CN109336047B - Multi-layer structure ion source chip based on MEMS (micro-electromechanical systems) process and mass spectrometry sample introduction system - Google Patents

Multi-layer structure ion source chip based on MEMS (micro-electromechanical systems) process and mass spectrometry sample introduction system Download PDF

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CN109336047B
CN109336047B CN201811168892.0A CN201811168892A CN109336047B CN 109336047 B CN109336047 B CN 109336047B CN 201811168892 A CN201811168892 A CN 201811168892A CN 109336047 B CN109336047 B CN 109336047B
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glass
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silicon
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CN109336047A (en
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刘坤
张�浩
郝明
巴要帅
谢元华
杜广煜
巴德纯
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Northeastern University China
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
    • B81B7/02—Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
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    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/68—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes

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Abstract

The invention relates to an ion source chip with a multilayer structure based on an MEMS (micro-electromechanical system) process, which comprises bottom silicon, middle layer glass, conductive silicon and top layer glass; an electrode layer and carbon nanotubes are arranged on the upper side of the bottom silicon; electrode layers are respectively arranged on two sides of the interlayer glass; an electrode layer is arranged on the lower side of the top glass layer; the bottom layer silicon is combined with the middle layer glass, and the middle layer glass and the top layer glass are respectively combined with the conductive silicon. The area above the middle glass layer corresponding to the carbon nano tube is of a grid structure, high voltage is applied to the lower side electrode layer of the middle glass layer and the bottom silicon electrode layer to excite the carbon nano tube to generate electrons, the electrons penetrate through the grid structure of the middle glass layer to enter an ionization chamber above the middle glass layer, the electrons collide with a gas sample to be detected in the ionization chamber to generate ions, and the ions are extracted, focused and accelerated by an ion extraction and focusing area arranged behind the ionization chamber. The ion source chip has a multilayer structure of silicon-carbon nanotube-glass-silicon-glass, and has the advantages of small volume, light weight, low power consumption, portability and the like.

Description

Multi-layer structure ion source chip based on MEMS (micro-electromechanical systems) process and mass spectrometry sample introduction system
Technical Field
The invention relates to the technical field of mass spectrometry equipment, in particular to a multi-layer structure ion source chip based on an MEMS (micro-electromechanical system) process and a mass spectrometry sample injection system.
Background
Mass spectrometry is a method of separating and detecting according to mass differences of substance atoms, molecules or molecular fragments based on the principle that charged particles can deflect in an electromagnetic field. The traditional mechanical processing method causes the mass spectrometer to have large volume, high price and complex operation steps, can not carry out real-time and rapid detection on the sample, and can only be stored in a laboratory for use. With the continuous development of food safety problems and space exploration activities and the urgent requirements of emergencies and public safety, the development and design of a miniature mass spectrometer device can promote the further application of the miniature mass spectrometer device in the fields of aerospace, military exploration and military and civil fusion, and has important theoretical significance and application value for the innovation of the existing mass spectrometry technology.
With the continued development and sophistication of micro-electro-mechanical systems (MEMS) fabrication methods, the dimensions of mass spectrometers are moving towards smaller orders of magnitude. The mass spectrometer generally comprises a sample feeding system, an ion source, a mass analyzer, a detector and the like. The ion source is a device for ionizing neutral atoms or molecules and extracting ion beams from the neutral atoms or molecules, is an indispensable component in a mass spectrometer, determines the ionization performance of the mass spectrometer and influences the final analysis result.
MEMS fabrication Process (Micro fabrication Process) is a generic term for Micro-structure fabrication Process down to the nanometer scale and up to the millimeter scale, many countries in the world currently use MEMS processing technology to fabricate ion sources, Tassetti C M, Duraflourg L, Danel J S et al A MEMS Electron Impact Source Integrated in a Micro-time-of-flight Mass Spectrometer [ J ]. Sensors & Actuators B Chemical,2013,189(12):173-178. use silicon-glass bonding technology to integrate an Electron Impact ion source and test ionized ionic current, but its Electron source uses an external Electron gun and is not Integrated, so the Micro device has yet to be improved, and the Integrated Electron source is used to integrate a chip constituting a complete MEMS ion source in a chip, HauseschistJ, Waraf E, ü, and the Micro device uses a glass bonding device to integrate a silicon gas source into a silicon gas supply device [ Massachusetts J ] (masware J, Masherd. plasma-plasma ionization device J, Masherd. A MEMS plasma ionization source is also used to prepare a Micro-plasma ionization Mass Spectrometer [ masware J ] (masware J, Masillustrating the Micro device, Masillustrating the use of a gas supply device, Masillustrating the Micro Electron Impact ion source, Masillustrating the use of the MEMS ion source Integrated Electron Impact source.
In summary, the conventional ion source chip has many disadvantages.
Disclosure of Invention
Technical problem to be solved
In order to solve the above problems in the prior art, the present invention provides a multi-layer structure ion source chip based on MEMS process, and the ion source chip of the present invention has a plurality of functional regions such as an ion generating region (including an electron source) and an ion extracting and focusing region along the ion flow direction, so as to greatly reduce the size and power consumption of the ion source and provide an important reference value for the design of a micro ion source.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a multi-layer structure ion source chip based on MEMS technology comprises bottom layer silicon (7), middle layer glass (5), conductive silicon (3) and top layer glass (1) in sequence in the height direction; wherein:
the upper side surface of the bottom layer silicon (7) is provided with a first electrode layer (8) and carbon nano tubes (9); the upper side surface and the lower side surface of the interlayer glass (5) are respectively provided with a second electrode layer (4) and a third electrode layer (6); a fourth electrode layer (2) is arranged on the lower side surface of the top layer glass (1);
the bottom layer silicon (7) is combined with the middle layer glass (5), and the middle layer glass (5) and the top layer glass (1) are both combined with the conductive silicon (3);
the area of the middle layer glass (5) corresponding to the carbon nano tube (9) is of a mesh or grid structure; the third electrode layer (6) of the middle layer glass (5), the first electrode layer (8) on the bottom layer silicon (7) and the carbon nano tubes (9) form an electron generation area (10), and the carbon nano tubes (9) generate electrons under high voltage by applying voltage to the third electrode layer (6) and the first electrode layer (8);
an ionization chamber (13) and an ion extraction and focusing region (16) are formed among the second electrode layer (4) of the middle layer glass (5), the conductive silicon (3) and the fourth electrode layer (2) of the top layer glass (1);
electrons generated by the carbon nano tube (9) under high pressure penetrate through the grid structure of the interlayer glass (5) to enter the ionization chamber (13) and collide with a gas sample to be detected to generate ions, and the generated ions are extracted, focused and accelerated by the ion extraction and focusing area (16).
Wherein, the area of the interlayer glass (5) corresponding to the upper part of the carbon nano tube (9) is processed into the mesh or grid structure (11) by laser.
As a preferred embodiment of the present invention, the electron generation region (10) and the ionization chamber (13) constitute an ion generation region (12).
In a preferred embodiment of the present invention, the carbon nanotubes (9) are grown on the first electrode layer (8) of the underlying silicon (7) by a catalyst growth method or a printing method.
As a preferred embodiment of the invention, the first electrode layer (8) on the bottom silicon (7), the fourth electrode layer (2) of the top glass (1), and the second and third electrode layers (4, 6) on both sides of the middle glass (5) are formed into electrode patterns by sputtering ion plating and etching.
As a preferred embodiment of the invention, the bottom layer silicon (7) is bonded and connected with the middle layer glass (5), and the middle layer glass (5) and the top layer glass (1) are bonded and connected with the conductive silicon (3).
As a preferred embodiment of the invention, the ionization chamber (13) is correspondingly arranged in the grid structure area of the interlayer glass (5), the grid structure area is enclosed in the ionization chamber (13) and is provided with an ion outlet and a capillary sample inlet, and the area enclosed by the ionization chamber (13) is not more than 1mm2。
Preferably, the ionization chamber (13) is rectangular or circular in shape.
As a preferred embodiment of the present invention, the ion extraction and focusing region (16) comprises an extraction electrode (14) and a focusing lens electrode group (15), both the extraction electrode (14) and the focusing lens electrode group (15) being part of the conductive silicon (3); the ion extraction and focusing region (16) is arranged corresponding to the ion outlet direction of the ionization chamber (13).
As a preferred embodiment of the invention, the voltage signs of the extraction electrode (14) and the ionization chamber (13) are opposite, the voltage of the ionization chamber (13) is positive, the voltage of the extraction electrode (14) is negative, and the ions generated in the ionization chamber (13) are extracted through an electric field formed between the extraction electrode (14) and the ionization chamber (13); the middle of the extraction electrode (14) is provided with an opening for the ions to pass through; the focusing lens electrode group (15) comprises an odd number of electrodes larger than 1, and each electrode is provided with an opening in the middle for passing ions.
As a preferred embodiment of the invention, the length, width and height of each electrode in the extraction electrode (14) and the focusing lens electrode group (15) are equal, the width and height of the electrode are not more than 500 mu m, the length of the electrode is not more than 4mm, and the distance between two adjacent electrodes is not more than 0.5 mm.
As a preferred embodiment of the invention, the focusing lens electrode group (15) is composed of 3 or 5 electrodes, the electrode voltages are distributed in a staggered way of 0, V, 0 or 0, V, 0, wherein V is a negative voltage and is used for focusing and outputting the ions extracted from the ionization chamber (13) by the extraction electrode (14).
As a preferred embodiment of the invention, the ionization chamber (13), the extraction electrode (14) and the focusing lens electrode group (15) are arranged in a coaxial line, the ion outlet of the ionization chamber (13), the openings of each electrode in the extraction electrode (14) and the focusing lens electrode group (15) are arranged in a coaxial line, and the opening width of each electrode in the extraction electrode (14) and the focusing lens electrode group (15) is not more than the ion outlet width of the ionization chamber (13); the opening width of the ionization chamber (13) is not more than 500 [ mu ] m.
As a preferred embodiment of the invention, the conductive silicon (3) is etched to form an ionization chamber (13), an extraction electrode (14) and a focusing lens electrode group (15). The upper, lower, fourth and second electrode layers (2, 4) corresponding to the extraction electrode (14) and the focusing lens electrode group (15) are also in the shape consistent with the electrodes, and no opening is left in the middle, so that the upper, lower, fourth and second electrode layers (2, 4) and the corresponding electrodes (the extraction electrode 14 and the focusing lens electrode group 15) enclose a closed loop structure.
In addition, the invention also provides a mass spectrometry sample injection system of the multi-layer structure ion source chip based on the MEMS technology, which comprises the multi-layer structure ion source chip of any embodiment, a capillary guide pipe (17), a one-way valve (18) and a micro piezoelectric pump (19), wherein the capillary guide pipe (17) is connected with the ionization chamber (13), the micro piezoelectric pump (19) sends sample gas to be detected into the ionization chamber (13) through the capillary guide pipe (17) to carry out ionization of the sample to be detected, the one-way valve (18) can prevent the backflow phenomenon, and the micro piezoelectric pump (19) is connected with a power supply and is controlled by a controller to control working parameters of the micro piezoelectric pump.
Preferably, the sampling system further comprises a power supply and a controller, the multilayer structure ion source chip is connected with the power supply through the controller, and the controller inputs and adjusts electric signals to enable the electric signals input by the electrodes to be pulse signals.
Pulsed electrical signals, i.e. 0-t1Time period without electrical signal, t1-t2With a time period of electric signal, with period T-T2. The charged ions are continuously extracted, focused, accelerated and transported into the mass selector by providing a pulsed electrical signal. The input of the pulse electric signal can solve the problem of simultaneously leading out different ions and improve the resolution ratio of the ions.
Preferably, the ion source chip with the multilayer structure is placed in a closed vacuum container (when a sample introduction system is used), and the vacuum degree is not higher than 10-5Pa, a molecular pump (high vacuum pump) and a vortex pump (low vacuum pump) can be combined to vacuumize the closed vacuum container.
(III) advantageous effects
The invention has the beneficial effects that:
① the inventive ion source chip based on MEMS process is designed as a multilayer structure of silicon-Carbon Nanotube (CNT) -glass-silicon-glass, comprising an ion generation region, an ion extraction and focusing region, wherein the ion generation region is integrated with an electron generation region, and has a series of advantages of small volume, light weight, low power consumption, and portability.
② the multi-layer structure ion source based on MEMS technology integrates an ion generating area, an ion extracting and focusing area, greatly improves the processing precision and the integration level, solves the problem of low integration precision of the traditional mechanical processing and assembling, simultaneously improves the ion transmission efficiency, reduces the ion loss and improves the ion source performance.
③ the electrodes in the multilayer structure ion source based on MEMS technology can be connected with the power supply through the controller, the controller inputs and adjusts the electric signals, so that the electric signals input by the electrodes are all pulse signals, which is convenient for the better focusing and extraction of ions with different mass ranges, and improves the resolution of the ions.
④ the multi-layer structure ion source based on MEMS technology uses Carbon Nanotube (CNT) excited by high voltage to generate electrons, and the carbon nanotube has the advantages of good conductivity, excellent mechanical property and chemical stability, low turn-on voltage, high emission current density and small scale when used as a field emission cathode.
Drawings
Fig. 1 is an exploded view of a multi-layered ion source chip based on MEMS process.
Fig. 2 is a schematic diagram of the multi-layer ion source chip based on MEMS technology.
Fig. 3 is a cross-sectional view of a multi-layered structure ion source chip based on MEMS process of the present invention.
Fig. 4 is a schematic diagram of a sample injection system incorporating the multi-layered ion source chip based on MEMS process.
[ description of reference ]
1-top layer glass; 2-top glass lower electrode layer; 3-conductive silicon; 4-interlayer glass upper electrode layer; 5-interlayer glass; 6-interlayer glass lower electrode layer; 7-bottom silicon; 8-a bottom silicon upper electrode layer; 9-Carbon Nanotubes (CNTs) grown on the underlying silicon; 10-electron generation region; 11-a grid structure; 12-an ion generation zone; 13-an ionization chamber; 14-extraction pole; 15-focusing lens electrode group; 16-ion extraction and focusing region; 17: a capillary conduit; 18: a one-way valve; 19: a miniature piezoelectric pump.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail by way of specific embodiments with reference to the accompanying drawings.
The invention is described in further detail below with reference to figures 1, 2 and 3 and the specific examples. Referring to fig. 1 and 3, the ion source chip with a multilayer structure based on the MEMS process of the present invention sequentially includes a bottom layer silicon 7, an intermediate layer glass 5, a conductive silicon 3, and a top layer glass 1 in a height direction.
The upper side surface of the bottom layer silicon 7 is provided with an electrode layer 8 and a carbon nano tube 9, and the upper side surface and the lower side surface of the middle layer glass 5 are respectively provided with an electrode layer 4 and an electrode layer 6. The top glass 1 and the middle glass 5 are combined together, and the middle glass 5 and the top glass 1 are both combined together with the conductive silicon 3. Preferably, the connection is by bonding.
The area of the middle layer glass 5 corresponding to the carbon nano tube 9 is a mesh or grid structure, the electrode layer 6 of the middle layer glass 5, the electrode layer 8 on the bottom layer silicon 7 and the carbon nano tube 9 form an electron generation area 10, and the carbon nano tube 9 generates electrons under high voltage by applying higher voltage to the electrode layer 6 and the electrode layer 8 on the bottom layer silicon 7. An ionization chamber 13 and an ion extraction and focusing region 16 are formed among the electrode layer 4, the conductive silicon 3 and the electrode layer 2 of the intermediate layer glass 5. Electrons generated by the carbon nano tube 9 under high pressure penetrate through the grid structure on the interlayer glass 5 to enter the ionization chamber 13, collide with an input gas sample to be detected to generate ions, and the generated ions are extracted and focused by the ion extraction and focusing area 16.
The invention relates to an ion source chip based on MEMS (micro-electromechanical systems) process, which is designed into a multi-layer bonding structure of silicon-Carbon Nano Tube (CNT) -glass-silicon-glass, and is provided with an ion generating area 12 and an ion extracting and focusing area 16 along the ion flowing direction.
The ion generation region 12 mainly includes an electron generation region 10 and an ionization chamber 13. The electron generation region 10 is composed of an electrode layer 8 on the bottom layer silicon, carbon nanotubes 9 grown on the bottom layer silicon 7, and an electrode layer 6 of the intermediate layer glass 5. The interlayer glass 5 is laser-processed into a mesh or grid structure 11 corresponding to the area above the carbon nanotubes 9. A voltage is applied across the electrode layer 6 on the lower side of the middle layer glass 5 and the lower silicon upper electrode layer 8, causing the carbon nanotubes 9 to generate electrons at a relatively high voltage. The grid structure 11 just allows electrons excited by the Carbon Nanotubes (CNTs) 9 to pass through the interlayer glass 5, enter the ionization chamber 13 above the interlayer glass 5, and collide with molecules of a sample to be detected to generate ions. The ionization chamber 13 is preferably rectangular or circular in shape, and is mainly formed by etching conductive silicon 3 to form an electrode pattern, and then mixing with the electrode patternThe corresponding electrodes of electrode layer 2 and electrode layer 4 are connected to form a closed loop structure of the ionization chamber 13. One side of the ionization chamber 13 is provided with an ion outlet, the other side is provided with a capillary sample inlet connected with the capillary conduit 17, and the area enclosed by the ionization chamber is not more than 1mm2。
As shown in connection with fig. 2, the ion extraction and focusing region 16 mainly includes extraction electrodes 14 and a focusing lens electrode group 15. The extraction electrodes 14 and the focusing lens electrode group 15 have the same length, width and height. Wherein the width and height of the electrodes are not more than 500 μm, the length is not more than 4mm, and the distance between the extraction electrode 14 and each adjacent electrode in the focusing lens electrode group 15 is not more than 0.5 mm. The voltage signs of the extraction electrode 14 and the ionization chamber 13 are opposite, the voltage of the ionization chamber 13 is positive, and the voltage of the extraction electrode 14 is negative (namely, a potential difference exists between the ionization chamber 13 and the extraction electrode 14), so that ions generated in the ionization chamber 13 are extracted through an electric field formed between the extraction electrode 14 and the ionization chamber 13. The extraction electrode 14 has an opening in the middle for the passage of ions.
The focusing lens electrode group 15 is composed of 3 or 5 electrodes, and the electrode voltages are symmetrically distributed at 0, V, 0 or 0, V, 0, where V is a negative voltage for focusing the ions extracted from the ionization chamber 13 by the extraction electrode 14. The focusing lens electrode group 15 has an opening in the middle of each electrode for passing ions.
The ionization chamber 13, the extraction electrode 14 and the focusing lens electrode group 15 are coaxially arranged, the opening width of the electrodes in the extraction electrode 14 and the focusing lens electrode group 15 is on the same extension straight line with the ions in the ionization chamber 13, the opening width of each electrode is not more than the ion outlet width of the ionization chamber 13, and the ion outlet width of the ionization chamber 13 is not more than 500 μm.
The conductive silicon 3 is etched to form the ionization chamber 13, the extraction electrode 14 and the focusing lens electrode group 15, that is: the conductive silicon 3 is etched to form an electrode pattern, and the electrode pattern is connected to the electrode layer 2 or the electrode layer 4, thereby forming a closed loop structure of the ionization chamber 13, the extraction electrode 14, the focus lens electrode group 15, and the like. The electrodes on the upper electrode layer 2 and the lower electrode layer 4, which are correspondingly connected with the ionization chamber 13, are also set to be rectangular or circular without any opening, so that the ionization chamber 13 can form a closed loop. Similarly, the electrodes provided on the electrode layers 2 and 4, which are connected to the extraction electrodes 14 and the focus lens electrode group 15, are also formed in a rectangular shape without any opening in the middle, so that the electrodes form a closed loop.
Among them, Carbon Nanotubes (CNTs) 9 are grown on the electrode layer 8 on the upper side of the underlying silicon 7, and a specific method may be a catalyst growth method or a printing method. The electrode layers (2, 4, 6, 8) on the bottom silicon 7, the top glass 1 and the middle glass 5 can be formed into circuit patterns by sputtering ion plating and etching. The bottom layer silicon 7 is bonded to the middle layer glass 5, and the middle layer glass 5 and the top layer glass 1 are bonded to the conductive silicon 3 between the two layers of glass. The silicon chip and the glass chip or the silicon chip and the silicon chip are bonded together after heating, voltage application or pressure application, and the bonding interface has good air tightness and long-term stability.
Referring to fig. 4, the invention further provides a mass spectrometry sample injection system of the multi-layer structure ion source chip based on the MEMS process, which includes the multi-layer structure ion source chip of the invention, a capillary conduit 17, a check valve 18, a micro piezoelectric pump 19, and the like. The capillary conduit 17 is connected with the ionization chamber 13 of the ion source chip with the multilayer structure (the capillary conduit 17 is inserted into a capillary sample inlet of the ionization chamber 13), the sample to be detected is sent into the ionization chamber 13 through the capillary conduit 17 by the micro piezoelectric pump 19, and the sample to be detected is ionized by the impact of electrons entering the ionization chamber 13 to generate ions. The micro piezoelectric pump 19 is connected to a power supply and is controlled by a controller to control its operating parameters, such as voltage, signal, start-stop time, etc.
The method for realizing the ionization of the gas sample to be detected by using the mass spectrometry sampling system shown in FIG. 4 comprises the following steps:
s1, placing the ion source chip with the multilayer structure into a vacuum container, and vacuumizing the closed vacuum container by combining a molecular pump (high vacuum pump) and a vortex pump (low vacuum pump) to ensure that the vacuum degree is not higher than 10-5Pa。
S2, the gas sample to be tested is sent into the ionization chamber 13 through the capillary conduit 17 by the piezoelectric micro pump 19. Carbon Nanotubes (CNTs) 9 are made to generate electrons at a relatively high voltage by applying a high voltage across the electrode layer 6 on the lower side of the interlayer glass 5 and the electrode layer 8 on the underlying silicon 7. By applying higher voltage between the lower electrode layer 2 of the top glass 1 and the upper electrode layer 8 of the bottom silicon, the generated electrons can pass through the grid area 11 of the middle glass 5 and enter the ionization chamber 13 to collide with a gas sample to be detected to generate ions.
By applying pulse voltage to the ionization chamber 13, the extraction electrode 14, the focusing lens electrode group 15 and the like, generated ions to be detected can be continuously led out of the ionization chamber 13, focused at the focusing lens electrode group 15 and then accelerated to be output, and then enter a subsequent mass analyzer for ion selection and differentiation. The input of the pulse electric signal can solve the problem of simultaneously leading out different ions and improve the resolution ratio of the ions.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. The multi-layer structure ion source chip based on the MEMS process is characterized by sequentially comprising bottom layer silicon (7), middle layer glass (5), conductive silicon (3) and top layer glass (1) in the height direction; wherein:
the upper side surface of the bottom layer silicon (7) is provided with a first electrode layer (8) and carbon nano tubes (9); the upper side surface and the lower side surface of the middle layer glass (5) are respectively provided with a second electrode layer (4) and a third electrode layer (6), and the lower side surface of the top layer glass (1) is provided with a fourth electrode layer (2);
the bottom layer silicon (7) is combined with the middle layer glass (5), and the middle layer glass (5) and the top layer glass (1) are combined with the conductive silicon (3);
the area of the middle layer glass (5) corresponding to the carbon nano tube (9) is of a mesh or grid structure; the third electrode layer (6) of the middle layer glass (5), the first electrode layer (8) on the bottom layer silicon (7) and the carbon nano tubes (9) form an electron generation area (10), and the carbon nano tubes (9) generate electrons under high voltage by applying voltage to the third electrode layer (6) and the first electrode layer (8);
an ionization chamber (13) and an ion extraction and focusing region (16) are formed among the second electrode layer (4) of the middle layer glass (5), the conductive silicon (3) and the fourth electrode layer (2) of the top layer glass (1);
electrons generated by the carbon nano tube (9) under high pressure penetrate through the mesh or grid structure of the interlayer glass (5) to enter the ionization chamber (13) and collide with a gas sample to be detected to generate ions, and the generated ions are extracted, focused and accelerated by the ion extraction and focusing area (16).
2. The multi-layered ion source chip based on MEMS process as claimed in claim 1, wherein the carbon nanotubes (9) are grown on the first electrode layer (8) on the top side of the bottom silicon (7) by catalyst growth method or printing method.
3. The MEMS process based multi-layer structure ion source chip is characterized in that the first electrode layer (8) on the bottom silicon (7), the fourth electrode layer (2) on the top glass (1), the second electrode layer and the third electrode layer (4 and 6) on two sides of the middle glass (5) are formed into an electrode pattern through sputtering ion plating and etching.
4. The MEMS process based multi-layer ion source chip according to claim 1, wherein the bottom layer silicon (7) is bonded to the middle layer glass (5), and the middle layer glass (5) and the top layer glass (1) are bonded to the conductive silicon (3).
5. The MEMS process-based multi-layered ion source chip of claim 1, whereinThe ionization chamber (13) is correspondingly arranged in the grid structure area of the interlayer glass (5), the grid structure area is enclosed in the ionization chamber (13), an ion outlet and a capillary sample inlet are reserved in the ionization chamber (13), and the area enclosed by the ionization chamber (13) is not more than 1mm2。
6. The MEMS process based multi-layer ion source chip according to claim 1, wherein the ion extraction and focusing region (16) comprises an extraction electrode (14) and a focusing lens electrode set (15), both extraction electrode (14) and focusing lens electrode set (15) being part of the conductive silicon (3); the ion extraction and focusing region (16) is arranged corresponding to the ion outlet direction of the ionization chamber (13); the length, width and height of each electrode in the extraction electrode (14) and the focusing lens electrode group (15) are equal, the width and height of the electrodes are not more than 500 mu m, the length of the electrodes is not more than 4mm, and the distance between two adjacent electrodes is not more than 0.5 mm.
7. The MEMS process based multi-layered ion source chip according to claim 6, wherein the voltage of the extraction electrode (14) and the ionization chamber (13) is opposite in sign, the voltage of the ionization chamber (13) is positive, and the voltage of the extraction electrode (14) is negative, for extracting ions generated in the ionization chamber (13) through an electric field formed between the extraction electrode (14) and the ionization chamber (13); the middle of the extraction electrode (14) is provided with an opening for the ions to pass through; the focusing lens electrode group (15) comprises an odd number of electrodes larger than 1, and each electrode is provided with an opening in the middle for passing ions.
8. The MEMS process based multi-layered ion source chip according to claim 7, wherein the focusing lens electrode set (15) consists of 3 or 5 electrodes with voltages in staggered distribution 0, V, 0 or 0, V, 0, where V is a negative voltage for focusing and outputting the ions extracted from the ionization chamber (13) by the extraction electrode (14).
9. The utility model provides a mass spectrometry sampling system of multilayer structure ion source chip based on MEMS technology which characterized in that includes:
the multilayer-structured ion source chip according to any one of claims 1 to 8, a capillary conduit (17), a check valve (18), and a micro piezoelectric pump (19);
the capillary guide pipe (17) is connected with the ionization chamber (13), the micro piezoelectric pump (19) sends gas of a sample to be detected into the ionization chamber (13) through the capillary guide pipe (17) to carry out ionization of the sample to be detected, and the one-way valve (18) can prevent a backflow phenomenon.
10. The mass spectrometry sample introduction system of claim 9, further comprising a power supply and a controller, wherein the multi-layer ion source chip is connected to the power supply through the controller, and the controller inputs and adjusts electrical signals so that the electrical signals input by each electrode are pulse signals; the ion source chip with the multilayer structure is placed in a closed vacuum container, and the vacuum degree is not higher than 10-5Pa。
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