CN113359404B - Method for manufacturing alkali metal atom gas chamber and alkali metal atom gas chamber - Google Patents

Method for manufacturing alkali metal atom gas chamber and alkali metal atom gas chamber Download PDF

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CN113359404B
CN113359404B CN202110611144.0A CN202110611144A CN113359404B CN 113359404 B CN113359404 B CN 113359404B CN 202110611144 A CN202110611144 A CN 202110611144A CN 113359404 B CN113359404 B CN 113359404B
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chamber
silicon wafer
windows
silicon
alkali metal
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CN113359404A (en
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贾云丛
焦斌斌
刘瑞文
孔延梅
云世昌
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Institute of Microelectronics of CAS
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    • 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
    • G04F5/145—Apparatus for producing preselected time intervals for use as timing standards using atomic clocks using Coherent Population Trapping
    • 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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Abstract

The invention discloses a method for manufacturing an alkali metal atom gas chamber and the alkali metal atom gas chamber, wherein the manufacturing method comprises the following steps: providing a silicon wafer; growing a hard mask layer on the upper surface and the lower surface of the silicon chip; processing each hard mask layer respectively to form a first window group and a second window group, wherein the first window group is two first windows corresponding to the first region of the silicon wafer in the axial direction, and the second window group is two second windows corresponding to the second region of the silicon wafer in the axial direction; opening silicon wafers between two first windows in the first window group to form a first cavity, and opening silicon wafers between two second windows in the second window group to form a second cavity; forming a V-shaped micro-channel with a rough inner wall surface on the upper surface of the silicon wafer between the first chamber and the second chamber by adopting a laser etching process, so that the first chamber is communicated with the second chamber; removing the hard mask layer; placing an alkali metal azide in the first chamber; and hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet.

Description

Method for manufacturing alkali metal atom gas chamber and alkali metal atom gas chamber
Technical Field
The invention belongs to the technical field of optical precision machining, and particularly relates to a manufacturing method of an alkali metal atom gas chamber and the alkali metal atom gas chamber.
Background
The chip-level atomic clock based on the coherent layout imprisoning (CPT) principle and the Micro Electro Mechanical System (MEMS) preparation process does not need a microwave resonant cavity, has the characteristics of small size, low power consumption, high stability, batch production and the like, and can be widely applied to various civil and military fields such as positioning, navigation, time service and the like. The atomic gas chamber is a core component of the chip-scale atomic clock, and determines the characteristics of the atomic clock, such as size, power consumption, stability and the like.
Because the melting point of an alkali metal simple substance used by an atomic clock is low (39.3 ℃ of rubidium and 28.4 ℃ of cesium), the chemical property is extremely active, flammable and explosive, the alkali metal simple substance cannot be placed into a cavity in a high-temperature anodic bonding mode, generally, the metal simple substance is replaced by the azide of rubidium or cesium, the azide has a high melting point and stable chemical property, and the azide is sealed into the atomic cavity in the anodic bonding mode and then is decomposed into metal atoms and buffer gas (nitrogen) by laser irradiation to form an alkali metal atomic gas chamber.
However, the laser decomposition process in the atomic gas chamber of the alkali metal may explode to generate solid residue particles, including material particles which are not completely decomposed, impurity particles on the surface of the material, and cavity particles generated by explosion damage, thereby reducing the stability and accuracy of the atomic clock frequency.
Disclosure of Invention
In view of the above, the present invention provides a method for manufacturing an alkali metal atom gas cell and an alkali metal atom gas cell, so as to at least partially solve the above technical problems.
To achieve the above object, as one aspect of the present invention, there is provided a method for manufacturing an alkali metal atom gas cell, comprising: providing a silicon wafer; and growing hard mask layers on the upper surface and the lower surface of the silicon chip. And respectively processing each hard mask layer by photoetching and etching processes to form a first window group and a second window group, wherein the first window group comprises two first windows corresponding to the first region of the silicon wafer in the axial direction, and the second window group comprises two second windows corresponding to the second region of the silicon wafer in the axial direction. And opening the silicon wafer between the two first windows in the first window group to form a first cavity, and opening the silicon wafer between the two second windows in the second window group to form a second cavity. And forming a V-shaped micro-channel with a rough inner wall surface on the upper surface of the silicon wafer between the first chamber and the second chamber by adopting a laser etching process, so that the first chamber is communicated with the second chamber. Removing the hard mask layer; placing an alkali metal azide in the first chamber; and hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet.
According to the embodiment of the invention, the step of growing the hard mask layer on the upper surface and the lower surface of the silicon chip comprises the steps of growing a first silicon oxide layer and a second silicon oxide layer on the upper surface and the lower surface of the silicon chip respectively, then growing a first silicon nitride layer on the upper surface of the first silicon oxide layer, and growing a second silicon nitride layer on the lower surface of the second silicon oxide layer.
According to the embodiment of the invention, the silicon wafer between the two first windows in the first window group is punched to form the first cavity, the silicon wafer between the two second windows in the second window group is punched to form the second cavity, the method comprises the steps of punching the silicon wafer between the two first windows in the first window group to form the first cavity by adopting any one of a wet etching process, deep reactive ion etching and sand blasting punching, and the silicon wafer between the two second windows in the second window group is punched to form the second cavity.
According to the embodiment of the invention, the silicon wafer between two first windows in the first window group is punched through to form a first chamber, and the silicon wafer between two second windows in the second window group is punched through to form a second chamber, wherein the silicon wafer between the two first windows in the first window group is etched by adopting a potassium hydroxide or tetramethylammonium hydroxide wet method to form the first chamber, and the silicon wafer between the two second windows in the second window group is etched by adopting the potassium hydroxide or tetramethylammonium hydroxide wet method to form the second chamber.
According to the embodiment of the invention, the hard mask layer removing comprises the step of removing the hard mask layer by adopting a wet etching method, wherein the wet etching method comprises a dilute phosphoric acid wet etching method and a buffered oxide etching solution wet etching method.
According to the embodiment of the invention, the step of hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet comprises the step of hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet by adopting an anodic bonding process.
As another aspect of the invention, the invention also provides an alkali metal atom gas cell, which comprises the alkali metal atom gas cell prepared by the method.
According to the embodiment of the invention, the alkali metal atom gas chamber comprises a double-chamber structure formed by sealing two glass sheets and a silicon wafer with double channels, and comprises a first chamber and a second chamber, wherein a V-shaped micro channel is arranged on the silicon sheet between the first chamber and the second chamber, and an alkali metal azide is arranged in the first chamber.
According to the embodiment of the invention, the depth of the V-shaped micro-channel is less than the thickness of the silicon chip.
According to the embodiment of the present invention, the inner wall of the V-shaped micro flow channel is rough.
The V-shaped micro-channel with the rough inner surface is formed between the first chamber and the second chamber in a laser etching mode, and the rough structure on the inner surface of the V-shaped micro-channel is used for adsorbing solid particles generated by laser explosion, so that the effect of filtering residue particles is achieved.
The invention adopts the method of growing the hard mask layer, then carrying out laser etching and then removing the hard mask layer, thereby overcoming the problem that the surface finish degree of the silicon wafer is influenced by solid residues attached to the surface of the area near the V-shaped micro-channel by the laser etching, and ensuring that the surface finish degree of the silicon wafer can meet the requirement of sealing connection with the glass sheet.
Drawings
FIG. 1 schematically illustrates a process flow diagram for the fabrication of an alkali metal atomic gas cell;
FIG. 2 is a schematic diagram showing a cross-sectional structure of a silicon wafer for forming a hard mask layer;
FIG. 3 is a schematic diagram showing a cross-sectional structure of a silicon wafer after a first window group and a second window group are formed;
FIG. 4a is a schematic diagram showing a cross-sectional structure of a silicon wafer after a first chamber and a second chamber are formed;
FIG. 4b is a schematic top view of the silicon wafer structure after the first and second chambers are formed;
FIG. 5a is a schematic diagram showing the cross-sectional structure of a silicon wafer after forming a V-shaped microchannel;
FIG. 5b is a schematic top view of the structure of the silicon wafer after the formation of the V-shaped micro flow channels;
FIG. 6 is a schematic cross-sectional view of a silicon wafer after the hard mask layer is removed;
FIG. 7a schematically shows a cross-sectional structural view of an alkali metal atom gas cell;
FIG. 7b schematically shows a top view of an alkali metal atom gas cell;
FIG. 8a is a schematic view showing a cross-sectional decomposition of an alkali metal atom in the alkali metal atom cell of the present embodiment;
FIG. 8b schematically illustrates a top view of the decomposition of alkali metal atoms within the alkali metal atom gas chamber of the present embodiment;
FIG. 9 is an electron microscopic view schematically showing the inner wall of the V-shaped microchannel.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
FIG. 1 schematically shows a method for manufacturing an alkali metal atom gas cell provided by the invention, comprising the following steps: providing a silicon wafer; growing hard mask layers on the upper surface and the lower surface of the silicon chip; processing each layer of hard mask layer respectively through photoetching and etching processes to form a first window group and a second window group, wherein the first window group is two first windows corresponding to the first region of the silicon wafer in the axial direction, and the second window group is two second windows corresponding to the second region of the silicon wafer in the axial direction; opening silicon wafers between two first windows in the first window group to form a first cavity, and opening silicon wafers between two second windows in the second window group to form a second cavity; forming a V-shaped micro-channel with a rough inner wall surface on the upper surface of the silicon wafer between the first chamber and the second chamber by adopting a laser etching process, so that the first chamber is communicated with the second chamber; removing the hard mask layer; placing an alkali metal azide in the first chamber; and hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet.
In the embodiment of the invention, the method of growing the hard mask layer, then carrying out laser etching and then removing the hard mask layer is adopted, so that the problem that the surface finish degree of the silicon wafer is influenced by solid residues attached to the surface of the area near the V-shaped micro flow channel by laser etching is solved, and the requirement that the surface finish degree of the silicon wafer can meet the sealing connection with the glass sheet is ensured.
In the embodiment of the invention, the V-shaped micro-channel with the rough inner surface is formed between the first chamber and the second chamber in a laser etching mode, and the rough structure on the inner surface of the V-shaped micro-channel is used for adsorbing solid particles generated by laser explosion, so that the effect of filtering residue particles is achieved.
According to the embodiment of the invention, the step of growing the hard mask layer on the upper surface and the lower surface of the silicon chip comprises the steps of growing a first silicon oxide layer and a second silicon oxide layer on the upper surface and the lower surface of the silicon chip respectively, then growing a first silicon nitride layer on the upper surface of the first silicon oxide layer, and growing a second silicon nitride layer on the lower surface of the second silicon oxide layer.
FIG. 2 is a schematic diagram showing the cross-sectional structure of a silicon wafer for forming a hard mask layer. As shown in fig. 2, a first silicon oxide layer 2 is disposed on the upper surface of a silicon wafer 1, a second silicon oxide layer 3 is disposed on the lower surface of the silicon wafer, a first silicon nitride layer 4 is disposed on the upper surface of the first silicon oxide layer 2, and a second silicon nitride layer 5 is disposed on the lower surface of the second silicon oxide layer 3.
In the embodiment of the invention, the silicon oxide and the silicon nitride are grown as the hard mask layer, so that the problem that the surface smoothness of the silicon wafer is influenced by the solid residues attached to the surface of the negative electrode area of the V-shaped micro-channel in the subsequent process of forming the V-shaped micro-channel by laser etching can be effectively solved.
Fig. 3 schematically shows a cross-sectional structure of the silicon wafer after the first window group and the second window group are formed. As shown in fig. 3, the first window groups are two first windows 6 corresponding to each other in the axial direction of the first region of the silicon wafer 1, and the second window groups are two second windows 7 corresponding to each other in the axial direction of the second region of the silicon wafer 1.
In the embodiment of the present invention, the first window and the second window include but are not limited to a square, and the side length of the first window is smaller than the side length of the second window.
Fig. 4a schematically shows a cross-sectional structure of the silicon wafer after the first and second chambers are formed, and fig. 4b schematically shows a top view of the silicon wafer after the first and second chambers are formed. As shown in fig. 4a and 4b, the silicon wafer between two first windows in the first window group is opened to form a first chamber 8, and the silicon wafer between two second windows in the second window group is opened to form a second chamber 9.
According to the embodiment of the invention, the silicon wafer between the two first windows in the first window group is punched to form the first cavity, the silicon wafer between the two second windows in the second window group is punched to form the second cavity, the method comprises the steps of punching the silicon wafer between the two first windows in the first window group to form the first cavity by adopting any one of a wet etching process, deep reactive ion etching and sand blasting punching, and the silicon wafer between the two second windows in the second window group is punched to form the second cavity.
According to the embodiment of the invention, the silicon wafer between two first windows in the first window group is punched through to form a first chamber, and the silicon wafer between two second windows in the second window group is punched through to form a second chamber, wherein the silicon wafer between the two first windows in the first window group is etched by adopting a potassium hydroxide or tetramethylammonium hydroxide wet method to form the first chamber, and the silicon wafer between the two second windows in the second window group is etched by adopting the potassium hydroxide or tetramethylammonium hydroxide wet method to form the second chamber.
FIG. 5a is a schematic diagram showing the cross-sectional structure of a silicon wafer after the formation of V-shaped microchannels, and FIG. 5b is a schematic diagram showing the top view of the structure of a silicon wafer after the formation of V-shaped microchannels. As shown in fig. 5a and 5b, the V-shaped microchannel 10 formed between the first chamber 8 and the second chamber 9 has an uneven surface on the inner wall surface, and the electron microscopic image thereof is shown in fig. 9.
In the embodiment of the invention, the V-shaped micro-channel is utilized to ensure that the gas carrying the solid particles can not pass through the V-shaped micro-channel along a straight line, the particles impact the inner wall of the V-shaped micro-channel and the inner wall of the first chamber, and meanwhile, the surface of the inner wall of the V-shaped micro-channel is rough and uneven, thereby playing a role in isolating and filtering the particles.
FIG. 6 is a schematic cross-sectional view of a silicon wafer after the hard mask layer is removed. The silicon wafer 1 is divided into: the device comprises a first chamber 8, a second chamber 9 and a silicon wafer between the first chamber 8 and the second chamber 9, wherein a V-shaped micro-channel 10 is arranged on the silicon wafer between the first chamber 8 and the second chamber 9.
According to the embodiment of the invention, the step of removing the hard mask layer comprises the step of removing the hard mask layer by adopting a wet etching method, wherein the wet etching method comprises a dilute phosphoric acid wet etching method and a buffered oxide etching solution wet etching method.
According to the embodiment of the invention, the step of hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet comprises the step of hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet by adopting an anodic bonding process.
As another aspect of the invention, the invention also provides an alkali metal atom gas chamber, which comprises the alkali metal atom gas chamber manufactured by the method.
Fig. 7a schematically shows a schematic cross-sectional structure of an alkali metal atom gas cell, and fig. 7b schematically shows a top view of the alkali metal atom gas cell. As shown in fig. 7a and 7b, the alkali metal atom air chamber includes a double-chamber structure formed by sealing two glass sheets 11 and a silicon wafer 1 with double-hole channels, and includes a first chamber 8 and a second chamber 9, wherein a V-shaped micro channel 10 is disposed on the silicon wafer between the first chamber 8 and the second chamber 9, and an alkali metal azide 12 is disposed in the first chamber.
According to the embodiment of the invention, the depth of the V-shaped micro-channel is less than the thickness of the silicon chip.
According to the embodiment of the present invention, the inner wall of the V-shaped micro flow channel is rough.
Fig. 8a schematically shows a cross-sectional view of the decomposition of the alkali metal atoms in the alkali metal atom cell of the present embodiment, and fig. 8b schematically shows a top view of the decomposition of the alkali metal atoms in the alkali metal atom cell of the present embodiment. As shown in fig. 8a and 8b, since the solid particles 13 generated by laser explosion in the first chamber 8 are blocked by the V-shaped microchannel 10 and cannot enter the second chamber 9, the purity of the alkali metal atom and the buffer gas combination 14 in the second chamber 9 is ensured, thereby improving the stability and accuracy of the atomic clock frequency.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A method for making an alkali metal atom gas cell, comprising:
providing a silicon wafer;
growing hard mask layers on the upper surface and the lower surface of the silicon chip;
respectively processing the hard mask layer on the upper surface of the silicon chip and the hard mask layer on the lower surface of the silicon chip by photoetching and etching processes to form a first window group and a second window group, wherein the first window group is two first windows corresponding to the first region of the silicon chip in the axial direction, and the second window group is two second windows corresponding to the second region of the silicon chip in the axial direction;
opening the silicon wafer between two first windows in the first window group to form a first cavity, and opening the silicon wafer between two second windows in the second window group to form a second cavity;
forming a V-shaped micro-channel with a rough inner wall surface on the upper surface of the silicon wafer between the first chamber and the second chamber by adopting a laser etching process, so that the first chamber is communicated with the second chamber, wherein the depth of the V-shaped micro-channel is less than the thickness of the silicon wafer;
removing the hard mask layer;
placing an alkali metal azide in the first chamber;
and hermetically connecting the upper surface and the lower surface of the silicon wafer with the glass sheet.
2. The method of claim 1, wherein the growing of the hard mask layer on both the upper surface and the lower surface of the silicon chip comprises growing a first silicon oxide layer and a second silicon oxide layer on the upper surface and the lower surface of the silicon chip respectively, and then growing a first silicon nitride layer on the upper surface of the first silicon oxide layer and a second silicon nitride layer on the lower surface of the second silicon oxide layer.
3. The method of claim 1, wherein the opening the silicon wafer between two first windows in the first window group to form a first chamber and the opening the silicon wafer between two second windows in the second window group to form a second chamber comprises opening the silicon wafer between two first windows in the first window group to form a first chamber and the opening the silicon wafer between two second windows in the second window group to form a second chamber by using any one of a wet etching process, a deep reactive ion etching process, and a sand blasting and drilling process.
4. The method of claim 3, wherein opening the silicon wafer between two first windows in the first window set to form a first chamber and opening the silicon wafer between two second windows in the second window set to form a second chamber comprises wet etching the silicon wafer between two first windows in the first window set to form a first chamber using potassium hydroxide or tetramethylammonium hydroxide, and wet etching the silicon wafer between two second windows in the second window set to form a second chamber using potassium hydroxide or tetramethylammonium hydroxide.
5. The method of claim 1, wherein the removing the hard mask layer comprises removing the hard mask layer by a wet etching method, wherein the wet etching method comprises a dilute phosphoric acid wet etching method and a buffered oxide etching solution wet etching method.
6. The method of claim 1, wherein hermetically connecting both the top and bottom surfaces of the silicon wafer to the glass sheet comprises hermetically connecting both the top and bottom surfaces of the silicon wafer to the glass sheet using an anodic bonding process.
7. An alkali metal atom gas cell comprising the alkali metal atom gas cell produced by the method according to any one of claims 1 to 6.
8. The alkali metal atom gas cell of claim 7, comprising a double-chamber structure formed by sealing two glass sheets and a silicon wafer with double channels, wherein the double-chamber structure comprises a first chamber and a second chamber, wherein a V-shaped micro channel is arranged on the silicon sheet between the first chamber and the second chamber, and an alkali metal azide is arranged in the first chamber.
9. The alkali metal atom gas cell according to claim 8, wherein the inner wall of the V-shaped microchannels is rough.
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CN114136377A (en) * 2021-12-02 2022-03-04 中国航空工业集团公司北京长城计量测试技术研究所 Alkali metal atom air chamber and manufacturing method thereof
CN114477074A (en) * 2021-12-22 2022-05-13 北京自动化控制设备研究所 Wafer-level atomic gas chamber processing method and device based on MEMS technology

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