CN117373896A - Electrostatic ion trap, manufacturing method thereof and mass spectrometer - Google Patents
Electrostatic ion trap, manufacturing method thereof and mass spectrometer Download PDFInfo
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- CN117373896A CN117373896A CN202311239037.5A CN202311239037A CN117373896A CN 117373896 A CN117373896 A CN 117373896A CN 202311239037 A CN202311239037 A CN 202311239037A CN 117373896 A CN117373896 A CN 117373896A
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- 238000005040 ion trap Methods 0.000 title claims abstract description 108
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 7
- 238000003466 welding Methods 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 238000005476 soldering Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
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Classifications
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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
- H01J49/062—Ion guides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/22—Electrostatic deflection
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
Abstract
The invention discloses an electrostatic ion trap, a manufacturing method thereof and a mass spectrometer, and belongs to the technical field of mass spectrometers. The electrostatic ion trap comprises a first electrostatic ion trap layer and a second electrostatic ion trap layer which are symmetrically assembled; the first electrostatic ion trap layer and the second electrostatic ion trap layer comprise insulating material discs, a plurality of electrodes and leads; the insulating material disc is provided with a plurality of concentric grooves, concentric annular protrusions are formed between two adjacent concentric grooves, the surface of each concentric annular protrusion is provided with a metal film to form a single electrode, and the lead wire is arranged on the surface or inside the insulating material disc and used for applying voltage to the electrode. The electrostatic ion trap is suitable for ultra-high vacuum, high voltage and other environments, and has high thermal stability, high resolution and high accuracy of detection results. The manufacturing method is simple, has higher precision, can reduce processing residues and improves the stability of products. The mass spectrometer with the electrostatic ion trap has a good application prospect.
Description
Cross Reference to Related Applications
The present application claims priority from chinese patent application No. 202310024914.0, entitled "an electrostatic ion trap and method of making same, and mass spectrometer" filed on month 09 2023, 01, which is incorporated herein by reference in its entirety.
Technical Field
The invention relates to the technical field of mass spectrometry instruments, in particular to an electrostatic ion trap, a manufacturing method thereof and a mass spectrometer.
Background
Resolution is one of the most important properties of mass spectrometry instruments, and the higher the resolution, the better the instrument performance. The current method for improving resolution is to lengthen the ion Flight path and increase the acquisition Time, corresponding to the MR-TOF (Multi-reflection Time-of-Flight) and FTMS (Fourier Transform Mass Spectrometer), respectively. MR-TOF detection time is fast, but folding ion flight path tends to cause mass range to be narrowed, if not folded, the ultra-long flight path can cause the volume of the instrument to be very huge, the problem is not completely solved at present, and the application range of the instrument is limited.
The main stream FTMS is divided into FT-ICR (Fourier Transform Ion Cyclotron Resonance) and Orbitrap, wherein FT-ICR is the mass spectrum with the highest resolution, but the FTMS is not widely applied because of the huge size and high use and maintenance cost. The other Orbitrap has high resolution, small volume and moderate price, and is the most successful ultra-high resolution mass spectrum in the last ten years, but the ultra-high (submicron-level) processing precision and the patent protection of the Simer flight make other teams unable to easily realize the development of the same type of instrument.
In recent years, a plurality of groups are exploring the possibility of novel ultra-high resolution mass spectrum, for example, an MR-TOF structure is adopted, a mirror charge detection method is introduced, a mass spectrum is analyzed by utilizing Fourier transform, and a novel ion trap mass spectrum with resolution of more than one hundred thousand is successfully developed, but the ion trap still has the problem of large space charge effect.
At present, partial schemes optimize the structure of an electrode in an ion trap so as to reduce the electrode voltage and reduce the discharge risk in the ion trap. But ions are trapped in the ion trap to stably and periodically oscillate, and a periodic mirror current signal is generated on an induction electrode in the oscillation process and is acquired and converted into a mass spectrogram. According to the working mode of the ion trap, a plurality of electrodes are needed to play roles of adjustable electric field in the trap, controllable working time sequence of the ion trap, chromatic aberration focusing of ion track and the like. Secondly, the machining error and assembly error of the electrode can distort the electric field in the trap, and the mechanical error of the electrode needs to be controlled to be about tens of micrometers. Finally, in order to reduce the influence of space charge effect, a disc type structure is adopted, the concentric ring electrodes of one circle need to be supported respectively, and the two halves need to be supported face to be matched into a complete ion trap.
That is, the disc-type ion trap described above is subject to the problems of a large number of electrodes, high tolerance requirements, complicated assembly support, and the like. The above problems cause difficulty in ensuring assembly accuracy in the method of mounting the metal electrode on the insulator base with conventional fasteners. Although roundness, symmetry and coaxiality of each ring electrode can be realized through finish machining after assembly, the process is complex, oil pollution and scraps generated by subsequent machining can remain in and are not easy to clean, vacuum degree and device pressure resistance can be affected, electric discharge is caused during working, and the residues are required to be completely cleaned up if being completely cleaned, but the precision which is originally realized through finish machining can be destroyed by disassembly and reassembly.
In addition, some methods in the prior art are to firstly metalize the bonding surface of an insulating substrate (such as a ceramic material) and then weld a metal electrode on the surface of the insulating substrate; there is also a method of bonding with an adhesive agent used in vacuum such as epoxy resin.
However, in the former scheme, the thermal stability of the welding and bonding process is poor, and most of materials of metal and ceramic have different thermal expansion coefficients, so that stress is generated between the metal and the ceramic during subsequent baking and vacuumizing to crack the ceramic; the latter solution is performed under ultra-high vacuum (10 -8 Pa), the vacuum glue can have a deflation phenomenon, and the vacuum degree is influenced by a gluing method.
In view of this, the present invention has been made.
Disclosure of Invention
One of the purposes of the invention is to provide an electrostatic ion trap which is suitable for the environment such as ultra-high vacuum, high voltage and the like, and has high thermal stability, high resolution and high accuracy of detection results.
The second object of the present invention is to provide a method for manufacturing the electrostatic ion trap, which has simple process, high precision, reduced processing residues, and improved product stability and mass spectrometer.
It is a further object of the present invention to provide a mass spectrometer comprising an electrostatic ion trap as described above.
The application can be realized as follows:
in a first aspect, the present application provides an electrostatic ion trap comprising a first electrostatic ion trap layer and a second electrostatic ion trap layer symmetrically assembled;
the first electrostatic ion trap layer and the second electrostatic ion trap layer comprise insulating material discs, a plurality of electrodes and leads;
the insulating material disc is provided with a plurality of concentric grooves, concentric annular protrusions are formed between two adjacent concentric grooves, the surface of each concentric annular protrusion is provided with a metal film to form a single electrode, and the lead wire is arranged on the surface or inside the insulating material disc and used for applying voltage to the electrode.
In an alternative embodiment, the plurality of electrodes includes a first electrode group for forming an ion entrance channel, a gate electrode for controlling the ion entrance state into the ion trap, and a second electrode group for forming the ion trap, which are disposed from outside to inside in a radial direction of the insulating material disk.
In an alternative embodiment, the first electrode set comprises at least 3 concentric ring electrodes; and/or the gate electrode is a concentric ring electrode; and/or the second electrode group comprises at least 4 concentric ring electrodes.
In an alternative embodiment, the first electrode group comprises a first concentric ring electrode, a second concentric ring electrode and a third concentric ring electrode which are arranged from outside to inside along the radial direction of the insulating material disc; the first concentric ring electrode and the second concentric ring electrode and the third concentric ring electrode form an ion inlet channel together;
the gate electrode is a fourth concentric ring electrode;
the second electrode group comprises a fifth concentric ring electrode, a sixth concentric ring electrode, a seventh concentric ring electrode, an eighth concentric ring electrode and a ninth concentric ring electrode which are arranged from outside to inside along the radial direction of the insulating material disc, and the areas between the fifth concentric ring electrode and the ninth concentric ring electrode are commonly used for forming an ion trap.
In an alternative embodiment, the insulating material disc is made of an insulating and non-gassing material;
and/or the metal in the metal film comprises at least one of molybdenum manganese and nickel;
and/or the leads are made of a low resistance material.
In an alternative embodiment, the material for preparing the insulating material disc comprises ceramic, glass or quartz; more preferably, the ceramic comprises alumina or zirconia.
In an alternative embodiment, the electrostatic ion trap is used in an ultra-high vacuum environment.
In an alternative embodiment, the ultra-high vacuum corresponds to a vacuum level of less than 10 -8 Pa。
In a second aspect, the present application provides a method for fabricating an electrostatic ion trap according to any one of the preceding embodiments, comprising the steps of: and manufacturing the electrostatic ion trap according to a preset structure.
In an alternative embodiment, the first electrostatic ion trap layer and the second electrostatic ion trap layer are prepared as follows: manufacturing an insulating material disc blank with a concentric groove and a concentric annular protrusion, processing the insulating material disc blank to form a required electrode shape, and arranging a lead wire and a metal film according to a preset position; and assembling the first electrostatic ion trap layer and the second electrostatic ion trap layer on static electricity.
In an alternative embodiment, the insulating material disc is formed by die-opening firing;
and/or concentric annular protrusions on the insulating material disc are formed by grooving or bonding;
and/or the processing of the insulating material disc blank is performed in a finish machining mode.
In an alternative embodiment, the grooving is performed by a grinding machine or engraving machine.
In an alternative embodiment, the finishing accuracy is not less than 0.01mm.
In an alternative embodiment, providing the leads includes the following: punching buried wires, penetrating screws, lateral groove opening pressing wires or punching welding.
In alternative embodiments, the means of perforating includes perforating the concentric annular protrusions vertically therethrough or perforating the sides of the concentric annular protrusions therethrough.
In an alternative embodiment, the wire is provided by directly soldering the wire to a predetermined location, or by pressing a metal tab at a predetermined location and then extracting the wire from the tab.
In an alternative embodiment, the design of the lead includes any of the following:
mode one: punching the protruding surfaces of the concentric annular protrusions, and arranging leads in the punched holes;
mode two: grooves are formed in the side faces of the concentric annular protrusions, and lead wires are arranged in the grooves;
mode three: grooves are formed in the side faces of the concentric annular protrusions, metal layers are arranged on the walls of the grooves, and then leads are arranged in the grooves;
mode four: punching the protruding surfaces of the concentric annular protrusions, arranging a metal layer on the hole wall after punching, and then arranging a lead in the hole after punching.
In an alternative embodiment, the metal film is disposed in a manner including: firstly, manufacturing a mask in a region where a metal film is not required to be arranged, then preparing the metal film at least in the region where the metal film is required to be arranged, and finally removing the mask;
alternatively, a mode of integrally preparing a metal film first and then removing the metal film corresponding to a region where the metal film is not required is adopted.
In an alternative embodiment, the mask is formed of a peelable material; more preferably, the exfoliatable material is a cured glue.
In alternative embodiments, the metal film may be prepared by magnetron sputtering, vacuum evaporation, chemical vapor deposition, or thick film.
In an alternative embodiment, the removing the mask includes: the mask formed of the exfoliatable material is torn off.
In alternative embodiments, the removal of the excess metal film is performed by grinding, milling or lathing.
In a third aspect, the present application provides a mass spectrometer comprising an electrostatic ion trap according to any of the preceding embodiments.
In an alternative embodiment, when ions entering the ion entry channel need to enter the ion trap, the gate electrode voltage is lower than the kinetic energy of the ions; after the ions enter the ion trap, the voltage of the gate electrode rises above the kinetic energy of the ions.
The beneficial effects of this application include:
the electrostatic ion trap with the specific structure is suitable for the environments of ultrahigh vacuum, high voltage and the like, and is high in thermal stability, high in resolution and high in accuracy of detection results. The manufacturing method is simple, has higher precision, can reduce processing residues and improves the stability of products. The mass spectrometer with the electrostatic ion trap has a good application prospect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic view of a part of the structure of an electrostatic ion trap according to an embodiment of the present application;
FIG. 2 is a graph showing the trend of potential field formed by partial electrode voltage after ions enter the ion trap in the embodiment of the present application;
FIG. 3 is a schematic diagram of a punching position in an embodiment of the present application;
FIG. 4 is a schematic diagram of a mask setting position in an embodiment of the present application;
fig. 5 is a schematic diagram of a groove arrangement position in an embodiment of the present application.
Icon: 10-an insulating material disc; 20-concentric grooves; 30-concentric annular projections; 40-metal film; 51-a first electrode set; 511-a first concentric ring electrode; 512-a second concentric ring electrode; 513-a third concentric ring electrode; 52-gate electrode; 53-a second electrode set; 531-a fifth concentric ring electrode; 532-sixth concentric ring electrode; 533-seventh concentric ring electrode; 534-eighth concentric ring electrode; 535-ninth concentric ring electrode; 60-holes; 70-grooves; 80-mask.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The electrostatic ion trap, the method for manufacturing the same and the mass spectrometer are specifically described below.
An electrostatic ion trap is presented that includes first and second electrostatic ion trap layers that are symmetrically assembled.
The first electrostatic ion trap layer and the second electrostatic ion trap layer may be vertically symmetrical or laterally symmetrical.
The first electrostatic ion trap layer and the second electrostatic ion trap layer comprise insulating material discs, a plurality of electrodes and leads.
The insulating material disc is provided with a plurality of concentric grooves, concentric annular protrusions are formed between two adjacent concentric grooves, the surface of each concentric annular protrusion is provided with a metal film to form a single electrode, and the lead wire is arranged on the surface or inside the insulating material disc and used for applying voltage to the electrode.
For reference, the plurality of electrodes include a first electrode group for forming an ion entrance channel, a gate electrode for controlling the ion entrance state into the ion trap, and a second electrode group for forming the ion trap, which are disposed from outside to inside in a radial direction of the insulating material disk.
Wherein the first electrode group comprises at least 3 concentric ring electrodes; the gate electrode is a concentric ring electrode; the second electrode set includes at least 4 concentric ring electrodes.
Illustratively, the first electrode set may include 3, 4, or more concentric ring electrodes; the second electrode set may include 4, 5 or more concentric ring electrodes.
In some embodiments, the first electrode set includes a first concentric ring electrode, a second concentric ring electrode, and a third concentric ring electrode disposed from outside to inside in a radial direction of the insulating disk. The first concentric ring electrode and the second concentric ring electrode and the third concentric ring electrode form an ion inlet channel together.
The gate electrode is a fourth concentric ring electrode.
The second electrode group comprises a fifth concentric ring electrode, a sixth concentric ring electrode, a seventh concentric ring electrode, an eighth concentric ring electrode and a ninth concentric ring electrode which are arranged from outside to inside along the radial direction of the insulating material disc. The regions between the fifth concentric ring electrode to the ninth concentric ring electrode are commonly used to form an ion trap.
The shape and size of each concentric ring electrode, the distance between two adjacent concentric ring electrodes, and the like may be set according to actual needs, and are not limited thereto.
In the use process, when ions entering the ion inlet channel need to enter the ion trap, the voltage of the gate electrode is lower than the kinetic energy of the ions; after the ions enter the ion trap, the voltage of the gate electrode rises above the kinetic energy of the ions.
For reference, the insulating material disc in the present application may be made of an insulating and non-outgassing material. Exemplary insulating and non-outgassing materials include ceramics (such as alumina or zirconia, etc.), glass, or quartz.
The metal in the metal film may include at least one of molybdenum manganese and nickel.
The number of layers of the metal film may be 1, or may be plural, such as 2, 3, 4, or more.
The leads are made of a low resistance material such as copper, silver, or aluminum.
The electrostatic ion trap in the application can be used for ultrahigh vacuum (vacuum degree is less than 10) -8 Pa) environment.
Correspondingly, the application also provides a manufacturing method of the electrostatic ion trap, which comprises the following steps: and manufacturing the electrostatic ion trap according to a preset structure.
Specifically, the first electrostatic ion trap layer and the second electrostatic ion trap layer were first prepared in the following manner: manufacturing an insulating material disc blank with a concentric groove and a concentric annular protrusion, processing the insulating material disc blank to form a required electrode shape, and arranging a lead wire and a metal film according to a preset position; and then assembling the prepared first electrostatic ion trap layer and the second electrostatic ion trap layer.
For reference, the insulating material disk may be manufactured by mold-opening firing.
The concentric annular protrusions on the insulating material disc may be formed by grooving or bonding. The grooving can be processed by a grinding machine or an engraving machine.
It should be noted that the above-mentioned slot is understood to be a groove formed by machining down from the surface of the insulating disc, and the connection portion between the grooves is a protrusion. Bonding is understood to mean bonding corresponding structures upwardly from the surface of the insulating material disc to form protrusions.
In the application, the machining of the disc blank made of the insulating material is performed in a finish machining mode, and the machining precision of the finish machining is not less than 0.01mm.
For reference, disposing the leads may include, by way of example and not limitation, the following: punching buried wires, penetrating screws, lateral groove opening pressing wires or punching welding.
The punching may include, for example, punching through the concentric annular protrusions vertically or punching through the concentric annular protrusions at the sides thereof. The open-sided slots may be either inboard slots or outboard slots.
In some alternative embodiments, the placement leads may be formed by soldering the wires directly to predetermined locations, and the surface protrusions may be manually scraped off; or the metal soldering lug is pressed at the preset position, then the lead is led out from the soldering lug, and finally the protruding part is scraped manually.
In some preferred embodiments, the design of the leads includes any of the following:
mode one: punching the protruding surfaces of the concentric annular protrusions, and arranging leads in the punched holes;
mode two: grooves are formed in the side faces of the concentric annular protrusions, and lead wires are arranged in the grooves;
mode three: grooves are formed in the side faces of the concentric annular protrusions, metal layers are arranged on the walls of the grooves, and then leads are arranged in the grooves;
mode four: punching the protruding surfaces of the concentric annular protrusions, arranging a metal layer on the hole wall after punching, and then arranging a lead in the hole after punching.
The fourth mode can increase the metal contact area and reduce the contact failure compared with the first mode. The second mode and the third mode are more suitable for the situation that part of the electrodes are longer and punching is difficult.
For reference, the metal film may be disposed in the following manner: firstly, manufacturing a mask in a region where a metal film is not required to be arranged, then preparing the metal film at least in the region where the metal film is required to be arranged, and finally removing the mask (marked as a mode (1));
alternatively, a method (referred to as method (2)) in which a metal film is integrally formed first and then a metal film corresponding to a region where the metal film is not required to be provided is removed (referred to as an excess metal film for short).
The mask is preferably formed of a peelable material, such as a cured glue.
The preparation method of the metal film can include, by way of example and not limitation, magnetron sputtering, vacuum evaporation, chemical vapor deposition or thick film method.
The mask removing method may include: the mask formed of the peelable material is peeled off (corresponding to the above-described mode (1)).
The removal of the excessive metal film may be performed by grinding, milling or lathing (corresponding to the above-mentioned mode (2)).
In some embodiments, if the ceramic is selected from alumina or zirconia materials, it is preferred to remove excess metal film using a grinder or diamond-plated tool; if the ceramic is a machinable ceramic (e.g., a macor or shape aluminum nitride material), the excess metal film may be removed directly by machining with a lathe or numerically controlled machine tool.
On the other hand, the manufacturing process eliminates the method of independently manufacturing the ceramic and the metal piece, assembling the ceramic and the metal piece by a welding or bonding method and finally finishing the ceramic and the metal piece in the prior art. According to the method, the electrode shape required by the ceramic finish machining is achieved through firing, the surface of the insulating part is metallized through a film plating process, then redundant metal parts are removed, and finally the ion trap structure which is simpler in process, less in processing residues, better in stability and suitable for the ultra-high vacuum, high-voltage and other environments is manufactured through a face-to-face assembly molding scheme. Before plating a metal film, a layer of mask is brushed at a non-metal position, the mask can be solidified in a few seconds under visible light, pollution and peeling can be avoided, metallization is carried out after the mask is solidified, and finally the solidified mask is removed.
More specifically, the manufacturing method provided by the application can ensure mechanical precision at first, and the electrode is assembled after finishing, so that a method of fixing the electrode by using a fastener and finishing the electrode again by using an insulating support is not needed, and pollution caused by finishing after finishing the assembly is reduced; secondly, the manufacturing method provided by the application avoids the problem that ultra-high vacuum cannot be achieved due to the use of vacuum glue; finally, compared with the welding joint scheme of ceramics and metals (the scheme is difficult to ensure that the thermal expansion coefficients of the two materials are kept consistent when the temperature is changed, and the reasons include that the problems of desoldering, deformation, fragmentation and the like can occur when the cavity is baked for achieving the ultrahigh vacuum requirement, the manufacturing method provided by the application simplifies the process, and one or more layers of metal films with better thermal stability can be obtained, and the phenomenon of desoldering and the like can not occur even when the cavity is baked.
In addition, the application also provides a mass spectrometer, which comprises the electrostatic ion trap.
It should be noted that, the description of the location of the electrostatic ion trap in the mass spectrometer and other structures included in the mass spectrometer may refer to the related art, and will not be repeated herein.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment provides an electrostatic ion trap for an ultra-high vacuum environment, referring to fig. 1, which includes a first electrostatic ion trap layer and a second electrostatic ion trap layer that are assembled symmetrically up and down.
The first electrostatic ion trap layer and the second electrostatic ion trap layer each comprise an insulating material disk 10, a plurality of electrodes and leads (not shown). The insulating material disc 10 has a plurality of concentric grooves 20, concentric annular protrusions 30 are formed between two adjacent concentric grooves 20, a metal film 40 is provided on the surface of each concentric annular protrusion 30 to form a single electrode, and a lead wire is provided on the surface or inside of the insulating material disc 10 for applying a voltage to the electrode.
The plurality of electrodes include a first electrode group 51 for forming an ion entrance path, a gate electrode 52 for controlling the ion entrance state into the ion trap, and a second electrode group 53 for forming the ion trap, which are disposed from outside to inside in the radial direction of the insulating material disk 10.
Wherein, the first electrode group 51 comprises a first concentric ring electrode 511, a second concentric ring electrode 512 and a third concentric ring electrode 513 which are arranged from outside to inside along the radial direction of the insulating material disc 10; together, the first concentric ring electrode 511 and the second concentric ring electrode 512 and the third concentric ring electrode 513 form a channel for ion entry.
The gate electrode 52 is a fourth concentric ring electrode.
The second electrode group 53 includes fifth, sixth, seventh, eighth, and ninth concentric ring electrodes 531, 532, 533, 534, 535, which are disposed from outside to inside in the radial direction of the insulating disk 10, and the regions between the fifth to ninth concentric ring electrodes 531 to 535 are commonly used to form an ion trap.
The insulating disc 10 is made of alumina. The metal in the metal film 40 is molybdenum manganese. The leads were made of copper.
The whole device operates in the following manner, ions are restrained to fly in an electric field formed by the first concentric ring electrode 511, the second concentric ring electrode 512 and the third concentric ring electrode 513, when the first concentric ring electrode 511 suddenly applies a pulse, the ions are subjected to radial force to be injected into the ion trap, and at the moment, the potential energy barrier is smaller than the ion kinetic energy due to the voltage reduction of the fourth concentric ring electrode, so that the ions pass smoothly. After the ions enter the ion trap, the potential well barrier is made larger than the ion kinetic energy by the voltage rise of the fourth concentric ring electrode, so that the ions are trapped in the ion trap, and thus the ions can do precession elliptical oscillation near the central plane between the electrodes at the two sides, and the potential field formed by the voltage applied to each electrode from the ninth concentric ring electrode 535 to the fourth concentric ring electrode (gate electrode 52) is shown in fig. 2. The voltage of each electrode needs to be adjusted to ensure the axial isochronism and the space focusing property when the ions stably oscillate, and the electric field in the ion trap meets the requirements through the voltage adjustment of a plurality of electrodes. In the process of stable oscillation of ions, a corresponding image charge signal can be induced on the charge detection electrode in the middle, and the signal is amplified by the low-noise amplifier and converted into a final mass spectrogram through formulas such as Fourier transformation, frequency-mass conversion and the like.
Example 2
The embodiment provides a method for manufacturing an electrostatic ion trap of embodiment 1, which includes the following steps:
first, preparing a first electrostatic ion trap layer and a second electrostatic ion trap layer in the following manner: manufacturing a blank of an insulating material disc 10 with concentric grooves 20 and concentric annular protrusions, processing the blank of the insulating material disc 10 to form a required electrode shape, and arranging leads and a metal film 40 according to preset positions; and then assembling the prepared first electrostatic ion trap layer and the second electrostatic ion trap layer.
The insulating disc 10 is formed by mold-opening firing.
The concentric annular protrusions 30 on the insulating disc 10 are formed by grooving. The grooving is specifically processed by a grinding machine (or engraving machine).
The processing of the blank of the insulating material disc 10 is carried out by adopting a finish machining mode, and the machining precision of the finish machining is not less than 0.01mm.
The design mode of the lead wire is as follows: referring to fig. 3, the protruding surfaces of the concentric annular protrusions 30 are perforated, and a lead is provided in the perforated hole 60. The surface protrusions were manually scraped.
The metal film 40 is provided in the following manner: referring to fig. 4, a mask 80 (formed by curing a cured adhesive) is first formed on a region where the metal film 40 is not required, then the metal film 40 is formed on the region where the metal film 40 is required by magnetron sputtering, and finally the mask 80 is removed.
Example 3
This embodiment differs from embodiment 2 in that: the concentric annular protrusions 30 on the insulating disc 10 are formed by bonding.
Example 4
This embodiment differs from embodiment 2 in that:
the design mode of the lead wire is as follows: referring to fig. 5, grooves 70 are provided on the side surfaces of the concentric annular protrusions 30, and leads are provided in the grooves 70.
Example 5
This embodiment differs from embodiment 2 in that:
the design mode of the lead wire is as follows: grooves 70 are provided on the side surfaces of the respective concentric annular protrusions 30, a metal layer is provided on the walls of the grooves 70, and then a lead is provided in the grooves 70.
Example 6
This embodiment differs from embodiment 2 in that:
the design mode of the lead wire is as follows: the protruding surfaces of the concentric annular protrusions 30 are perforated, metal layers are provided on the perforated hole walls, and then leads are provided in the perforated holes 60.
Example 7
This embodiment differs from embodiment 2 in that:
the metal film 40 is provided in the following manner: the metal film 40 is integrally prepared, and then the excessive metal film 40 is removed by a grinding machine.
Example 8
This embodiment differs from embodiment 2 in that: the metal film 40 is prepared by vacuum evaporation.
Example 9
This embodiment differs from embodiment 2 in that: the metal film 40 is prepared by chemical vapor deposition.
Example 10
This embodiment differs from embodiment 2 in that:
the insulating material disk 10 is made of zirconia.
Excess metal film 40 is removed using a diamond-plated tool.
Example 11
This embodiment differs from embodiment 2 in that:
the insulating material disk 10 is made of shape aluminum nitride.
The excess metal film 40 is removed by machining using a lathe (or a numerical control machine).
In conclusion, the electrostatic ion trap provided by the application is suitable for the environments of ultrahigh vacuum, high voltage and the like, and is high in thermal stability, high in resolution and high in accuracy of detection results. The manufacturing method is simple, has higher precision, can reduce processing residues and improves the stability of products. The mass spectrometer with the electrostatic ion trap has a good application prospect.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An electrostatic ion trap, comprising a first electrostatic ion trap layer and a second electrostatic ion trap layer which are symmetrically assembled;
the first electrostatic ion trap layer and the second electrostatic ion trap layer comprise insulating material discs, a plurality of electrodes and leads;
the insulating material disc is provided with a plurality of concentric grooves, concentric annular protrusions are formed between two adjacent concentric grooves, a metal film is arranged on the surface of each concentric annular protrusion to form a single electrode, and the lead is arranged on the surface or inside the insulating material disc and used for applying voltage to the electrodes.
2. An electrostatic ion trap according to claim 1, wherein the plurality of electrodes comprises a first electrode group for forming an ion entrance channel, a gate electrode for controlling the ion entrance into the ion trap state, and a second electrode group for forming the ion trap, which are arranged from outside to inside in a radial direction of the insulating material disk;
preferably, the first electrode group comprises at least 3 concentric ring electrodes; and/or the gate electrode is a concentric ring electrode; and/or the second electrode group comprises at least 4 concentric ring electrodes;
preferably, the first electrode group comprises a first concentric ring electrode, a second concentric ring electrode and a third concentric ring electrode which are arranged from outside to inside along the radial direction of the insulating material disc; the first concentric ring electrode and the second concentric ring electrode and the third concentric ring electrode together form an ion inlet channel;
the gate electrode is a fourth concentric ring electrode;
the second electrode group comprises a fifth concentric ring electrode, a sixth concentric ring electrode, a seventh concentric ring electrode, an eighth concentric ring electrode and a ninth concentric ring electrode which are arranged from outside to inside along the radial direction of the insulating material disc, and the areas between the fifth concentric ring electrode and the ninth concentric ring electrode are commonly used for forming the ion trap.
3. An electrostatic ion trap according to claim 1, wherein the insulating material discs are made of an insulating and non-gassing material;
and/or the metal in the metal film comprises at least one of molybdenum manganese and nickel;
and/or, the lead is made of a low-resistance material;
preferably, the material for preparing the insulating material disc comprises ceramic, glass or quartz; more preferably, the ceramic comprises alumina or zirconia.
4. An electrostatic ion trap according to any one of claims 1 to 3, wherein the electrostatic ion trap is used in an ultra-high vacuum environment;
preferably, the vacuum degree corresponding to the ultra-high vacuumLess than 10 -8 Pa。
5. A method of fabricating an electrostatic ion trap according to any one of claims 1 to 4, comprising the steps of: manufacturing the electrostatic ion trap according to a preset structure;
preferably, the first electrostatic ion trap layer and the second electrostatic ion trap layer are prepared in the following manner: manufacturing an insulating material disc blank with the concentric grooves and the concentric annular protrusions, processing the insulating material disc blank to form a required electrode shape, and arranging a lead wire and a metal film according to preset positions; assembling the first electrostatic ion trap layer and the second electrostatic ion trap layer.
6. The method according to claim 5, wherein the insulating disc is formed by mold-opening firing;
and/or concentric annular protrusions on the insulating material disc are formed by grooving or bonding;
and/or the processing of the insulating material disc blank is performed in a finish machining mode;
preferably, the grooving is processed by a grinding machine or an engraving machine;
preferably, the finishing accuracy of the finishing is not less than 0.01mm.
7. The method of manufacturing of claim 5, wherein providing the leads comprises: punching buried lines, penetrating screws, side slot line pressing or punching welding;
preferably, the punching means comprises punching through the concentric annular protrusions vertically or punching through the concentric annular protrusions at the sides thereof;
preferably, the lead is arranged by directly welding the lead at a preset position, or by firstly pressing a metal soldering lug at the preset position and then leading out the lead from the soldering lug;
more preferably, the design mode of the lead wire comprises any one of the following modes:
mode one: punching the protruding surfaces of the concentric annular protrusions, and arranging leads in the punched holes;
mode two: grooves are formed in the side faces of the concentric annular protrusions, and lead wires are arranged in the grooves;
mode three: grooves are formed in the side faces of the concentric annular protrusions, metal layers are arranged on the groove walls of the grooves, and then leads are arranged in the grooves;
mode four: punching the protruding surfaces of the concentric annular protrusions, arranging a metal layer on the hole wall after punching, and then arranging a lead in the hole after punching.
8. The method according to claim 5, wherein the metal film is provided in a manner comprising: firstly, manufacturing a mask in a region where a metal film is not required to be arranged, then preparing the metal film at least in the region where the metal film is required to be arranged, and finally removing the mask;
or, a mode of integrally preparing the metal film firstly and then removing the metal film corresponding to the area without the metal film is adopted;
preferably, the mask is formed of a peelable material; more preferably, the exfoliatable material is a cured gel;
preferably, the preparation method of the metal film comprises magnetron sputtering, vacuum evaporation, chemical vapor deposition or thick film method;
preferably, the mask removing method includes: tearing off a mask formed of a peelable material;
preferably, the removal of the excess metal film is performed by grinding, milling or lathing.
9. A mass spectrometer comprising an electrostatic ion trap as claimed in any one of claims 1 to 4.
10. The mass spectrometer of claim 9, wherein when ions entering the ion entrance channel are required to enter the ion trap, the voltage of the gate electrode is lower than the kinetic energy of the ions; after ions enter the ion trap, the voltage of the gate electrode rises above the kinetic energy of the ions.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2023100249140 | 2023-01-09 | ||
| CN202310024914.0A CN115985753A (en) | 2023-01-09 | 2023-01-09 | Electrostatic ion trap, manufacturing method thereof and mass spectrometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117373896A true CN117373896A (en) | 2024-01-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310024914.0A Withdrawn CN115985753A (en) | 2023-01-09 | 2023-01-09 | Electrostatic ion trap, manufacturing method thereof and mass spectrometer |
| CN202311239037.5A Pending CN117373896A (en) | 2023-01-09 | 2023-09-22 | Electrostatic ion trap, manufacturing method thereof and mass spectrometer |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310024914.0A Withdrawn CN115985753A (en) | 2023-01-09 | 2023-01-09 | Electrostatic ion trap, manufacturing method thereof and mass spectrometer |
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| Country | Link |
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| CN (2) | CN115985753A (en) |
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2023
- 2023-01-09 CN CN202310024914.0A patent/CN115985753A/en not_active Withdrawn
- 2023-09-22 CN CN202311239037.5A patent/CN117373896A/en active Pending
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| CN115985753A (en) | 2023-04-18 |
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