CN106504973A - A kind of transference tube of the integration based on ceramic material - Google Patents
A kind of transference tube of the integration based on ceramic material Download PDFInfo
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- CN106504973A CN106504973A CN201710000666.0A CN201710000666A CN106504973A CN 106504973 A CN106504973 A CN 106504973A CN 201710000666 A CN201710000666 A CN 201710000666A CN 106504973 A CN106504973 A CN 106504973A
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- Prior art keywords
- ionization
- migration
- ion
- ionization chamber
- acquisition zone
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/107—Arrangements for using several ion sources
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of transference tube of the integration based on ceramic material, including earthenware, ionization chamber, vacuum ultraviolet-ionization source, ion gate, ion detection device；One end of the ceramic tube inside is ionization chamber, and the indoor top of the ionization and bottom are respectively equipped with relative upper vacuum ultraviolet-ionization source and lower vacuum ultraviolet-ionization source；The other end of the ceramic tube inside is acquisition zone, is provided with the ion detection device in the acquisition zone；Part between the ceramic tube inside ionization chamber and acquisition zone is migration area；Ion gate is provided between the migration area and ionization chamber；The ionization chamber is provided with the outlet of migration gas and carrier gas inlet；The acquisition zone is provided with migration gas entrance；The ionization chamber, migration area and acquisition zone are coaxially disposed.The features such as present invention is using the outstanding insulating properties of ceramic material, excellent mechanical property, suitable surface smoothness, good thermal conductivity is made into one the transference tube of formula.
Description
Technical field
The present invention relates to field of analytic instrument, and in particular to a kind of transference tube based on ceramic material.The migration tube
Ionized using VUV uviol lamps and special ion gate, ionizing efficiency can be effectively improved, improved the resolution of ion mobility spectrometry
Rate, is conducive to the miniaturization of ionic migration spectrometer to produce.
Background technology
Affected by international overflow of drugs, the infiltration of Drug-related crimes overseas makes the Drug-related crimes of China also begin to dying embers again
Combustion, and in the situation for growing in intensity.In order to tackle increasing economic association activity, various safety check equipment also arise at the historic moment.
Ion mobility spectrometry detection technique (ionmobility spectrometry, IMS) as a kind of Broad Spectrum Analysis of Infinitesimal technology, with detection
Speed is fast, sensitivity is high, be easy to miniaturization, low in energy consumption the advantages of, be at present in the world the field such as drug law enforcement, anti-terrorism for trace thing
The mainstream technology of matter Site Detection.The important critical point such as customs, airport has been greatly reinforced to belongings and bag using IMS detection techniques
The monitoring dynamics that wraps up in, has effectively hit the enforcement of the criminal activities such as smuggling traffic in drugs.
Transference tube is the core devices of IMS, is the key factor for realizing the detection of ion high efficiency separation.Based on traditional machine
The concentric structure ion migration tube structure complexity of tool processing technique, single function, integrated level are low；Again due to air-tightness and temperature
Etc. condition cannot precise control, resolution, sensitivity and stability is all undesirable, so as to be dfficult to apply to live independent detection.
Dalian Physical and Chemical Inst. of the Chinese Academy of Sciences proposes a kind of ion migration of array photoemission ionization source
Pipe, before breakthrough, the limitation of single photoemission ionization source, increases substantially light intensity, can greatly improve the ion of ionized region ionization
Number, effectively improves the sensitivity of transference tube.But transference tube is assembled by numerous parts, and structure is more multiple
Miscellaneous, problems are brought to the sealing of migration tube；Secondly, the temperature resistant grade of common engineering plastic product is not high, limit from
The operating temperature of sub- migration tube, have impact on the practical effect of Ion mobility spectrometry.Therefore in recent years high integration from
Sub- migration tube becomes the focus that studies in industry.
Content of the invention
For the deficiencies in the prior art, the present invention is intended to provide a kind of ion migration of the integration based on ceramic material
Pipe, using the outstanding insulating properties of ceramic material, excellent mechanical property, suitable surface smoothness, good thermal conductivity etc.
Feature is made into one the transference tube of formula.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of transference tube of the integration based on ceramic material, including earthenware, ionization chamber, vacuum ultraviolet-ionization
Source, ion gate, ion detection device；One end of the ceramic tube inside is ionization chamber, the indoor top of the ionization and bottom
It is respectively equipped with relative upper vacuum ultraviolet-ionization source and lower vacuum ultraviolet-ionization source；The other end of the ceramic tube inside is collection
Area, is provided with the ion detection device in the acquisition zone；Part between the ceramic tube inside ionization chamber and acquisition zone is
Migration area；Ion gate is provided between the migration area and ionization chamber；The ionization chamber is provided with the outlet of migration gas and carrier gas inlet；Institute
State acquisition zone and be provided with migration gas entrance；The ionization chamber, migration area and acquisition zone are coaxially disposed.
Further, the upper and lower in the upper vacuum ultraviolet-ionization source and lower vacuum ultraviolet-ionization source is respectively arranged
There is becket.
Further, the ion gate is flake structure, and central authorities are provided with regular hexagon hole array, the regular hexagon hole
The outline of array is also in regular hexagon；Spacing between adjacent regular hexagon hole is 0.1mm.
Further, the ion gate adopts polonium Mo alloy 1J85 materials, and surface gold-plating.
Further, the roof and diapire in the migration area is equipped with coaxial metal ring arranged in parallel, and each gold
Mutually isolated and for being placed equidistant between category ring.
Further, the ion detection device is adopted and is provided with institute between Faraday plate, and the acquisition zone and migration area
State aperture plate.
The beneficial effects of the present invention is：
1st, the present invention is using outstanding insulating properties of ceramic material, excellent mechanical property, suitable surface smoothness, good
The features such as good thermal conductivity, using ceramic material as the main body of transference tube, and it is integrated with reaction zone (ionization chamber), migration
Area and acquisition zone, greatly eliminate in the transference tube of traditional structure multiple environmental factorss and technological factor to migration tube
Affect.
2nd, using vacuum ultraviolet-ionization source, the present invention has the advantages which is unique.First, it is not necessary to active material, it is to avoid
Many troubles that radiation management and control brings；Secondly, low-energy photoelectron is only produced, is suppressed the compound reaction in ionization source, is made
The spectrogram for detecting is simpler；Finally, ionizing power can be strengthened to the ultraviolet ionization source to distribution using two, extends ion
The time of ionization source changed by migration tube.
3rd, adopt and high pressure potential well is formed between ionization source and special ion gate with ion of bottling up, by attached on ionization chamber
Plus pulse voltage releases ion, plays good enrichment to the ionic species of ionization chamber, improves the sensitivity of migration tube.
4th, the double mode detection of the negative ions that transference tube achieved by pulse voltage, and multiple by one-time detection
Collection, comprehensive data analysis technology improve the accuracy of detection.
Description of the drawings
Fig. 1 is the cross section structure schematic diagram of the transference tube of the present invention；
Fig. 2 is the three dimensional structure diagram of the transference tube of the present invention
Fig. 3 is the structural representation of the ion gate in Fig. 1；
Fig. 4 is the high pressure schematic diagram in the upper vacuum ultraviolet-ionization source in Fig. 1；
Fig. 5 is the voltage sequential chart of the ionization chamber and ion gate in Fig. 1
Fig. 6 is the VUV-IMS spectrograms of the acetone in embodiment；
Fig. 7 is the VUV-IMS spectrograms of cocaine and acetone (dopant) in embodiment.
Specific embodiment
Below with reference to accompanying drawing, the invention will be further described, it should be noted that the present embodiment is with this technology side
Premised on case, detailed embodiment and specific operating process is given, but protection scope of the present invention is not limited to this reality
Apply example.
As Figure 1-3, a kind of transference tube of the integration based on ceramic material, it is characterised in that including pottery
Pipe (includes that earthenware top 1 and earthenware bottom 9, the earthenware top 1 and earthenware top 9 combine in the present embodiment
Entirety for earthenware), ionization chamber 2, vacuum ultraviolet-ionization source is (using vacuum ultraviolet lamp, including upper vacuum ultraviolet-ionization source
31 and lower vacuum ultraviolet-ionization source 32), ion gate 6, ion detection device 8；One end of the earthenware 1 is the ionization chamber 2
(i.e. reaction zone X), the top and bottom in the ionization chamber 2 are respectively equipped with relative upper vacuum ultraviolet-ionization source 31 and lower vacuum
Ultraviolet ionization source 32；The other end of the earthenware 1 is acquisition zone Z, is provided with the ion detection device 8 in the acquisition zone；
Part between the reaction zone X and acquisition zone Z is migration area Y；The ion is provided between the migration area Y and ionization chamber 2
Door 6；The ionization chamber 2 is provided with migration gas outlet C, and (in the present embodiment, the migration gas outlet is located at the outer of the ionization chamber 2
The overall end in end, i.e. earthenware), and the ionization chamber 2 is additionally provided with carrier gas inlet A (in the present embodiment, the carrier gas enters
Mouth A is on the side wall of ionization chamber 2)；The outer end of the acquisition zone Z is provided with migration gas entrance B；2 (reaction zone of the ionization chamber
X), migration area Y and acquisition zone Z are coaxially disposed.
The ionization interior has essentially formed a reaction zone X, upper vacuum ultraviolet-ionization source and lower vacuum ultraviolet-ionization
Source is oppositely arranged up and down so that the light path in vacuum ultraviolet-ionization source is perpendicular with the axial direction of transference tube, it is to avoid photon is straight
Connect the baseline drift that irradiation ion gate causes.Carrier gas sample introduction from before ion gate, migrates gas and enters from the outer end of ion detection device
In transference tube, finally empty from the outer end of ionization chamber, so as to realize one-way gas flow.
Further, the upper and lower in the upper vacuum ultraviolet-ionization source 31 and lower vacuum ultraviolet-ionization source 32 covers respectively
It is provided with becket 4 and 5.By arranging becket, then applying high pressure in vacuum ultraviolet-ionization source axis direction can make vacuum purple
Outer ionization source forms circular light spot, strengthens the effective area of ionized space.As shown in Figure 4.
The transference tube is bottled up ion using forming high pressure potential well between ionization chamber and special ion gate, sample molecule
After ion is formed in ionization chamber, under normality, add and ion migration electricity in opposite direction on ionization chamber and special ion gate
Pressure signal (as shown in Figure 5), due to the effect of the electric field, ion can be bound in ionization interior, concentrate at the front portion of ion gate,
Now ion gate is closed；When the additional voltage signal of ion gate is removed, ion gate is opened, and ion is entered in migration area in electric field
Travel motion is produced in the presence of power.Ion gate plays good enrichment to the ionic species of ionized region, improves migration
The sensitivity of pipe.
Further, the ion gate 6 is flake structure (shape of cooperation earthenware is rounded in the present embodiment), in
Centre is provided with regular hexagon hole array, and the outline of the regular hexagon hole array is also in regular hexagon；Adjacent regular hexagon hole
Between spacing be 0.1mm.As shown in Figure 3.The ion thickness gate is little, and when ion gate is closed, ion can be very good to concentrate on
Before ion gate, ion gate can timely enter migration area after opening, and the regular hexagon hole array that central authorities are arranged is provided enough
The loss that passes through region, effectively reduce sample ions.
Further, the ion gate 6 adopts polonium Mo alloy 1J85 materials, and carries out gold-plated surface treatment.
Further, in the migration area, the roof and diapire of ceramic tube inside (are the upper pottery in the present embodiment
The inside one side of pipe 1 and lower earthenware 9) on be equipped between groove arranged in parallel, and each groove mutually isolated for etc. between
Away from setting.Equally distributed coaxial metal ring 10, equally distributed metal are provided with the mutually isolated and groove that is equally spaced
Ring can carry out uniform partial pressure to migration area, form uniform electric field.As shown in figure 1, the concentric structure of migration area makes migration electricity
Field maintains constant gradient, and the gradient has focussing force to ion, can reduce the loss of ion.
Further, the ion detection device is adopted and is provided with institute between Faraday plate, and the acquisition zone and migration area
State aperture plate 7.The setting of aperture plate can reduce the faradic impact produced when ion is moved to Faraday plate, and aperture plate can be protected
Card signal is undistorted, has also intercepted impact of other high-frequency noises to ion current signal.
The operation principle of the transference tube is：Testing sample passes through Thermal desorption injector heating and gasifying, in carrier gas
Carrying under, after semi-transparent membrane filtration, by carrier gas inlet A enter transference tube inside.In order to realize negative ions bimodulus
Formula data acquisition, adds pulse voltage as shown in Figure 5 on ionization chamber and ion gate；Under positive ion mode, ionization chamber and ion
Add the positive high voltage of 1000V on door, between ionization chamber and ion gate, form a positive potential well, the sample just ionized for bottling up；Negative
Under ion mode, add the negative high voltage of 1000V on ionization chamber and ion gate, between ionization chamber and ion gate, form a negative potential well,
For bottle up negative electricity from sample.Carrier gas ionizes the sample ions for obtaining under positive ion mode or negative ion mode and passes through pulse
The ion gate of unlatching enters migration area, and the difference according to its mobility in migration area is separated, and finally reaches ion detection
Device, the ion signal received by ion detection device send signal acquiring and processing system to, obtain the VUV-IMS of sample
Spectrogram, for the detection and analysis of sample component.
All parts are encapsulated eventually through inorganic adhesive, constitute linear electric fields and cylindrical streams passage.Achieve from
The integration of sub- drift tube, miniaturization.
Each tubular structure in Fig. 2 shown in top is that each consuming parts such as becket, ionization chamber, ion detection device are drawn
Electrode, for each part that is electrically connected.
Embodiment
The present invention is tested as dopant with cocaine (Cocaine) as sample with acetone (acetone), is utilized
The ion migration of present invention description has been in control their VUV-IMS spectrograms, demonstrates the migration tube in power consumption, leakage current, gas
The excellent properties of the aspects such as close property, sensitivity, resolution and stability.
Experiment condition is：The input mode of dopant acetone and sample cocaine is direct injected, and sample size is controlled to
10ng；Transference tube operating temperature is 250 DEG C, and carrier gas is the air of the purify air filtered through over-molecular sieve and activated carbon,
Carrier gas inlet speed is 200ml/min, migrates gas inlet rate for 200ml/min, migration area field intensity E=250V/cm.Using bag
The ionic migration spectrometer for including above-mentioned transference tube is detected to testing sample.
VUV-IMS spectrograms of the Fig. 6 for acetone, tests the spectrogram peak position for obtaining and is set to 4.35ms, peak height is 6350, half-peak
A width of 0.322ms.Can be calculated by mobility formula, the mobility K of the acetone of the transference tubeC=3.69, reduction is migrated
Rate is 2.12.
Fig. 7 is the VUV-IMS spectrograms of cocaine and acetone (dopant), tests the spectrogram peak position for obtaining and is set to 7.95ms,
Peak height is 6465, a width of 0.647ms of half-peak.Can be calculated by mobility formula, the mobility of the cocaine of the transference tube
KT=2.02, reduction mobility is 1.16.The result of calculation migrates the data in rate database with drugs reduction and matches.
The acetone measured from Fig. 6 and 7, the migration tube and the peak height value of cocaine reach more than 6000, and signal is strong
Degree is higher.The ion concentration of detection signal intensity and arrival detecting electrode is directly proportional, and the migration tube air-tightness of integration is good, sample
Substantially it is not lost from ionization area by way of migration area, sensitivity is higher.
From Fig. 6 and 7, the spectrogram peak position of cocaine is set to 7.95ms, a width of 0.697ms of half-peak.Public according to resolution
Formula is calculated the unimodal resolution of cocaine test experience and is respectively 11.4, and resolution is higher.
For a person skilled in the art, can be made various corresponding according to above technical scheme and design
Change and deform, and all these changes and deformation is should be construed as being included within the protection domain of the claims in the present invention.
Claims (6)
1. a kind of transference tube of the integration based on ceramic material, it is characterised in that including earthenware, ionization chamber, vacuum
Ultraviolet ionization source, ion gate, ion detection device；One end of the ceramic tube inside is ionization chamber, the top of the ionization interior
Portion and bottom are respectively equipped with relative upper vacuum ultraviolet-ionization source and lower vacuum ultraviolet-ionization source；The ceramic tube inside another
Hold as acquisition zone, in the acquisition zone, be provided with the ion detection device；Between the ceramic tube inside ionization chamber and acquisition zone
Part be migration area；Ion gate is provided between the migration area and ionization chamber；The ionization chamber is provided with the outlet of migration gas and carries
Gas entrance；The acquisition zone is provided with migration gas entrance；The ionization chamber, migration area and acquisition zone are coaxially disposed.
2. the transference tube of the integration based on ceramic material according to claim 1, it is characterised in that described true
The upper and lower in empty ultraviolet ionization source and lower vacuum ultraviolet-ionization source is respectively arranged with becket.
3. the transference tube of the integration based on ceramic material according to claim 1, it is characterised in that the ion
Door is flake structure, and central authorities are provided with regular hexagon hole array, and the outline of the regular hexagon hole array is also in regular hexagon；
Spacing between adjacent regular hexagon hole is 0.1mm.
4. the transference tube of the integration based on ceramic material according to claim 1 or 3, it is characterised in that described
Ion gate adopts polonium Mo alloy 1J85 materials, and surface gold-plating.
5. the transference tube of the integration based on ceramic material according to claim 1, it is characterised in that the migration
Roof and diapire in area is equipped with coaxial metal ring arranged in parallel, and mutually isolated between each becket and for equidistantly setting
Put.
6. the transference tube of the integration based on ceramic material according to claim 1, it is characterised in that the ion
Detection device is adopted and is provided with the aperture plate between Faraday plate, and the acquisition zone and migration area.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710000666.0A CN106504973A (en) | 2017-01-03 | 2017-01-03 | A kind of transference tube of the integration based on ceramic material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710000666.0A CN106504973A (en) | 2017-01-03 | 2017-01-03 | A kind of transference tube of the integration based on ceramic material |
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Cited By (5)
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| CN108470672A (en) * | 2018-03-19 | 2018-08-31 | 塔里木大学 | A kind of ion implanting component and its control and data processing method |
| CN108807130A (en) * | 2018-05-03 | 2018-11-13 | 塔里木大学 | A kind of migration tube and ionic migration spectrometer for ionic migration spectrometer |
| CN109243961A (en) * | 2018-09-30 | 2019-01-18 | 镇江华智睿安物联科技有限公司 | A kind of microflow control technique electrode ion migration tube and preparation method thereof |
| CN110310882A (en) * | 2019-07-03 | 2019-10-08 | 清华大学深圳研究生院 | The ion door control method of BN discrimination effects in a kind of improvement ion mobility spectrometry |
| CN112802732A (en) * | 2021-01-07 | 2021-05-14 | 上海奕瑞光电子科技股份有限公司 | Ceramic migration tube and manufacturing method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108470672A (en) * | 2018-03-19 | 2018-08-31 | 塔里木大学 | A kind of ion implanting component and its control and data processing method |
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| CN110310882A (en) * | 2019-07-03 | 2019-10-08 | 清华大学深圳研究生院 | The ion door control method of BN discrimination effects in a kind of improvement ion mobility spectrometry |
| CN110310882B (en) * | 2019-07-03 | 2021-03-12 | 清华大学深圳研究生院 | Ion gate control method for improving discrimination effect of BN gate in ion mobility spectrometry |
| CN112802732A (en) * | 2021-01-07 | 2021-05-14 | 上海奕瑞光电子科技股份有限公司 | Ceramic migration tube and manufacturing method thereof |
| CN112802732B (en) * | 2021-01-07 | 2023-04-07 | 上海奕瑞光电子科技股份有限公司 | Ceramic migration tube and manufacturing method thereof |
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Application publication date: 20170315 |