CN117451910A - Helium ion detector and preparation method thereof - Google Patents
Helium ion detector and preparation method thereof Download PDFInfo
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- CN117451910A CN117451910A CN202311526934.4A CN202311526934A CN117451910A CN 117451910 A CN117451910 A CN 117451910A CN 202311526934 A CN202311526934 A CN 202311526934A CN 117451910 A CN117451910 A CN 117451910A
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- 229910052734 helium Inorganic materials 0.000 title claims abstract description 68
- 239000001307 helium Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000758 substrate Substances 0.000 claims description 90
- 230000005284 excitation Effects 0.000 claims description 37
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 26
- 239000010703 silicon Substances 0.000 claims description 26
- 239000011521 glass Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 10
- 238000000059 patterning Methods 0.000 claims description 9
- 230000000149 penetrating effect Effects 0.000 claims description 6
- 238000001514 detection method Methods 0.000 abstract description 17
- 230000005684 electric field Effects 0.000 abstract description 15
- 238000009826 distribution Methods 0.000 abstract description 11
- 230000035945 sensitivity Effects 0.000 abstract description 11
- -1 Helium ion Chemical class 0.000 description 51
- 239000007789 gas Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 229910052814 silicon oxide Inorganic materials 0.000 description 9
- 239000012159 carrier gas Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000000306 component Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229920002120 photoresistant polymer Polymers 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- 230000004308 accommodation Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000000708 deep reactive-ion etching Methods 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- 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
- G01N27/64—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 wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
- G01N27/66—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 wave or particle radiation to ionise a gas, e.g. in an ionisation chamber and measuring current or voltage
Abstract
The invention provides a helium ion detector and a preparation method thereof, wherein the collection electrode is arranged in a closed cavity to obtain ideal electric field distribution, and the offset electrode is arranged in the closed cavity in a combined way to effectively improve the ion collection efficiency, so that the helium ion detector has lower detection limit and higher detection sensitivity on the premise of smaller volume. In addition, the helium ion detector adopts a sandwich structure, and is suitable for being combined with a chromatographic column or being monolithically integrated with a micro-chromatographic column.
Description
Technical Field
The invention belongs to the field of micro-electromechanical systems, and relates to a helium ion detector and a preparation method thereof.
Background
The gas chromatographic system is one technological means of separating and detecting complex mixed gas components and has chromatographic column and detector as the core components. Currently, the detectors commonly used in gas chromatography systems are flame ionization detectors, which are simple in structure and have a high response to almost all volatile and semi-volatile organic compounds, but which are unable to detect water and permanent gases, and thermal conductivity detectors; the thermal conductivity detector is responsive to all gases except the carrier gas, but is less sensitive to flow and temperature changes.
The helium ion detector is a universal gas detector, and can detect all gases except neon due to high ionization energy (19.8 eV), has a detection limit of ppb level, and can be well combined with a chromatographic column to detect trace gases.
In 1960, berry first proposed a gas detection technique using helium as a carrier gas, and ionized analytes by a gas discharge phenomenon, and after further research on this detection technique, researchers have found that the detection capability of a helium ion detector is related to the stability of plasma and the number, structure and position of excitation electrodes and collection electrodes. The increased chamber volume allows for higher sensitivity and greater linear detection range, while the placement of multiple pairs of bias/collection electrodes within the chamber increases sensitivity, improves peak symmetry, and allows for lower helium flow rates without affecting peak tailing.
In recent years, with the development of MEMS technology, a micro helium ion detector has been proposed, but due to the reduction of the device volume, the chamber volume is reduced, and the smaller chamber volume affects the sensitivity and the detection limit of the micro helium ion detector. To solve the above-mentioned problems, it is necessary to design and prepare a bias/collection electrode group structure having high collection efficiency for improving the sensitivity of the micro helium ion detector.
Therefore, it is desirable to provide a helium ion detector and a method of manufacturing the same.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a helium ion detector and a manufacturing method thereof, which are used for solving the detection problem caused by miniaturization of the helium ion detector in the prior art.
To achieve the above and other related objects, the present invention provides a method for manufacturing a helium ion detector, comprising the steps of:
providing a substrate;
providing an upper cover plate and a lower cover plate, forming a first collecting electrode on the upper cover plate, forming a second collecting electrode on the lower cover plate, and forming a first bias electrode and a second bias electrode which are positioned on two sides of the second collecting electrode;
bonding the lower cover plate with the lower surface of the substrate;
patterning the substrate, forming a through groove penetrating through the substrate, an input/output through groove communicated with the through groove and an excitation electrode through groove in the substrate, wherein the through groove exposes the second collecting electrode, the first bias electrode and the second bias electrode;
and bonding the upper cover plate with the upper surface of the substrate, covering the through groove by the upper cover plate to form a closed cavity, covering the input/output through groove to form a closed input/output channel and covering the excitation electrode through groove to form an excitation electrode channel, wherein the first collecting electrode is exposed in the closed cavity and is correspondingly arranged with the second collecting electrode to form a opposite collecting electrode.
Optionally, the step of patterning the substrate is completed before the bonding step.
Optionally, the upper cover plate is bonded to the upper surface of the substrate, and then the lower cover plate is bonded to the lower surface of the substrate.
Optionally, an electrode accommodating groove for accommodating the first collecting electrode is formed on the upper surface of the substrate, and electrode accommodating grooves for accommodating the second collecting electrode, the first bias electrode and the second bias electrode are formed on the lower surface of the substrate.
Optionally, the step of forming an electrode protection layer covering the electrode is further included before patterning the substrate to form the through groove, and the step of removing the electrode protection layer is further included after patterning the substrate to form the through groove.
Optionally, the method further includes a step of dicing, and during dicing, forward and reverse dicing is performed from the upper cover plate and the lower cover plate respectively, so as to expose the electrical connection ends of the first collecting electrode, the second collecting electrode, the first bias electrode and the second bias electrode.
Optionally, the first bias electrode and the second bias electrode are symmetrically arranged along the second collecting electrode, the distances between the first bias electrode and the second bias electrode and between the second collecting electrode and between the first bias electrode and the second collecting electrode are 300 μm-1000 μm, the distances between the adjacent bias electrode and the exciting electrode are 500 μm-2000 μm, and the distances between the first collecting electrode and the second collecting electrode are 200 μm-700 μm.
Optionally, the substrate comprises a silicon substrate, a ceramic substrate, or a glass substrate; the upper cover plate comprises a silicon cover plate, a ceramic cover plate or a glass cover plate; the lower cover plate comprises a silicon cover plate, a ceramic cover plate or a glass cover plate.
The present invention also provides a helium ion detector comprising:
the upper cover plate is provided with a first collecting electrode;
the lower cover plate is provided with a second collecting electrode, a first bias electrode and a second bias electrode which are positioned at two sides of the second collecting electrode;
the patterned substrate, be provided with in the substrate run through the base plate the slot that link up, with the input and output that link up the slot that link up is led to the slot and excitation electrode leads to the slot, just the upper surface of base plate with the upper cover plate bonding, the lower surface of base plate with the lower cover plate bonding, through upper cover plate with the lower cover plate covers the slot constitutes closed cavity, covers the input and output leads to the slot and constitutes closed input and output passageway and covers excitation electrode leads to the slot constitutes excitation electrode passageway, just first collecting electrode, second collecting electrode first biasing electrode and second biasing electrode expose in closed cavity, first collecting electrode with the second collecting electrode corresponds the setting and constitutes to receiving the collecting electrode.
Optionally, the first bias electrode and the second bias electrode are symmetrically arranged along the second collecting electrode, the distances between the first bias electrode and the second bias electrode and between the second collecting electrode and between the first bias electrode and the second collecting electrode are 300 μm-1000 μm, the distances between adjacent bias electrodes and the excitation electrode are 500 μm-2000 μm, and the distances between the first collecting electrode and the second collecting electrode are 200 μm-700 μm.
As described above, the helium ion detector and the preparation method thereof can obtain ideal electric field distribution by arranging the pair of collecting electrodes in the closed chamber, and can effectively improve the ion collecting efficiency by combining the pair of offset electrodes in the closed chamber, so that the helium ion detector can have lower detection limit and higher detection sensitivity on the premise of smaller volume. In addition, the helium ion detector adopts a sandwich structure, and is suitable for being combined with a chromatographic column or being monolithically integrated with a micro-chromatographic column.
Drawings
FIG. 1 shows a flow chart of a process for manufacturing a helium ion detector according to the present invention.
FIGS. 2 a-2 h are schematic diagrams illustrating the structure of helium ion detectors according to the present invention.
Fig. 3 is a schematic diagram showing a three-dimensional structure of a helium ion detector according to the present invention.
Fig. 4a shows the flow field distribution diagram in a helium ion detector according to the present invention.
FIG. 4b shows the flow rate at the glow excitation of a helium ion detector according to the present invention as a function of the x-coordinate.
Fig. 5a shows a simulated distribution of electric field lines for a helium ion detector of the present invention employing a collection electrode.
Fig. 5b shows a simulated distribution of electric field lines for a helium ion detector of the present invention employing a planar collection electrode.
Fig. 5c shows the intensity of the electric field at the collecting electrode pad as a function of Y-coordinate for a helium ion detector according to the present invention.
Fig. 5d shows the electric field strength at the plate of a flat collecting electrode used in the helium ion detector according to the present invention as a function of Y-coordinate.
FIG. 6 shows a graph of chromatographic effluent for a helium ion detector of the present invention in combination with a chromatographic column versus a C2-C4 test.
Description of element reference numerals
100. Silicon substrate
101. Top silicon oxide layer
102. Bottom silicon oxide layer
103. First collecting electrode accommodating groove
104. Second collecting electrode accommodation groove
105. First bias electrode accommodation groove
106. Second bias electrode accommodation groove
107. Through groove
200. Upper glass cover plate
201. First collecting electrode
300. Lower glass cover plate
301. A second collecting electrode
302. First bias electrode
303. Second bias electrode
400. Electrode protection layer
500. Closed chamber
600. Sample input channel
700. Carrier gas inlet channel
800. Gas output channel
900. Excitation electrode channel
110. Excitation electrode
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
As described in detail in the embodiments of the present invention, the cross-sectional view of the device structure is not partially enlarged to a general scale for convenience of explanation, and the schematic drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in actual fabrication.
For ease of description, spatially relative terms such as "under", "below", "beneath", "above", "upper" and the like may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that these spatially relative terms are intended to encompass other orientations of the device in use or operation in addition to the orientation depicted in the figures, including embodiments in which the first and second features are formed in direct contact, as well as embodiments in which additional features are formed between the first and second features, such that the first and second features may not be in direct contact, and further, when a layer is referred to as being "between" two layers, it may be the only layer between the two layers, or there may be one or more intervening layers.
It should be noted that, the illustrations provided in the present embodiment merely illustrate the basic concept of the present invention by way of illustration, and only the components related to the present invention are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of each component in actual implementation may be changed at will, and the layout of the components may be more complex.
As shown in fig. 1, the present embodiment provides a method for manufacturing a helium ion detector, which includes the following steps:
s1: providing a substrate;
s2: providing an upper cover plate and a lower cover plate, forming a first collecting electrode on the upper cover plate, forming a second collecting electrode on the lower cover plate, and forming a first bias electrode and a second bias electrode which are positioned on two sides of the second collecting electrode;
s3: bonding the lower cover plate with the lower surface of the substrate;
s4: patterning the substrate, forming a through groove penetrating through the substrate, an input/output through groove communicated with the through groove and an excitation electrode through groove in the substrate, wherein the through groove exposes the second collecting electrode, the first bias electrode and the second bias electrode;
s5: and bonding the upper cover plate with the upper surface of the substrate, covering the through groove by the upper cover plate to form a closed cavity, covering the input/output through groove to form a closed input/output channel and covering the excitation electrode through groove to form an excitation electrode channel, wherein the first collecting electrode is exposed in the closed cavity and is correspondingly arranged with the second collecting electrode to form a opposite collecting electrode.
The preparation of the helium ion detector is further described below with reference to fig. 2 a-2 h and 3.
First, referring to fig. 1, step S1 is performed to provide a substrate.
Specifically, referring to fig. 2a, the substrate may include, for example, a silicon substrate, a ceramic substrate, or a glass substrate, and in this embodiment, the substrate is a silicon substrate 100 that is easier to perform a MEMS process, so that the helium ion detector and the chromatographic column can be conveniently and quickly manufactured to be integrated, manufactured, or combined, and matched for application, but the type of the substrate is not limited thereto.
As an example, the upper surface of the substrate may be formed with an electrode receiving groove to receive the first collecting electrode, and the lower surface of the substrate is formed with electrode receiving grooves to receive the second collecting electrode, the first bias electrode, and the second bias electrode, respectively, so as to ensure airtight bonding of the substrate and the cover plate in the bonding process.
Specifically, referring to fig. 2a to 2c, in the present embodiment, a first collecting electrode accommodating groove 103 for accommodating the first collecting electrode is formed in the silicon substrate 100, and a second collecting electrode accommodating groove 104 for accommodating the second collecting electrode, a first biasing electrode accommodating groove 105 for accommodating the first biasing electrode, and a second biasing electrode accommodating groove 106 for accommodating the second biasing electrode are formed in the lower surface of the silicon substrate 100.
Wherein, in preparing the first collecting electrode accommodating groove 103, the second collecting electrode accommodating groove 104, the first bias electrode accommodating groove 105 and the second bias electrode accommodating groove 106, a top silicon oxide layer 101 located on the upper surface of the silicon substrate 100 and a bottom silicon oxide layer 102 located on the lower surface of the silicon substrate 100 may be formed on the surface of the silicon substrate 100 by, for example, a thermal oxidation process, as shown in fig. 2a; then, the top silicon oxide layer 101 and the bottom silicon oxide layer 102 may be patterned in a BOE solution with photoresist and the like as masks, and etched with, for example, KOH solution, to pattern the silicon substrate 100 to form a desired electrode accommodating groove, as shown in fig. 2b; excess photoresist and the top silicon oxide layer 101 and the bottom silicon oxide layer 102 are then removed, as shown in fig. 2c.
The method for preparing the electrode receiving groove is not limited thereto, and, for example, dry etching or the like may be employed, and is not excessively limited thereto.
In another embodiment, if the collecting electrode and the bias electrode are embedded in the cover plate, so that the air tightness problem is not caused when the cover plate and the substrate are bonded, the substrate may not be prepared with the electrode accommodating groove, but the corresponding electrode accommodating groove is prepared in the cover plate, and the electrode accommodating groove may be specifically selected according to the needs, and is not excessively limited herein.
Next, referring to fig. 1, step S2 is performed, in which an upper cover plate and a lower cover plate are provided, a first collecting electrode is formed on the upper cover plate, and a second collecting electrode, and a first bias electrode and a second bias electrode located at two sides of the second collecting electrode are formed on the lower cover plate.
As an example, the upper cover plate may include a silicon cover plate, a ceramic cover plate, or a glass cover plate; the lower cover plate may include a silicon cover plate, a ceramic cover plate, or a glass cover plate.
Specifically, referring to fig. 2d and 2g, in the present embodiment, the upper cover plate and the lower cover plate are both glass cover plates, but the materials of the upper cover plate and the lower cover plate are not limited thereto, and may be silicon cover plates, ceramic cover plates, or the like. In this embodiment, a patterned first collecting electrode 201 is formed on the upper glass cover 200, a second collecting electrode 301, a first bias electrode 302 and a second bias electrode 303 are formed on the lower glass cover 300, and the first bias electrode 302 and the second bias electrode 303 are symmetrically disposed along the second collecting electrode 301.
The first collecting electrode 201, the second collecting electrode 301, the first bias electrode 302 and the second bias electrode 303 may be manufactured by sputtering, etching and photoresist removing processes, but the material of the electrodes may be Cr/Au, etc., and is not limited thereto.
Next, referring to fig. 1, step S3 is performed to bond the lower cover plate to the lower surface of the substrate.
Specifically, referring to fig. 2e, in this embodiment, the silicon substrate 100 is used as the substrate, the lower glass cover 300 is used as the lower cover, and thus, the bonding method between the lower cover and the lower surface of the substrate may be an anodic bonding method, but the bonding method is not limited thereto, and may be specifically selected according to the materials of the lower cover and the substrate.
As an example, as shown in fig. 2d, before bonding the lower cover plate with the lower surface of the substrate, a step of forming an electrode protection layer 400 covering the electrode may be further included.
Specifically, since the substrate needs to be etched later to prepare the through groove 107 exposing the electrode, as shown in fig. 2f, before the lower cover plate is bonded to the lower surface of the substrate, the patterned electrode protection layer 400 covering the electrode may be formed first, so that the electrode protection layer 400 covers the electrode surface to protect the electrode, and damage to the electrode caused by the subsequent steps such as etching is avoided.
The electrode protection layer 400 may include a silicon oxide layer, etc., and the preparation method may include photolithography, PECVD deposition, photoresist removal, etc.
Next, referring to fig. 1, step S4 is performed to pattern the substrate, and a through groove penetrating the substrate, an input/output through groove communicating with the through groove, and an excitation electrode through groove are formed in the substrate, wherein the through groove exposes the second collecting electrode, the first bias electrode, and the second bias electrode.
Specifically, referring to fig. 2f, deep Reactive Ion Etching (DRIE) may be performed on the upper surface of the silicon substrate 100 using photoresist as a mask, to form a through groove 107 penetrating the silicon substrate 100, an input/output through groove (not shown) and an excitation electrode through groove (not shown) which are in communication with the through groove 107, and the through groove 107 exposes the second collecting electrode 301, the first bias electrode 302 and the second bias electrode 303. Due to the presence of the electrode protection layer 400, the electrode protection layer 400 on the electrode may be removed after etching using a BOE solution or the like.
Next, referring to fig. 1, step S5 is performed, wherein the upper cover plate is bonded to the upper surface of the substrate, the through groove is covered by the upper cover plate to form a closed chamber, the input/output through groove is covered to form a closed input/output channel, the excitation electrode through groove is covered to form an excitation electrode channel, and the first collecting electrode is exposed in the closed chamber and is arranged corresponding to the second collecting electrode to form a counter collecting electrode.
Specifically, referring to fig. 2h, in this embodiment, the silicon substrate 100 is used as the substrate, the upper glass cover 200 is used as the upper cover, and thus, the bonding method between the upper cover and the upper surface of the substrate may be an anodic bonding method, but the bonding method is not limited thereto, and may be specifically selected according to the materials of the upper cover and the substrate.
Referring to fig. 3, after the bonding process is completed, the through groove 107 forms a closed chamber 500, the input/output through groove forms a closed input/output channel, and the closed chamber includes a sample input channel 600, a carrier gas input channel 700, a gas output channel 800, and an excitation electrode channel 900 for accommodating the excitation electrode 110, and the first collecting electrode 201 is exposed in the closed chamber 500 and is disposed corresponding to the second collecting electrode 301 to form a counter collector.
In this embodiment, the ideal electric field distribution can be obtained by forming the pair of collecting electrodes in the closed chamber 500, and the ion collecting efficiency can be effectively improved by combining the first bias electrode 302 and the second bias electrode 303 in the closed chamber 500, so that the helium ion detector can have a lower detection limit and a higher detection sensitivity on the premise of a smaller volume; and the helium ion detector is suitable for being combined with a chromatographic column or monolithically integrated due to the adoption of a sandwich structure.
In another embodiment, the patterned substrate may be formed before the bonding step, that is, the through-slot 107, the input-output through-slot, and the excitation electrode through-slot may be formed in the substrate, and then the bonding process step may be performed to form the closed chamber 500, the sample input channel 600, the carrier gas input channel 700, the gas output channel 800, and the excitation electrode channel 900, which are not limited herein.
In another embodiment, the upper cover plate may be bonded to the upper surface of the substrate before the lower cover plate is bonded to the lower surface of the substrate, which is not limited herein.
As an example, the method may further include a step of dicing, and during dicing, forward and backward dicing is performed from the upper cover plate and the lower cover plate respectively to expose the electrical connection ends of the first collecting electrode, the second collecting electrode, the first bias electrode and the second bias electrode.
Specifically, a helium ion detector meeting the size requirement can be obtained through the process step of dicing after bonding is completed. The helium ion detector may be manufactured to have an overall size of 19.3mm×9.96mm×1.45mm, the closed chamber 500 may have a size of 8.2mm×5mm×0.45mm, and the input/output port may have a width of 400 μm, and the specific size of the helium ion detector may be selected as required.
Referring to fig. 3, in the embodiment, during dicing, forward and backward dicing is preferably performed from the upper glass cover 200 and the lower glass cover 300 respectively, so as to form a zigzag shape in fig. 3 by dicing, so as to expose the electrical connection ends of the first collecting electrode 201, the second collecting electrode 301, the first bias electrode 302 and the second bias electrode 303, so as to facilitate subsequent electrical connection.
Further, the method may further include the steps of installing a capillary (not shown) in the sample input channel 600, the carrier gas input channel 700, and the gas output channel 800, sealing, such as an epoxy pipe, and inserting the excitation electrode 110 into the excitation electrode channel 900 to connect the helium ion detector to a chromatographic column, and performing corresponding detection.
As an example, the first bias electrode 302 and the second bias electrode 303 are formed symmetrically along the second collecting electrode 301, and the first bias electrode 302 and the second bias electrode 303 may have a pitch of 300 μm to 1000 μm, such as 300 μm, 500 μm, 600 μm, 800 μm, 1000 μm, etc., and the adjacent second bias electrode 303 and the excitation electrode 110 may have a pitch of 500 μm to 2000 μm, such as 500 μm, 1000 μm, 1500 μm, 2000 μm, etc., and the first collecting electrode 201 and the second collecting electrode 301 may have a pitch of 200 μm to 700 μm, such as 200 μm, 450 μm, 600 μm, 700 μm, etc. The specific arrangement of the first collecting electrode 201, the second collecting electrode 301, the first bias electrode 302, and the second bias electrode 303 may be selected as needed.
Referring to fig. 2 a-2 h and 3, the present embodiment also provides a helium ion detector, which can be directly manufactured by the manufacturing process, but is not limited thereto, and can be obtained by other manufacturing processes.
In this embodiment, the helium ion detector is directly prepared by the above process, so that details regarding materials, preparation processes, structures, etc. of the helium ion detector are not described here.
Specifically, the helium ion detector comprises a sandwich structure formed by an upper cover plate, a lower cover plate and a patterned substrate, wherein a first collecting electrode 201 is arranged on the upper cover plate, namely the upper glass cover plate 200; the lower cover plate, that is, the lower glass cover plate 300 is provided with a second collecting electrode 301, a first bias electrode 302 and a second bias electrode 303 positioned at two sides of the second collecting electrode 301; the substrate, that is, the silicon substrate 100 is provided with a through groove 107 penetrating the silicon substrate 100, an input/output through groove (not shown) and an excitation electrode through groove (not shown) which are communicated with the through groove 107, the upper surface of the silicon substrate 100 is bonded to the upper glass cover plate 200, the lower surface of the silicon substrate 100 is bonded to the lower glass cover plate 300, the upper glass cover plate 200 and the lower glass cover plate 300 cover the through groove 107 to form a closed chamber 500, the input/output through groove is covered to form a closed input/output channel, the closed input/output channel comprises a sample input channel 600, a carrier gas input channel 700, a gas output channel 800 and an excitation electrode through groove is covered to form an excitation electrode channel 900, the first collecting electrode 201, the second collecting electrode 301, the first biasing electrode 302 and the second biasing electrode 303 are exposed to the closed chamber 500, and the first collecting electrode 201 and the second collecting electrode 301 are correspondingly arranged to form a counter collector.
The detection performance of the helium ion detector in this embodiment is tested below, wherein the excitation voltage may be 100V to 600V, the first collecting electrode 201 is electrically connected to the signal collecting module, and the second collecting electrode 301, the first biasing electrode 302 and the second biasing electrode 303 provide the positive bias for testing.
Referring to FIG. 4a, a graph of flow velocity field distribution in a helium ion detector according to the present embodiment is shown, and FIG. 4b, a graph of flow velocity at glow excitation in accordance with x-coordinate of the helium ion detector according to the present embodiment is shown. As can be seen from fig. 4b, the flow velocity field in the helium ion discharge region is stable, the flow velocity is small, stable plasma radicals can be obtained, and the flow velocity is stable, so that the shaking of the plasma radicals is small, and lower noise can be obtained.
Referring to fig. 5a, a simulated distribution diagram of electric field lines of a helium ion detector using a collecting electrode in this embodiment is shown, fig. 5b, a simulated distribution diagram of electric field lines of a helium ion detector using a planar collecting electrode in this embodiment is shown, fig. 5c, a graph of electric field strength of a helium ion detector using a collecting electrode plate in this embodiment as a function of Y-coordinate is shown, and fig. 5d, a graph of electric field strength of a helium ion detector using a planar collecting electrode plate in this embodiment as a function of Y-coordinate is shown. As can be seen from fig. 5c and 5d, the electric field strength in the collecting electrode is about 5 times that in the planar collecting electrode as seen from the electric field strength above the collecting electrode plate. The combination of the bias electrode has more ideal electric field line distribution to the collecting electrode structure and higher ion collecting efficiency.
Referring to FIG. 6, there is shown a graph of the chromatographic outflow of the helium ion detector of this example in combination with a chromatographic column versus C2-C4 test, wherein the sensitivity of the helium ion detector with high sensitivity to the collecting electrode was tested with 1ppm C2-C4 alkane mixture, which can be seen to have a higher sensitivity to 1ppm C2-C4 with a signal to noise ratio of up to 13.
In summary, according to the helium ion detector and the preparation method thereof, the ideal electric field distribution can be obtained by arranging the pair of collecting electrodes in the closed chamber, and the ion collecting efficiency can be effectively improved by combining the pair of collecting electrodes in the closed chamber, so that the helium ion detector has lower detection limit and higher detection sensitivity on the premise of smaller volume. In addition, the helium ion detector adopts a sandwich structure, and is suitable for being combined with a chromatographic column or being monolithically integrated with a micro-chromatographic column.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. A method of manufacturing a helium ion detector comprising the steps of:
providing a substrate;
providing an upper cover plate and a lower cover plate, forming a first collecting electrode on the upper cover plate, forming a second collecting electrode on the lower cover plate, and forming a first bias electrode and a second bias electrode which are positioned on two sides of the second collecting electrode;
bonding the lower cover plate with the lower surface of the substrate;
patterning the substrate, forming a through groove penetrating through the substrate, an input/output through groove communicated with the through groove and an excitation electrode through groove in the substrate, wherein the through groove exposes the second collecting electrode, the first bias electrode and the second bias electrode;
and bonding the upper cover plate with the upper surface of the substrate, covering the through groove by the upper cover plate to form a closed cavity, covering the input/output through groove to form a closed input/output channel and covering the excitation electrode through groove to form an excitation electrode channel, wherein the first collecting electrode is exposed in the closed cavity and is correspondingly arranged with the second collecting electrode to form a opposite collecting electrode.
2. A method of making a helium ion detector according to claim 1, wherein: the step of patterning the substrate is completed before the bonding step.
3. A method of making a helium ion detector according to claim 1, wherein: the upper cover plate is bonded with the upper surface of the base plate, and then the lower cover plate is bonded with the lower surface of the base plate.
4. A method of making a helium ion detector according to claim 1, wherein: an electrode accommodating groove for accommodating the first collecting electrode is formed on the upper surface of the substrate, and electrode accommodating grooves for accommodating the second collecting electrode, the first biasing electrode and the second biasing electrode are formed on the lower surface of the substrate.
5. A method of making a helium ion detector according to claim 1, wherein: the patterning of the substrate to form the through-slot further comprises a step of forming an electrode protection layer covering the electrode, and the patterning of the substrate to form the through-slot further comprises a step of removing the electrode protection layer.
6. A method of making a helium ion detector according to claim 1, wherein: and the method further comprises the step of scribing, and during scribing, positive and negative scribing is performed from the upper cover plate and the lower cover plate respectively so as to expose the electrical connection ends of the first collecting electrode, the second collecting electrode, the first biasing electrode and the second biasing electrode.
7. A method of making a helium ion detector according to claim 1, wherein: the first bias electrode and the second bias electrode are symmetrically arranged along the second collecting electrode, the distances between the first bias electrode and the second bias electrode and between the second collecting electrode and between the first bias electrode and the second collecting electrode are 300-1000 microns, the distances between the adjacent bias electrodes and the exciting electrode are 500-2000 microns, and the distances between the first collecting electrode and the second collecting electrode are 200-700 microns.
8. A method of making a helium ion detector according to claim 1, wherein: the substrate comprises a silicon substrate, a ceramic substrate or a glass substrate; the upper cover plate comprises a silicon cover plate, a ceramic cover plate or a glass cover plate; the lower cover plate comprises a silicon cover plate, a ceramic cover plate or a glass cover plate.
9. A helium ion detector, wherein the helium ion detector comprises:
the upper cover plate is provided with a first collecting electrode;
the lower cover plate is provided with a second collecting electrode, a first bias electrode and a second bias electrode which are positioned at two sides of the second collecting electrode;
the patterned substrate, be provided with in the substrate run through the base plate the slot that link up, with the input and output that link up the slot that link up is led to the slot and excitation electrode leads to the slot, just the upper surface of base plate with the upper cover plate bonding, the lower surface of base plate with the lower cover plate bonding, through upper cover plate with the lower cover plate covers the slot constitutes closed cavity, covers the input and output leads to the slot and constitutes closed input and output passageway and covers excitation electrode leads to the slot constitutes excitation electrode passageway, just first collecting electrode, second collecting electrode first biasing electrode and second biasing electrode expose in closed cavity, first collecting electrode with the second collecting electrode corresponds the setting and constitutes to receiving the collecting electrode.
10. A helium ion detector according to claim 9 wherein: the first bias electrode and the second bias electrode are symmetrically arranged along the second collecting electrode, the distances between the first bias electrode and the second bias electrode and between the second collecting electrode and between the first bias electrode and the second collecting electrode are 300-1000 microns, the distances between adjacent bias electrodes and the excitation electrode are 500-2000 microns, and the distances between the first collecting electrode and the second collecting electrode are 200-700 microns.
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| CN202311526934.4A CN117451910A (en) | 2023-11-15 | 2023-11-15 | Helium ion detector and preparation method thereof |
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| CN202311526934.4A CN117451910A (en) | 2023-11-15 | 2023-11-15 | Helium ion detector and preparation method thereof |
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