CN116625347A - Atomic gas chamber and manufacturing method thereof - Google Patents
Atomic gas chamber and manufacturing method thereof Download PDFInfo
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- CN116625347A CN116625347A CN202310593744.8A CN202310593744A CN116625347A CN 116625347 A CN116625347 A CN 116625347A CN 202310593744 A CN202310593744 A CN 202310593744A CN 116625347 A CN116625347 A CN 116625347A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 291
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 177
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 177
- 239000010703 silicon Substances 0.000 claims abstract description 177
- 239000011521 glass Substances 0.000 claims abstract description 125
- 229920002120 photoresistant polymer Polymers 0.000 claims description 56
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 44
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 19
- 238000005530 etching Methods 0.000 claims description 16
- 238000000059 patterning Methods 0.000 claims description 15
- 238000009832 plasma treatment Methods 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 abstract description 10
- 239000007789 gas Substances 0.000 description 56
- 238000004140 cleaning Methods 0.000 description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000001994 activation Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 230000000977 initiatory effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000008358 core component Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01C—MEASURING DISTANCES, LEVELS OR BEARINGS; SURVEYING; NAVIGATION; GYROSCOPIC INSTRUMENTS; PHOTOGRAMMETRY OR VIDEOGRAMMETRY
- G01C19/00—Gyroscopes; Turn-sensitive devices using vibrating masses; Turn-sensitive devices without moving masses; Measuring angular rate using gyroscopic effects
- G01C19/58—Turn-sensitive devices without moving masses
- G01C19/60—Electronic or nuclear magnetic resonance gyrometers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/02—Measuring direction or magnitude of magnetic fields or magnetic flux
- G01R33/032—Measuring direction or magnitude of magnetic fields or magnetic flux using magneto-optic devices, e.g. Faraday or Cotton-Mouton effect
-
- G—PHYSICS
- G04—HOROLOGY
- G04F—TIME-INTERVAL MEASURING
- G04F5/00—Apparatus for producing preselected time intervals for use as timing standards
- G04F5/14—Apparatus for producing preselected time intervals for use as timing standards using atomic clocks
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Radar, Positioning & Navigation (AREA)
- Remote Sensing (AREA)
- Power Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Micromachines (AREA)
Abstract
The invention provides an atomic gas chamber and a manufacturing method thereof, and belongs to the technical field of manufacturing of atomic gas chambers. An atomic gas chamber including a first silicon substrate, a glass substrate, and a second silicon substrate laminated in this order; the first surface of the first silicon substrate facing the second silicon substrate is provided with a plurality of first grooves which are arranged at intervals; the glass substrate comprises a plurality of through holes which are arranged at intervals, the through holes are in one-to-one correspondence with the first grooves, and orthographic projection of the through holes on the first silicon substrate falls into the corresponding first grooves; a plurality of second grooves which are arranged at intervals are formed in the second surface of the second silicon substrate, which faces the first silicon substrate, the through holes are in one-to-one correspondence with the second grooves, and orthographic projection of the through holes on the second silicon substrate falls into the corresponding second grooves; each through hole, the corresponding first groove and the corresponding second groove form a cavity. The technical scheme of the invention can simplify the preparation process of the atomic gas chamber.
Description
Technical Field
The invention relates to the technical field of manufacturing of atomic air chambers, in particular to an atomic air chamber and a manufacturing method thereof.
Background
The atomic air chamber is a core physical component of an atomic instrument such as a nuclear magnetic resonance gyroscope, an atomic clock, an atomic interference magnetometer and the like, and the performance of the atomic air chamber directly determines the precision of the atomic instrument.
Disclosure of Invention
The invention aims to provide an atomic air chamber and a manufacturing method thereof, which can simplify the preparation process of the atomic air chamber and improve the performance of the atomic air chamber.
In order to solve the technical problems, the embodiment of the invention provides the following technical scheme:
in one aspect, an atomic gas chamber is provided, comprising a first silicon substrate, a glass substrate, and a second silicon substrate, which are sequentially stacked;
the first surface of the first silicon substrate facing the second silicon substrate is provided with a plurality of first grooves which are arranged at intervals;
the glass substrate comprises a plurality of through holes which are arranged at intervals, the through holes are in one-to-one correspondence with the first grooves, and orthographic projection of the through holes on the first silicon substrate falls into the corresponding first grooves;
a plurality of second grooves which are arranged at intervals are formed in the second surface of the second silicon substrate, which faces the first silicon substrate, the through holes are in one-to-one correspondence with the second grooves, and orthographic projection of the through holes on the second silicon substrate falls into the corresponding second grooves;
each through hole, the corresponding first groove and the corresponding second groove form a cavity.
In some embodiments, further comprising:
a first silicon nitride film located on a side surface of the first groove facing the second silicon substrate;
and the second silicon nitride film is positioned on one side surface of the second groove facing the first silicon substrate.
In some embodiments, the first silicon nitride film has a thickness of 0.1-1 μm;
the thickness of the second silicon nitride film is 0.1-1 mu m.
In some embodiments, the distance between adjacent chambers is 0.1-1mm, and the diameter of the chambers is 0.1-1mm.
The embodiment of the invention also provides a manufacturing method of the atomic air chamber, which comprises the following steps:
providing a first silicon substrate, patterning the first silicon substrate, and forming a plurality of first grooves which are arranged at intervals on the first surface of the first silicon substrate;
providing a glass substrate, patterning the glass substrate, and forming a plurality of through holes which are arranged at intervals, wherein the through holes are in one-to-one correspondence with the first grooves;
providing a second silicon substrate, patterning the second silicon substrate, forming a plurality of second grooves which are arranged at intervals on the second surface of the second silicon substrate, wherein the through holes are in one-to-one correspondence with the second grooves;
and bonding the glass substrate with the first surface and the second surface respectively, wherein orthographic projections of the through holes on the first silicon substrate fall into corresponding first grooves, orthographic projections of the through holes on the second silicon substrate fall into corresponding second grooves, and each through hole and the corresponding first grooves and second grooves form a cavity.
In some embodiments, bonding the glass substrate to the first surface and the second surface, respectively, comprises:
the first surface and the glass substrate are respectively connected with the positive electrode and the negative electrode of a power supply, and the glass substrate and the first surface are subjected to anodic bonding for 0.1-3 hours under the conditions that the pressure is 0-100kN, the temperature is 100-500 ℃ and the voltage is 100-1200V;
and respectively connecting the second surface and the glass substrate with the positive electrode and the negative electrode of a power supply, and performing anodic bonding on the glass substrate and the second surface for 0.1-3 hours under the conditions that the pressure is 0-100kN, the temperature is 100-500 ℃ and the voltage is 100-1200V.
In some embodiments, bonding the glass substrate to the first surface and the second surface, respectively, comprises:
silicon-silicon bonding the glass substrate and the first surface for 0.1-3 hours under the conditions that the pressure is 0-100kN and the temperature is 100-500 ℃;
and (3) silicon-silicon bonding the glass substrate and the second surface for 0.1-3 hours under the conditions that the pressure is 0-100kN and the temperature is 100-500 ℃.
In some embodiments, before the bonding the glass substrate to the first surface and the second surface, respectively, the method further comprises:
forming a first silicon nitride film on the first surface with the first groove by chemical vapor deposition, wherein the first silicon nitride film covers the first groove;
and forming a second silicon nitride film on the second surface with the second groove by chemical vapor deposition, wherein the second silicon nitride film covers the second groove.
In some embodiments, the patterning the glass substrate to form a plurality of spaced-apart vias includes:
irradiating a preset area of the glass substrate with laser light;
and removing the preset area by using an acidic etching solution to obtain the through hole.
In some embodiments, the patterning the first silicon substrate includes:
coating photoresist on the first surface of the first silicon substrate, exposing and developing the photoresist to form a photoresist pattern, and etching the first silicon substrate by taking the photoresist pattern as a mask to form the first groove;
the patterning the second silicon substrate includes:
and coating photoresist on the second surface of the second silicon substrate, exposing and developing the photoresist to form a photoresist pattern, and etching the second silicon substrate by taking the photoresist pattern as a mask to form the second groove.
In some embodiments, before the bonding the glass substrate to the first surface and the second surface, respectively, the method further comprises:
and performing plasma treatment on the first surface, the second surface and the surface of the glass substrate.
The embodiment of the invention has the following beneficial effects:
in the scheme, the atomic gas chamber with the silicon-glass-silicon structure is prepared, metal sputtering is not needed in the preparation process, metal removal is not needed after bonding is completed, the preparation process of the atomic gas chamber can be simplified, the occurrence of bad risks is avoided, and the performance of the atomic gas chamber is improved.
Drawings
Fig. 1-9 are schematic diagrams of an atomic gas chamber according to an embodiment of the present invention.
Reference numerals
01. First silicon substrate
02. Glass substrate
03. Third silicon substrate
04. Photoresist
05. Silicon nitride film
06. Chamber chamber
011. First groove
031. Second groove
021. Through hole
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the embodiments of the present invention more apparent, the following detailed description will be given with reference to the accompanying drawings and the specific embodiments.
In the related art, an atomic gas chamber adopts a glass-silicon-glass structure, after a silicon substrate and a first glass substrate are prepared, the silicon substrate and the first glass substrate are subjected to first anodic bonding under vacuum, the glass substrate is connected with a negative electrode of a power supply during bonding, the silicon substrate is connected with a positive electrode of the power supply, both an upper electrode and a lower electrode are heated to 330 ℃, the pressure of 500mbar is applied to enable the silicon substrate and the glass substrate to be closely attached, after the pressure and the temperature are stable, 1000V voltage is applied for 20-30 minutes, na+ in the glass substrate moves towards the negative electrode, a depletion layer is formed at a silicon/glass bonding interface, O2-in the glass substrate is subjected to chemical reaction with silicon at the silicon/glass bonding interface to form a firm Si-O chemical bond, and the silicon/glass is bonded together, so that the first anodic bonding is completed. In the second anodic bonding of the silicon substrate and the second glass substrate, in order to improve conductivity in the bonding process, an Al film is formed on one side of the second glass substrate away from the silicon substrate, and silver colloid is formed on the side edges of the silicon substrate and the second glass substrate, so that the Al film on the back surface of the glass substrate can be communicated with the silicon substrate through the silver colloid on the side edges in the second anodic bonding, and then the second anodic bonding is performed, wherein the conditions of the second anodic bonding are the same as those of the first anodic bonding. After the second anodic bonding is completed, the Al film on the back surface of the glass substrate needs to be removed, cleaning and drying are performed, when metal removal is performed, the pollution caused by the metal removal cannot meet the requirement of the atomic gas chamber on cleanliness, in addition, the Al film is formed to waste materials, and the preparation process flow of the atomic gas chamber is long and complex, so that the industrial production is not facilitated.
The embodiment of the invention provides an atomic air chamber and a manufacturing method thereof, which can simplify the preparation process of the atomic air chamber and improve the performance of the atomic air chamber.
The embodiment of the invention also provides a manufacturing method of the atomic air chamber, which comprises the following steps:
providing a first silicon substrate, patterning the first silicon substrate, and forming a plurality of first grooves which are arranged at intervals on the first surface of the first silicon substrate;
providing a glass substrate, patterning the glass substrate, and forming a plurality of through holes which are arranged at intervals, wherein the through holes are in one-to-one correspondence with the first grooves;
providing a second silicon substrate, patterning the second silicon substrate, forming a plurality of second grooves which are arranged at intervals on the second surface of the second silicon substrate, wherein the through holes are in one-to-one correspondence with the second grooves;
and bonding the glass substrate with the first surface and the second surface respectively, wherein orthographic projections of the through holes on the first silicon substrate fall into corresponding first grooves, orthographic projections of the through holes on the second silicon substrate fall into corresponding second grooves, and each through hole and the corresponding first grooves and second grooves form a cavity.
In the embodiment, the atomic gas chamber with the silicon-glass-silicon structure is prepared, metal sputtering is not needed in the preparation process, metal removal is not needed after bonding is completed, the preparation process of the atomic gas chamber can be simplified, the risk of causing bad is avoided, and the performance of the atomic gas chamber is improved.
After the atomic gas chamber of the embodiment is manufactured, the atomic gas chamber can be used as a core component of an atomic clock, a magnetometer, an interferometer and a gyroscope, and in order to solve the problem of corrosion and oxidation of the traditional atomic gas chamber and improve the service life of the atomic gas chamber, a first silicon nitride film can be formed on the first surface with the first groove formed by chemical vapor deposition before the glass substrate is bonded with the first surface and the second surface respectively, and the first silicon nitride film covers the first groove; and forming a second silicon nitride film on the second surface with the second groove by chemical vapor deposition, wherein the second silicon nitride film covers the second groove. The first silicon nitride film and the second silicon nitride film have better compactness, can protect the chamber from corrosion, and improve the service life of the atomic gas chamber.
In a specific example, the silicon substrate and the glass substrate may be bonded by anodic bonding, and the method for preparing the atomic gas chamber of the present embodiment includes the steps of:
step 1, as shown in fig. 1, providing a first silicon substrate 01, a glass substrate 02 and a second silicon substrate 03;
step 2, as shown in fig. 2, irradiating a preset area of the glass substrate 02 with laser to modify the preset area, and removing the preset area with an acidic etching solution to obtain the through hole 021;
of course, the present embodiment is not limited to the method of forming the through hole as shown in fig. 2, and the glass substrate 02 may be coated with photoresist, the photoresist pattern may be formed by exposing and developing a mask plate, and the glass substrate 02 may be etched with the photoresist pattern as a mask to form the through hole 021.
Specifically, HF in an amount of 0 to 10% by mass and HNO in an amount of 0 to 10% by mass can be used at 25 to 100 DEG C 3 Etching the preset region of the glass substrate 02 with the solution to form a through hole 021, wherein the aperture of the through hole 021 can be 0.1-1mm, the depth is the same as the thickness of the glass substrate,the spacing between adjacent through holes 021 may be 0.1-1mm.
Step 3, as shown in fig. 3, coating a photoresist 04 on a first silicon substrate 01, exposing and developing the photoresist by using a mask plate to form a pattern of the photoresist 04, etching the first silicon substrate 01 by using the pattern of the photoresist 04 as a mask, forming a first groove 011 on a first surface of the first silicon substrate 01, and removing the rest of the photoresist 04;
the diameter of the first groove 011 is the same as the aperture of the through hole 021, and may be 0.1-1mm, the distance between adjacent first grooves may be 0.1-1mm, and the depth of the first groove may be 1-120 μm.
Step 4, cleaning the first silicon substrate and the glass substrate by using RCA cleaning liquid for 1-50 minutes, washing the first silicon substrate and the glass substrate by using water after cleaning, and drying the first silicon substrate and the glass substrate;
step 5, performing plasma treatment on the first surface of the first silicon substrate 01 and the surface of the glass substrate 02;
specifically, the first surface of the first silicon substrate 01 and the surface of the glass substrate 02 may be subjected to plasma treatment with oxygen and/or argon plasma for 0.1 to 3 hours under the conditions that the gas flow is 5 to 300sccm and the power is 5 to 500W, the first silicon substrate 01 and the glass substrate 02 are washed with water, and then the first silicon substrate 01 and the glass substrate 02 are dried; the embodiment increases the ion activation process to improve the bonding strength and can meet the requirement of an atomic clock on the evaluation index of the atomic gas chamber.
Step 6, as shown in fig. 5, connecting a first surface of a first silicon substrate 01 and the glass substrate 02 with a positive electrode and a negative electrode of a power supply respectively, and performing anodic bonding on the glass substrate 02 and the first surface for 0.1-3 hours under the conditions of 0-100kN of pressure, 100-500 ℃ of temperature and 100-1200V of voltage to obtain a bonding body shown in fig. 5;
step 7, coating photoresist on the second silicon substrate 03, exposing and developing the photoresist by using a mask plate to form a photoresist pattern, etching the second silicon substrate 03 by using the photoresist pattern as a mask, forming a second groove 031 on the second surface of the second silicon substrate 03, and removing the residual photoresist as shown in fig. 4;
wherein the diameter of the second grooves 031 is the same as the aperture of the through holes 021, and may be 0.1-1mm, the distance between adjacent second grooves 031 may be 0.1-1mm, and the depth of the second grooves 031 may be 1-120 μm.
Cleaning the second silicon substrate 03 by using RCA cleaning solution for 1-50 minutes, washing the second silicon substrate 03 by using water after cleaning, and drying the second silicon substrate 03;
plasma processing is carried out on the second surface of the second silicon substrate 03 and the surface of the glass substrate 02 on the side far away from the first silicon substrate;
specifically, the second surface of the second silicon substrate 03 and the surface of the glass substrate 02 may be subjected to plasma treatment with oxygen and/or argon plasma at a gas flow rate of 5-300sccm and a power of 5-500W for 0.1-3 hours, and the bonded body shown in fig. 5 and the second silicon substrate 03 may be washed with water, and then dried; the embodiment increases the ion activation process to improve the bonding strength and can meet the requirement of an atomic clock on the evaluation index of the atomic gas chamber.
Step 8, as shown in fig. 6, the second surface of the second silicon substrate 03 and the glass substrate 02 are respectively connected with the positive electrode and the negative electrode of the power supply, and the second surface of the second silicon substrate 03 and the glass substrate 02 are subjected to anodic bonding for 0.1-3 hours under the conditions of the pressure of 0-100kN, the temperature of 100-500 ℃ and the voltage of 100-1200V.
After the secondary anodic bonding is performed, a chamber 06 as shown in fig. 6 is formed, and the thickness of the chamber 06 is equal to the sum of the depth of the first groove, the depth of the through hole, and the depth of the second groove. Compared with the traditional large-size glass bubble photoinitiation atomic gas chamber, the structural size of the full-angle chamber manufactured by the embodiment can be greatly and little adjusted, the limit value of the using angle of the full-angle chamber is changed by the polarized size, the full-angle chamber can be used for photoinitiation and thermal initiation of the two atomic gas chambers, and the application scene is expanded.
The present embodiment can firmly bond the silicon substrate with the glass substrate by optimizing the discharge time.
In another specific example, the silicon substrate may be bonded to the glass substrate by silicon-silicon bonding, and the method of manufacturing the atomic gas cell of the present embodiment includes the steps of:
step 1, as shown in fig. 1, providing a first silicon substrate 01, a glass substrate 02 and a second silicon substrate 03;
step 2, as shown in fig. 2, irradiating a preset area of the glass substrate 02 with laser to modify the preset area, and removing the preset area with an acidic etching solution to obtain the through hole 021;
of course, the present embodiment is not limited to the method of forming the through hole as shown in fig. 2, and the glass substrate 02 may be coated with photoresist, the photoresist pattern may be formed by exposing and developing a mask plate, and the glass substrate 02 may be etched with the photoresist pattern as a mask to form the through hole 021.
Specifically, HF in an amount of 0 to 10% by mass and HNO in an amount of 0 to 10% by mass can be used at 25 to 100 DEG C 3 The solution etches the preset area of the glass substrate 02 to form through holes 021, the aperture of the through holes 021 can be 0.1-1mm, the depth is the same as the thickness of the glass substrate, and the interval between adjacent through holes 021 can be 0.1-1mm.
Step 3, as shown in fig. 3, coating a photoresist 04 on a first silicon substrate 01, exposing and developing the photoresist by using a mask plate to form a pattern of the photoresist 04, etching the first silicon substrate 01 by using the pattern of the photoresist 04 as a mask, forming a first groove 011 on a first surface of the first silicon substrate 01, and removing the rest of the photoresist 04;
the diameter of the first groove 011 is the same as the aperture of the through hole 021, and may be 0.1-1mm, the distance between adjacent first grooves may be 0.1-1mm, and the depth of the first groove may be 1-120 μm.
Step 4, cleaning the first silicon substrate and the glass substrate by using RCA cleaning liquid for 1-50 minutes, washing the first silicon substrate and the glass substrate by using water after cleaning, and drying the first silicon substrate and the glass substrate;
step 5, performing plasma treatment on the first surface of the first silicon substrate 01 and the surface of the glass substrate 02;
specifically, the first surface of the first silicon substrate 01 and the surface of the glass substrate 02 may be subjected to plasma treatment with oxygen and/or argon plasma for 0.1 to 3 hours under the conditions that the gas flow is 5 to 300sccm and the power is 5 to 500W, the first silicon substrate 01 and the glass substrate 02 are washed with water, and then the first silicon substrate 01 and the glass substrate 02 are dried; the embodiment increases the ion activation process to improve the bonding strength and can meet the requirement of an atomic clock on the evaluation index of the atomic gas chamber.
Step 6, as shown in fig. 5, under the conditions that the pressure is 0-100kN and the temperature is 100-500 ℃, silicon-silicon bonding is carried out on the glass substrate 02 and the first surface of the first silicon substrate 01 for 0.1-3 hours, so as to obtain a bonding body shown in fig. 5;
step 7, coating photoresist on the second silicon substrate 03, exposing and developing the photoresist by using a mask plate to form a photoresist pattern, etching the second silicon substrate 03 by using the photoresist pattern as a mask, forming a second groove 031 on the second surface of the second silicon substrate 03, and removing the residual photoresist as shown in fig. 4;
wherein the diameter of the second grooves 031 is the same as the aperture of the through holes 021, and may be 0.1-1mm, the distance between adjacent second grooves 031 may be 0.1-1mm, and the depth of the second grooves 031 may be 1-120 μm.
Cleaning the second silicon substrate 03 by using RCA cleaning solution for 1-50 minutes, washing the second silicon substrate 03 by using water after cleaning, and drying the second silicon substrate 03;
plasma processing is carried out on the second surface of the second silicon substrate 03 and the surface of the glass substrate 02 on the side far away from the first silicon substrate;
specifically, the second surface of the second silicon substrate 03 and the surface of the glass substrate 02 may be subjected to plasma treatment with oxygen and/or argon plasma at a gas flow rate of 5-300sccm and a power of 5-500W for 0.1-3 hours, and the bonded body shown in fig. 5 and the second silicon substrate 03 may be washed with water, and then dried; the embodiment increases the ion activation process to improve the bonding strength and can meet the requirement of an atomic clock on the evaluation index of the atomic gas chamber.
And 8, as shown in fig. 6, silicon-silicon bonding is carried out on the second surface of the glass substrate 02 and the second silicon substrate 03 for 0.1-3 hours under the conditions that the pressure is 0-100kN and the temperature is 100-500 ℃.
After the secondary anodic bonding is performed, a chamber 06 as shown in fig. 6 is formed, and the thickness of the chamber 06 is equal to the sum of the depth of the first groove, the depth of the through hole, and the depth of the second groove. Compared with the traditional large-size glass bubble photoinitiation atomic gas chamber, the structural size of the full-angle chamber manufactured by the embodiment can be greatly and little adjusted, the limit value of the using angle of the full-angle chamber is changed by the polarized size, the full-angle chamber can be used for photoinitiation and thermal initiation of the two atomic gas chambers, and the application scene is expanded.
The embodiment solves the bonding problem of the micron-sized dielectric layer by optimizing the pressure and the temperature, and can firmly combine the silicon substrate with the glass substrate.
In another specific example, a silicon substrate may be bonded to a glass substrate by anodic bonding, and a durable atomic gas chamber may be prepared, and the method of preparing the atomic gas chamber of the present embodiment includes the steps of:
step 1, as shown in fig. 1, providing a first silicon substrate 01, a glass substrate 02 and a second silicon substrate 03;
step 2, as shown in fig. 2, irradiating a preset area of the glass substrate 02 with laser to modify the preset area, and removing the preset area with an acidic etching solution to obtain the through hole 021;
of course, the present embodiment is not limited to the method of forming the through hole as shown in fig. 2, and the glass substrate 02 may be coated with photoresist, the photoresist pattern may be formed by exposing and developing a mask plate, and the glass substrate 02 may be etched with the photoresist pattern as a mask to form the through hole 021.
Specifically, it can be at 2At 5-100deg.C, HF with mass fraction of 0-10% and HNO with mass fraction of 0-10% 3 The solution etches the preset area of the glass substrate 02 to form through holes 021, the aperture of the through holes 021 can be 0.1-1mm, the depth is the same as the thickness of the glass substrate, and the interval between adjacent through holes 021 can be 0.1-1mm.
Step 3, as shown in fig. 3, coating a photoresist 04 on a first silicon substrate 01, exposing and developing the photoresist by using a mask plate to form a pattern of the photoresist 04, etching the first silicon substrate 01 by using the pattern of the photoresist 04 as a mask, forming a first groove 011 on a first surface of the first silicon substrate 01, and removing the rest of the photoresist 04;
the diameter of the first groove 011 is the same as the aperture of the through hole 021, and may be 0.1-1mm, the distance between adjacent first grooves may be 0.1-1mm, and the depth of the first groove may be 1-120 μm.
Step 4, cleaning the first silicon substrate and the glass substrate by using RCA cleaning liquid for 1-50 minutes, washing the first silicon substrate and the glass substrate by using water after cleaning, and drying the first silicon substrate and the glass substrate;
step 5, as shown in fig. 7, forming a silicon nitride film 05 on the first silicon substrate 01, wherein the silicon nitride film 05 covers the first groove 011;
specifically, a dense silicon nitride film with a thickness of 0.1-1 μm can be formed on the first silicon substrate 01 by controlling the film forming gas ratio through chemical vapor deposition. In this embodiment, the thickness of the silicon nitride film 05 is designed so that the silicon nitride film 05 does not affect the subsequent bonding process. The silicon nitride film 05 has better compactness, can protect the first silicon substrate 01 from corrosion, improves the service life of the atomic gas chamber, and widens the application field of the atomic gas chamber.
Step 6, performing plasma treatment on the first surface of the first silicon substrate 01 and the surface of the glass substrate 02;
specifically, the first surface of the first silicon substrate 01 and the surface of the glass substrate 02 may be subjected to plasma treatment with oxygen and/or argon plasma for 0.1 to 3 hours under the conditions that the gas flow is 5 to 300sccm and the power is 5 to 500W, the first silicon substrate 01 and the glass substrate 02 are washed with water, and then the first silicon substrate 01 and the glass substrate 02 are dried; the embodiment increases the ion activation process to improve the bonding strength and can meet the requirement of an atomic clock on the evaluation index of the atomic gas chamber.
Step 7, as shown in fig. 9, connecting a first surface of a first silicon substrate 01 and the glass substrate 02 with a positive electrode and a negative electrode of a power supply respectively, and performing anodic bonding on the glass substrate 02 and the first surface for 0.1-3 hours under the conditions that the pressure is 0-100kN, the temperature is 100-500 ℃ and the voltage is 100-1200V;
step 8, coating photoresist on the second silicon substrate 03, exposing and developing the photoresist by using a mask plate to form a photoresist pattern, etching the second silicon substrate 03 by using the photoresist pattern as a mask, forming a second groove 031 on the second surface of the second silicon substrate 03, and removing the rest photoresist;
wherein the diameter of the second grooves 031 is the same as the aperture of the through holes 021, and may be 0.1-1mm, the distance between adjacent second grooves 031 may be 0.1-1mm, and the depth of the second grooves 031 may be 1-120 μm.
Cleaning the second silicon substrate 03 by using RCA cleaning solution for 1-50 minutes, washing the second silicon substrate 03 by using water after cleaning, and drying the second silicon substrate 03;
as shown in fig. 8, a silicon nitride film 05 is formed on the second surface of the second silicon substrate 03, the silicon nitride film 05 covering the second grooves 031;
specifically, a dense silicon nitride film with a thickness of 0.1-1 μm can be formed on the second silicon substrate 03 by controlling the film forming gas ratio by chemical vapor deposition. In this embodiment, the thickness of the silicon nitride film 05 is designed so that the silicon nitride film 05 does not affect the subsequent bonding process. The silicon nitride film 05 has better compactness, can protect the second silicon substrate 03 from corrosion, improves the service life of the atomic gas chamber, and widens the application field of the atomic gas chamber.
Plasma processing is carried out on the second surface of the second silicon substrate 03 and the surface of the glass substrate 02 on the side far away from the first silicon substrate;
specifically, the second surface of the second silicon substrate 03 and the surface of the glass substrate 02 may be subjected to plasma treatment with oxygen and/or argon plasma at a gas flow rate of 5-300sccm and a power of 5-500W for 0.1-3 hours, the second silicon substrate 03 and the bonded body may be washed with water, and then the second silicon substrate 03 and the bonded body may be dried; the embodiment increases the ion activation process to improve the bonding strength and can meet the requirement of an atomic clock on the evaluation index of the atomic gas chamber.
Step 9, as shown in fig. 9, the second surface of the second silicon substrate 03 and the glass substrate 02 are respectively connected with the positive electrode and the negative electrode of the power supply, and the second surface of the second silicon substrate 03 and the glass substrate 02 are subjected to anodic bonding for 0.1-3 hours under the conditions of the pressure of 0-100kN, the temperature of 100-500 ℃ and the voltage of 100-1200V.
After the secondary anodic bonding, a chamber 06 as shown in fig. 9 is formed. Compared with the traditional large-size glass bubble photoinitiation atomic gas chamber, the structural size of the full-angle chamber manufactured by the embodiment can be greatly and little adjusted, the limit value of the using angle of the full-angle chamber is changed by the polarized size, the full-angle chamber can be used for photoinitiation and thermal initiation of the two atomic gas chambers, and the application scene is expanded.
The present embodiment can firmly bond the silicon substrate with the glass substrate by optimizing the discharge time.
The embodiment of the invention also provides an atomic gas chamber which is manufactured by adopting the method, and comprises a first silicon substrate, a glass substrate and a second silicon substrate which are sequentially laminated;
the first surface of the first silicon substrate facing the second silicon substrate is provided with a plurality of first grooves which are arranged at intervals;
the glass substrate comprises a plurality of through holes which are arranged at intervals, the through holes are in one-to-one correspondence with the first grooves, and orthographic projection of the through holes on the first silicon substrate falls into the corresponding first grooves;
a plurality of second grooves which are arranged at intervals are formed in the second surface of the second silicon substrate, which faces the first silicon substrate, the through holes are in one-to-one correspondence with the second grooves, and orthographic projection of the through holes on the second silicon substrate falls into the corresponding second grooves;
each through hole, the corresponding first groove and the corresponding second groove form a cavity.
In the embodiment, the atomic gas chamber with the silicon-glass-silicon structure is prepared, metal sputtering is not needed in the preparation process, metal removal is not needed after bonding is completed, the preparation process of the atomic gas chamber can be simplified, the risk of causing bad is avoided, and the performance of the atomic gas chamber is improved.
After the atomic gas chamber of this embodiment is manufactured, can be used as the core component of atomic clock, magnetometer, interferometer, gyroscope, in order to solve the corrosion oxidation problem of traditional atomic gas chamber, improve the life-span of atomic gas chamber, in some embodiments, atomic gas chamber still includes:
a first silicon nitride film located on a side surface of the first groove facing the second silicon substrate;
and the second silicon nitride film is positioned on one side surface of the second groove facing the first silicon substrate.
The first silicon nitride film and the second silicon nitride film have better compactness, can protect the chamber from corrosion, and improve the service life of the atomic gas chamber.
In some embodiments, the thickness of the first silicon nitride film may be 0.1-1 μm;
the second silicon nitride film may have a thickness of 0.1 to 1 μm.
In this embodiment, the thickness of the silicon nitride film is designed so that the silicon nitride film does not affect the subsequent bonding process. The silicon nitride film has better compactness, can protect the first silicon substrate and the second silicon substrate from corrosion, improves the service life of the atomic gas chamber, and widens the application field of the atomic gas chamber.
In some embodiments, the distance between adjacent chambers may be 0.1-1mm, and the diameter of the chambers may be 0.1-1mm. Compared with the traditional large-size glass bubble photoinitiation atomic air chamber, the structural size of the full-angle chamber manufactured by the embodiment can be greatly and little adjusted, the limit value of the use angle of the full-angle chamber is changed by the maximized size, the full-angle chamber can be used for photoinitiation and thermal initiation of the two atomic air chambers, and the application scene is expanded.
In the method embodiments of the present invention, the serial numbers of the steps are not used to define the sequence of the steps, and it is within the scope of the present invention for those skilled in the art to change the sequence of the steps without performing any creative effort.
In this specification, all embodiments are described in a progressive manner, and identical and similar parts of the embodiments are all referred to each other, and each embodiment is mainly described in a different way from other embodiments. In particular, for the embodiments, since they are substantially similar to the product embodiments, the description is relatively simple, and the relevant points are found in the section of the product embodiments.
Unless defined otherwise, technical or scientific terms used in this disclosure should be given the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The terms "first," "second," and the like, as used in this disclosure, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
It will be understood that when an element such as a layer, film, region or substrate is referred to as being "on" or "under" another element, it can be "directly on" or "under" the other element or intervening elements may be present.
In the description of the above embodiments, particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely specific embodiments of the disclosure, but the protection scope of the disclosure is not limited thereto, and any person skilled in the art can easily think about changes or substitutions within the technical scope of the disclosure, and it is intended to cover the scope of the disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (11)
1. An atomic gas chamber is characterized by comprising a first silicon substrate, a glass substrate and a second silicon substrate which are sequentially laminated;
the first surface of the first silicon substrate facing the second silicon substrate is provided with a plurality of first grooves which are arranged at intervals;
the glass substrate comprises a plurality of through holes which are arranged at intervals, the through holes are in one-to-one correspondence with the first grooves, and orthographic projection of the through holes on the first silicon substrate falls into the corresponding first grooves;
a plurality of second grooves which are arranged at intervals are formed in the second surface of the second silicon substrate, which faces the first silicon substrate, the through holes are in one-to-one correspondence with the second grooves, and orthographic projection of the through holes on the second silicon substrate falls into the corresponding second grooves;
each through hole, the corresponding first groove and the corresponding second groove form a cavity.
2. An atomic gas chamber according to claim 1, further comprising:
a first silicon nitride film located on a side surface of the first groove facing the second silicon substrate;
and the second silicon nitride film is positioned on one side surface of the second groove facing the first silicon substrate.
3. An atomic gas chamber according to claim 2, wherein,
the thickness of the first silicon nitride film is 0.1-1 mu m;
the thickness of the second silicon nitride film is 0.1-1 mu m.
4. An atomic gas chamber according to claim 1, wherein the distance between adjacent chambers is 0.1-1mm, the diameter of the chambers being 0.1-1mm.
5. A method of making an atomic gas cell comprising:
providing a first silicon substrate, patterning the first silicon substrate, and forming a plurality of first grooves which are arranged at intervals on the first surface of the first silicon substrate;
providing a glass substrate, patterning the glass substrate, and forming a plurality of through holes which are arranged at intervals, wherein the through holes are in one-to-one correspondence with the first grooves;
providing a second silicon substrate, patterning the second silicon substrate, forming a plurality of second grooves which are arranged at intervals on the second surface of the second silicon substrate, wherein the through holes are in one-to-one correspondence with the second grooves;
and bonding the glass substrate with the first surface and the second surface respectively, wherein orthographic projections of the through holes on the first silicon substrate fall into corresponding first grooves, orthographic projections of the through holes on the second silicon substrate fall into corresponding second grooves, and each through hole and the corresponding first grooves and second grooves form a cavity.
6. The method of manufacturing an atomic gas cell according to claim 5, wherein bonding the glass substrate to the first surface and the second surface, respectively, comprises:
the first surface and the glass substrate are respectively connected with the positive electrode and the negative electrode of a power supply, and the glass substrate and the first surface are subjected to anodic bonding for 0.1-3 hours under the conditions that the pressure is 0-100kN, the temperature is 100-500 ℃ and the voltage is 100-1200V;
and respectively connecting the second surface and the glass substrate with the positive electrode and the negative electrode of a power supply, and performing anodic bonding on the glass substrate and the second surface for 0.1-3 hours under the conditions that the pressure is 0-100kN, the temperature is 100-500 ℃ and the voltage is 100-1200V.
7. The method of manufacturing an atomic gas cell according to claim 5, wherein bonding the glass substrate to the first surface and the second surface, respectively, comprises:
silicon-silicon bonding the glass substrate and the first surface for 0.1-3 hours under the conditions that the pressure is 0-100kN and the temperature is 100-500 ℃;
and (3) silicon-silicon bonding the glass substrate and the second surface for 0.1-3 hours under the conditions that the pressure is 0-100kN and the temperature is 100-500 ℃.
8. The method of claim 5, wherein prior to bonding the glass substrate to the first surface and the second surface, respectively, the method further comprises:
forming a first silicon nitride film on the first surface with the first groove by chemical vapor deposition, wherein the first silicon nitride film covers the first groove;
and forming a second silicon nitride film on the second surface with the second groove by chemical vapor deposition, wherein the second silicon nitride film covers the second groove.
9. The method of claim 5, wherein patterning the glass substrate to form a plurality of spaced apart vias comprises:
irradiating a preset area of the glass substrate with laser light;
and removing the preset area by using an acidic etching solution to obtain the through hole.
10. The method of claim 5, wherein patterning the first silicon substrate comprises:
coating photoresist on the first surface of the first silicon substrate, exposing and developing the photoresist to form a photoresist pattern, and etching the first silicon substrate by taking the photoresist pattern as a mask to form the first groove;
the patterning the second silicon substrate includes:
and coating photoresist on the second surface of the second silicon substrate, exposing and developing the photoresist to form a photoresist pattern, and etching the second silicon substrate by taking the photoresist pattern as a mask to form the second groove.
11. The method of claim 5, wherein prior to bonding the glass substrate to the first surface and the second surface, respectively, the method further comprises:
and performing plasma treatment on the first surface, the second surface and the surface of the glass substrate.
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