of the present invention is used to eliminate influencing each other of electric field between ionization district, migration area, the detection zone, especially influencing each other between ionization district and the migration area, under identical condition, add that the later ionization district of guarded electrode can reduce more than 100 times the influence of migration area, arrives negligible degree.Simultaneously, the increase of guarded electrode makes the gap between ionization district and the migration area to shorten as far as possible, can reduce the recombination time of plasma like this, increases the plasma density that arrives the migration area, thus the sensitivity that has improved transference tube.
Its four, the present invention is because of the effect of integrated ionization source and guarded electrode, makes the height that arrives the more external ionization source of number of ions of detection zone by transference tube, thereby pick-up unit required lower, can directly detect with Pi Anbiao.
They are five years old, apparatus of the present invention manufacture craft mainly comprises the making of ionization source and the making of guarded electrode, the ionization source major parameter comprises ionization electrode shape, ionization electrode separation, ionization district size, dielectric thickness, shape of medium, the major parameter of guarded electrode comprises the size and the position of guarded electrode, the manufacture craft that realizes these parameters comprises the evaporation of the electrode on the burn into Pyrex of Pyrex, the bonding of Pyrex, because do not have complicated microstructure, so manufacture craft is all simpler.
Description of drawings
Figure 1A is the texture edge synoptic diagram of apparatus of the present invention.
Figure 1B is the structure schematic top plan view of apparatus of the present invention.
Fig. 2 A is the pectination ionization electrode synoptic diagram of ionization source.
Fig. 2 B is the latticed ionization electrode synoptic diagram of ionization source.
The synoptic diagram of Fig. 3 ionization source ionization for a change area size.
Fig. 4 A is for increasing ionization source ionization electrode separation synoptic diagram.
Fig. 4 B is for reducing ionization source ionization electrode separation synoptic diagram.
Fig. 5 A is an ionization source column block media synoptic diagram.
Fig. 5 B is the most advanced and sophisticated block media synoptic diagram of ionization source.
Fig. 6 A is the air motion synoptic diagram when having Z direction projection in the gas channel.
Fig. 6 B is a kind of embodiment synoptic diagram of migration area, ionization district gap flow passage.
Fig. 7 is the transference tube fundamental diagram.
Fig. 8 is the shield effectiveness comparison diagram of guarded electrode.
Fig. 9 is the detector structural representation.
Embodiment is further explained embodiments of the invention below in conjunction with accompanying drawing
Figure 1A is the texture edge synoptic diagram of apparatus of the present invention.In Fig. 1:
The 1st, Pyrex comprise first Pyrex and second Pyrex;
The 2nd, the ionization electrode comprises the first ionization electrode and the second ionization electrode;
The 3rd, ionization migration inner screening electrode comprises first ionization migration inner screening electrode and second ionization migration inner screening electrode;
The 4th, ionization migration external shield electrode comprises first ionization migration external shield electrode and second ionization migration external shield electrode;
The 5th, the migration electrode comprises the first migration electrode and the second migration electrode;
The 6th, migration detects guarded electrode, comprises that first migration detects guarded electrode and second migration detects guarded electrode;
The 7th, detecting electrode comprises first detecting electrode and second detecting electrode;
The 8th, air pump; The 9th, the gas outlet;
The 10th, the end silicon strip comprises the first end silicon strip and the second end silicon strip;
The 11st, detection zone; The 12nd, testing circuit; The 13rd, the migration circuit; The 14th, the migration area;
The 15th, gap, migration area, ionization district; The 16th, the ionization circuit; The 17th, the ionization district;
The 18th, air intake opening; The 19th, the air inlet sample; The 20th, gas channel;
The 21st, the side silicon strip comprises the first side silicon strip and the second side silicon strip.
Longitudinal high-field asymmetric waveform ion mobility spectrometry apparatus among Figure 1A comprises dielectric barrier discharge ionization source, transference tube, guarded electrode, detector, extract system.
The dielectric barrier discharge ionization source comprises ionization electrode 2 and the ionization circuit 16 that directly is coated with on the block media Pyrex 1; Transference tube is equipped with migration electrode 5 and migration circuit 13; Guarded electrode comprises that parallel respectively ionization migration inner screening electrode 3, ionization migration external shield electrode 4 and the migration that is plated on the Pyrex 1 detects guarded electrode 6; Detector is equipped with detecting electrode 7 and testing circuit 12, and testing circuit 12 is equipped with direct voltage source and Pi Anbiao; The rectangle gas channel 20 that extract system is equipped with air pump 8, gas outlet 9, air intake opening 18 and is made up of Pyrex 1 and silicon strip, silicon strip is promptly held silicon strip 10 and side silicon strip 21, its middle-end silicon strip 10 comprises the first end silicon strip and the second end silicon strip, side silicon strip 21 comprises the first side silicon strip and the second side silicon strip, gas channel 20 comprises migration area 14, ionization district 17, detection zone 11 and gap, migration area, ionization district 15, and gap, migration area 15, ionization district is between migration area 14 and ionization district 17;
Pyrex 1 comprise first Pyrex and the second following Pyrex of device above the device, and wherein first Pyrex are equipped with air admission hole 18 and venthole 9.First Pyrex in the Pyrex 1 and second Pyrex are by the first end silicon strip in the end silicon strip 10 and first side silicon strip in the second end silicon strip and the side silicon strip 21 and the support of the second side silicon strip, utilize the bonding techniques bonding to be combined into a rectangle, end silicon strip 10 and side silicon strip 21 can oxidation also can not oxidation.Air-flow is entered by air intake opening 18, and discharge gas outlet 9, and the used air pump 8 of apparatus of the present invention is a micropump, and volume is little, several watts approximately of power.
The ionization mode of ionization source of the present invention is a dielectric barrier discharge, and the Pyrex 1 that are positioned at 2 at ionization electrode are block medias, the gas channel 20 that is positioned at wherein is region of discharge, the discharge that apparatus of the present invention adopt is the high-frequency impulse discharge, frequency is the magnitude of M, recurrence interval is the ms magnitude, and discharge power is about several watts.
As a kind of embodiment, what Pyrex 1 also can be by other has high-k, easily processing, a cheap material substitution; The rectangle that end silicon strip 10 and side silicon strip 21 bondings form can directly be reduced by silicon strip and form, and it is higher to do seal degree like this, but technology is complicated.
Figure 1B is the structure schematic top plan view of apparatus of the present invention.In Figure 1B, can more clearly see the structure of auto levelizer integral body, ionization electrode 2, ionization migration external shield electrode 4, migration detect the outside surface that guarded electrode 6 is positioned at device, and ionization migration inner screening electrode 3, migration electrode 5, detecting electrode 7 is positioned at the device inside surface.
Guarded electrode comprises that external shield electrode 4 i.e. first ionization migration external shield electrodes are moved in ionization migration inner screening electrode 3 i.e. first ionization migration inner screening electrodes and second ionization migration inner screening electrode, ionization and second ionization migration external shield electrode, i.e. first migration of migration detection guarded electrode 6 detect the guarded electrode and the second migration detection guarded electrode.The width of guarded electrode is wider than other electrode, use guarded electrode purpose is that ionization electrode 2 is the first ionization electrode and the second ionization electrode, promptly the first migration electrode and second moves electrode to migration electrode 5, detecting electrode 7 is influencing each other between first detecting electrode and second detecting electrode in order to reduce, and all guarded electrodes are ground connection all.
The discharge uniformity coefficient of ionization source, ionization efficient, discharge power etc. are also followed shape, the spacing of ionization electrode 2, block media shape, thickness, and ionization district 17 sizes etc. are relevant.
Fig. 2 A is the pectination ionization electrode synoptic diagram of ionization source.Fig. 2 B is the latticed ionization electrode synoptic diagram of ionization source.
The shape of ionization electrode is relevant with the discharge degree of uniformity, and in the present invention, as a kind of embodiment, ionization electrode 2 can be made comb dress or latticed, and such ionization electrode manufacture craft is simple.
The synoptic diagram of Fig. 3 ionization source ionization for a change area size.
The size of region of discharge is relevant with the degree of uniformity of plasma, in the present invention, as a kind of embodiment, thereby can corrode the size that increases ionization district 17, and be very simple in the hole of a given shape of Pyrex 1 inboard corrosion to the block media inboard.
Fig. 4 A is for increasing ionization source ionization electrode separation synoptic diagram.Fig. 4 B is for reducing ionization source ionization electrode separation synoptic diagram.
The spacing of ionization electrode 2 is relevant with distribution with the size of the field intensity in the ionization district 17, and the size of field intensity is relevant with the discharge degree of uniformity with discharge power with distribution.In the present invention, as a kind of embodiment, just can change the spacing of ionization electrode 2 by the thickness that increases or reduce medium, the increase dielectric thickness only needs the Pyrex of specific region bonding on Pyrex 1, and at this making ionization electrode on glass, the Pyrex thickness of institute's bonding depends on the needs again, only need in hole of corrosion, specific region and reduce dielectric thickness, the degree of depth in hole also depends on the needs, and makes the ionization electrode then in this hole, and these technologies are all uncomplicated.
Fig. 5 A is an ionization source column block media synoptic diagram.Fig. 5 B is the most advanced and sophisticated block media synoptic diagram of ionization source.
The shape of medium is relevant with the Electric Field Distribution in the ionization district 17, and Electric Field Distribution is relevant with the discharge degree of uniformity with discharge power.In the present invention,, the shape of block media can be made into column or tip-shape, and these need and be in part between the ionization electrode 2 at Pyrex 1 and corrode and get final product as a kind of embodiment.
Fig. 6 A is the air motion synoptic diagram when having Z direction projection in the gas channel.Fig. 6 B is a kind of embodiment synoptic diagram of migration area, ionization district gap flow passage.
The very little about 3mm of the spacing of ionization electrode 2 of the present invention and migration area 14, the purpose of doing like this is in order to reduce ion recombination time, under atmospheric conditions, the plasma that the dielectric barrier discharge ionization source is produced can be totally compound in 10ms, therefore will shorten recombination time as far as possible.Improving gas velocity is a selection, but the raising of gas velocity can increase the length of migration electrode 5, and this is disadvantageous to microminiaturization.As a kind of embodiment, the sectional area that reduces gap, migration area, ionization district 15 can reduce the time that ion passes through.
The sectional area that reduces gap, migration area, ionization district 15 can reach by the length that reduces Y direction or Z direction.If reduce the passage length of Z direction, then must there be big projection in the gas channel Z direction, Fig. 6 A is the air motion synoptic diagram when existence is protruding up and down in the gas channel, this can make the motion of 14 li in the migration area in air-flow that longitudinal component is arranged, and the transference tube principle of work that is equipped with migration electrode 5 and migration circuit 13 is exactly the lengthwise movement by ion, and this obviously can have influence on the sensitivity and the stability of transference tube.
As an embodiment, can reduce gap, migration area, ionization district 15 width, as Fig. 6 B in the Y direction.Air-flow flows to migration area 14 from ionization district 17, and 15 make a Y direction arcuation projection barrier air to improve the flowing velocity of air-flow in gap, migration area, ionization district 15 in gap, migration area, ionization district.Gas channel 20 sectional areas of the present invention are very little, can tolerate very high gas velocity and be unlikely to produce turbulent flow, and the projection on the Y direction can't change the motion of air-flow on the Z direction, therefore can not have influence on the Z direction motion of ion in migration area 14, promptly can not have influence on the stability and the sensitivity of transference tube.
Fig. 7 is the transference tube fundamental diagram.
The 22nd, be added in the alternating electric field in the migration area 14,23 is that three kinds of different material A, B, the C ion mobility under different electric field actions changes synoptic diagram.
The ion that comes out from ionization district 17, separated in migration area 14 through gap, migration area 15, ionization district.At migration electrode 5 is to add asymmetric friendship voltage frequently on the first migration electrode and the second migration electrode, produce by high frequency signal generator, this friendship frequency voltage is asymmetric friendship frequency electric field of 14 generations in the migration area, about 10000～the 20000V/cm of the High-Field of electric field, low 200～2000V/cm, frequency is in the magnitude of M, and the dutycycle of High-Field and low field is variable, the waveform of voltage can be a square wave, also can be several different friendships stacks of signal frequently.
Different ions has different mobilities, even if mobility is close after the match hanging down, when high electric field, also have very big difference, as Fig. 7 upper right 23 shown in, when high electric field, mobility no longer is a definite value, but the amount with electric field change, and be non-linear, on migration electrode 5, add the asymmetric frequency voltage of handing in migration area 14, to produce a low suitable E
MinWith High-Field E
MaxUnder asymmetric action of alternative electric field, the motion of ion in migration area 14 is the translation on the directions X and the vibration of Z direction, if the vibration of ion on Z direction amplitude up and down is identical then by migration area 14, if then ion inequality can arrive migration the electrode 5 i.e. first migration electrode and the second migration electrode and be neutralized, the ion by migration area 14 is detected at detection zone 11.If add a direct current scan bias voltage in migration again on the electrode 5, each ion to be detected can descend by migration area 14 in certain scan bias voltage, these different scan bias voltage are just corresponding different ion.
Fig. 8 is the shield effectiveness comparison diagram of guarded electrode.
Ionization migration inner screening electrode 3 and ionization migration external shield electrode 4 are used to eliminate the influence to ion motion of electric field that the high voltage of ionization electrode 2 produces in migration area 14.In order to reflect shield effectiveness more clearly, get under the specified conditions one group and test resulting result and make comparisons.
In experiment, each parameter is as follows: get ionization migration inner screening electrode 3 and ionization migration external shield electrode 4 on directions X, cover gap, migration area, ionization district 15 2/3, cover 1/3 of migration area 14, ionization electrode 2 is taken as the square of 1cm * 1cm, migration electrode 5 is taken as the rectangle of 2cm * 1cm, wherein on the directions X 2cm, on the Y direction 1cm, ionization migration inner screening electrode 3 and ionization migration external shield electrode 4 width on the Y direction is got the voltage peak 5000V of ionization electrode 2 greater than the 2mm of ionization electrode 2 and migration electrode 5.Under these conditions, compare the effect that gap, migration area, ionization district 15 different size on directions X reflects shielding.
Fig. 8 transverse axis is the size of gap, migration area, ionization district 15 on directions X, and the longitudinal axis is the induction field of ionization voltage on migration area 14, and for the convenience of mapping, the data on the longitudinal axis have all been got natural logarithm.Ionization electrode 2 and migration electrode 5 spacings are 1.5mm respectively, 2.4mm, 3.0mm, when not shielding, induction field in the migration area is respectively 700V/cm, 212V/cm, 167V/cm, and in the migration area low about 200～1500V/cm of the asymmetric electric field of 14 centrifugations, obviously have very big influence, after having added ionization migration external shield electrode 4, induction field is respectively 18.2V/cm, 4.4V/cm, 3.6V/cm, dropped to original about 1/50, if add ionization migration inner screening electrode 3, then further reduce, induction field will be respectively 4.5V/cm, 1.5V/cm, 1.1V/cm, influence is reduced to former about 1/150, and so low induction field can be ignored the influence of the ion motion of 14 li of migration areas.
Ion to be detected is by after the migration area 14, enter detection zone 11, make migration and detect guarded electrode 6 between migration area 14 and detection zone 11, its order is that added migration voltage is to the influence of ion motion in the detection zone 11 on the elimination migration electrode 5, and migration detects guarded electrode 6 ground connection.
Fig. 9 is the detector structural representation.
The 24th, direct voltage source, the 25th, Pi Anbiao.
When treating that measured ion passes through detection zone 11, under the effect of direct voltage source 24, will arrive detecting electrode 7, so just produce electric current for 12 li, thereby detected by skin peace table 25 at testing circuit.
In the device of external ionization source, cause plasma density to reduce because ion recombination time is very long, thereby the number of ions that arrives detection zone 11 seldom, therefore needs the electric charge multiplying arrangement.In the present invention, the plasma density that ionization source produced is big, the most important thing is that ion is short recombination time, makes that the number of ions that arrives detection zone 11 is more, thereby can directly detect with skin peace table 25.
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