Preparation method and system for sapphire coating atomic gas chamber
By forming a sapphire coating on the wall of the atomic gas cell, the shortcomings of sapphire material atomic gas cells in low-frequency signal shielding effect were solved, enabling high-sensitivity electromagnetic signal measurement and promoting the development of quantum precision measurement technology.
Patent Information
- Application Number
- CN202511656463.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-12
- Publication Date
- 2025-12-12
- Estimated Expiration
- 2045-11-12
AI Technical Summary
The atomic gas cells made of existing sapphire materials have difficulty improving the receiving sensitivity due to the shielding effect of low-frequency signals, which limits their application in high-precision electromagnetic signal measurement.
A sapphire coating is formed on the wall of the atomic gas chamber using atomic layer deposition technology. An aluminum oxide film is formed by alternating pulse filling of aluminum source gas and oxide gas, and combined with alkali metal filling, a sapphire-coated atomic gas chamber with high anti-shielding performance is prepared.
It enhances the anti-shielding capability of the alkali metal atom gas cell, improves the precision measurement performance of electromagnetic waves, and enables low-cost, high-performance, high-sensitivity measurement of low-frequency electromagnetic signals.
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Figure CN121109987A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of quantum precision measurement, and in particular to a preparation method and system for a sapphire-coated atomic cell. BACKGROUND
[0002] Precision measurement techniques based on quantum effects are widely used in physical parameter measurement systems such as time, electric field, magnetic field, and gravitational field. Currently, high-precision measurement devices such as atomic clocks, atomic electric field meters, atomic magnetometers, and quantum gravimeters have been successfully developed, greatly promoting the development of technologies in civilian fields. In the field of atomic electric field meters, for example, electromagnetic information is obtained by using external electromagnetic waves to disturb the energy levels of Rydberg atoms. The electric field measurement probe has the characteristics of size independence, high measurement sensitivity, and wide frequency band. In particular, for kHz signal measurement, the probe size can be reduced by 4-5 orders of magnitude compared to conventional antennas, and the sensitivity is expected to break through the thermal noise limit, which is very suitable for small-sized and high-sensitivity submarine communication applications and has great research value. Among them, the alkali metal atomic cell is the core physical device of the quantum precision measurement system. It is filled with alkali metal atomic vapor inside and can realize the preparation of highly excited atoms by laser driving, thereby realizing high-precision measurement of multiple physical parameters such as magnetic field, electric field, optical field, and gravitational field, and supporting research work in the quantum field. In the field of electric field measurement, the atomic cell is the core physical element for electromagnetic sensing. Its packaging shell is usually made of high-boron silicon, quartz, or other materials, and is filled with alkali metal (such as cesium, rubidium) gas. When receiving low-frequency signals such as kHz and MHz, the adsorption effect between the inner wall of the cell and the atoms will have a static shielding effect on the signal, severely limiting the improvement of its receiving sensitivity. Currently, using sapphire material (Al2O3) to prepare the atomic cell is an effective way to solve the shielding effect of low-frequency signals, but due to the limitations of sapphire shell material preparation and packaging process, the atomic cell using sapphire material is still difficult to be widely applied. SUMMARY
[0003] The technical problem to be solved by the present application is to provide a preparation method and system for a sapphire-coated atomic cell.
[0004] To achieve the above-mentioned application purposes, the present application provides a preparation method for a sapphire-coated atomic cell, comprising the following steps: S1. Placing the cleaned atomic cell on the heating base of the reaction chamber, and filling the reaction chamber with displacement gas to discharge the residual gas therein; S2. Filling the reaction chamber with aluminum source gas, and chemically adsorbing on the wall surface of the atomic cell based on atomic layer deposition technology to form a first film layer; S3. Filling the reaction chamber with displacement gas to discharge the residual aluminum source gas therein; S4. Filling the reaction chamber with oxide gas to oxidize the first film layer and convert it into an aluminum oxide film layer; S5. Filling the reaction chamber with replacement gas to discharge residual oxide gas therein; S6. Repeating steps S2 to S5 to form aluminum oxide film layers of a preset number of layers and a preset thickness on the wall surface of the atomic gas chamber to form the atomic gas chamber with a sapphire coating.
[0005] According to one aspect of the present application, further comprising: S7. Taking out the atomic gas chamber and performing alkali metal charging.
[0006] According to one aspect of the present application, in step S1, during the step of placing the cleaned atomic gas chamber on the heating base of the reaction chamber, the working temperature of the heating base is 250-300°C. The gas inlet of the atomic gas chamber is arranged perpendicular to the gas inlet direction of the reaction chamber.
[0007] According to one aspect of the present application, in step S2, during the step of filling the reaction chamber with aluminum source gas, an alternating pulse gas inlet method is used to fill the reaction chamber with aluminum source gas; wherein the alternating pulse gas inlet method used has a pulse gas inlet time of greater than or equal to 10 minutes.
[0008] According to one aspect of the present application, in step S4, during the step of filling the reaction chamber with oxide gas to oxidize the first film layer and convert it into an aluminum oxide film layer, the thickness of the aluminum oxide film layer is 0.1-0.2 nm.
[0009] According to one aspect of the present application, in step S7, during the step of taking out the atomic gas chamber and performing alkali metal charging, comprising: S71. Connecting an alkali metal source and at least one atomic gas chamber to the same gas charging pipeline; S72. Based on the gas charging pipeline, vacuumizing the atomic gas chamber, and placing the atomic gas chamber, the alkali metal source, and at least part of the gas charging pipeline in a heating oven; S73. Opening the sealing structure between the alkali metal source and the gas charging pipeline, and starting the heating oven to perform coating heating according to a preset heating scheme; wherein the preset heating scheme is: increasing the temperature from room temperature to 200°C, taking 1 hour, maintaining 200°C for 2 hours, and decreasing the temperature from 200°C to room temperature, taking 1 hour; S74. After the heating oven completes heating based on the preset heating scheme, removing the heating oven, and taking out the atomic gas chamber from the gas charging pipeline after sealing, completing the alkali metal charging of the atomic gas chamber.
[0010] According to an aspect of the present application, in step S72, the vacuum degree of the vacuuming step is superior to 10 -5 Pa.
[0011] According to an aspect of the present application, the atomic gas chamber is a high borosilicate glass chamber or a quartz material chamber. The aluminum source gas is trimethylaluminum gas. The oxide gas is deionized water vapor. The alkali metal of the alkali metal source is cesium metal or rubidium metal.
[0012] To achieve the above-mentioned purposes, the present application provides a system for the preparation method of the sapphire coating atomic gas chamber, comprising a coating unit. The coating unit comprises a reaction chamber with a heating base, a first pipeline connected to the reaction chamber, an aluminum source device, an oxide source device, and a displacement gas source device connected to the first pipeline. The reaction chamber comprises a regular and hollow reaction chamber body, a first hole plate and a second hole plate respectively arranged at opposite ends of the reaction chamber body. One end of the first pipeline is connected to the position where the first hole plate is arranged on the reaction chamber body. The first hole plate has a plurality of first through holes penetrating through the body, and the diameters of some of the first through holes on the first hole plate are different. The second hole plate has a plurality of second through holes penetrating through the body, and the diameters of some of the second through holes on the second hole plate are different.
[0013] According to an aspect of the present application, it further comprises an alkali metal charging unit. The alkali metal charging unit comprises a gas charging pipeline, an alkali metal source, a heating oven, and a vacuumizing unit. The gas charging pipeline is partially arranged in the heating oven. The alkali metal source is connected to the part of the gas charging pipeline in the heating oven. The vacuumizing unit is connected to the end of the gas charging pipeline outside the heating oven. The heating oven comprises a hollow upper cover and a bottom plate. The upper cover and the bottom plate are arranged openably and closably.
[0014] According to an aspect of the present application, the present application can effectively enhance the shielding resistance of the alkali metal atomic gas chamber and improve the performance of the atomic gas chamber in electromagnetic wave precision measurement.
[0015] According to one aspect of the present invention, this approach utilizes an ALD atomic gas chamber coating method based on heterogeneous cavity flow field homogenization technology. It employs porous baffles to precisely control the precursor gas flow rate and, by setting the operating temperature of the heating platform to 250℃~300℃, significantly improves the sapphire coating efficiency on the inner wall of the atomic gas chamber. This supports the fabrication of low-cost, high-performance shielded atomic gas chambers and high-sensitivity measurement of low-frequency electromagnetic signals, thus promoting the leapfrog development of quantum precision measurement technologies such as magnetic field measurement, electric field measurement, and gravitational field measurement.
[0016] According to one aspect of the present invention, the aperture of the porous baffle is set as an array of circular holes with unequal radii, which can precisely control the flow rate of the precursor gas, allowing the gas to enter the narrow inlet, non-planar atomic gas chamber with extremely high efficiency to complete the coating process.
[0017] According to one aspect of the present invention, a specially designed non-uniform pore array porous baffle is used to precisely control the flow rate of the precursor gas, thereby improving the chemical adsorption capacity of the inner wall of the atomic gas chamber and the film formation efficiency of the medium.
[0018] According to one aspect of the present invention, the sapphire-coated atomic gas cell prepared by this approach has the advantages of low cost, high anti-shielding performance, and high sensitivity measurement of low-frequency electromagnetic signals. Attached Figure Description
[0019] Figure 1 This is a flowchart illustrating the steps of a method for preparing an atomic gas chamber for sapphire coating according to one embodiment of the present invention. Figure 2 This is a structural block diagram of a coating unit according to one embodiment of the present invention; Figure 3 This is a structural diagram of the first perforated plate according to one embodiment of the present invention; Figure 4 This is a simulation result diagram of the first perforated plate according to one embodiment of the present invention, wherein, Figure 4 (a) is a simulation result of the gas pressure in the first through hole 112a of the first perforated plate 112. Figure 4 (b) is a simulation result of the gas flow velocity in the first through hole 112a of the first perforated plate 112; Figure 5 This is a combined configuration diagram of the first perforated plate according to one embodiment of the present invention; Figure 6 This is a structural diagram of a through-hole structure according to one embodiment of the present invention; Figure 7 This is a cross-sectional view of a through-hole structure according to one embodiment of the present invention; Figure 8 This is a structural diagram of a first annular elastic member and a second annular elastic member assembly according to one embodiment of the present invention; Figure 9 This is a structural diagram of a combination of a first annular elastic element and a second annular elastic element according to another embodiment of the present invention; Figure 10 This is a structural diagram of the first annular elastic element according to one embodiment of the present invention; Figure 11 This is a structural diagram of the second annular elastic member according to one embodiment of the present invention; Figure 12 This is a structural diagram of the second perforated plate according to one embodiment of the present invention; Figure 13 This is a structural diagram of an alkali metal filling unit according to one embodiment of the present invention.
[0020] In the attached diagram, 1-coating unit, 11-reaction chamber, 12-first pipeline, 13-aluminum source device, 14-oxide source device, 15-displacement gas source device, 111-reaction chamber body, 112-first orifice plate, 113-second orifice plate, 121-horizontal pipeline section, 122-vertical pipeline section, 112a-first through hole, 1121-orifice plate body, 1122-through hole structure, 1121a-structure mounting position, 1122a-outer cylinder of structure, 1122b-first annular elastic element, 1122c-second annular elastic element, 1122d-aperture adjustment element, 1122b1-first connecting ring, 1122b2-first elastic plate, 1122c1-second connecting ring, 1122c2-second elastic plate, 113a - Second through hole, 2- Alkali metal filling unit, 21- Gas filling pipe, 22- Alkali metal source, 23- Heating oven, 231- Top cover, 232- Bottom plate. Detailed Implementation
[0021] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the accompanying drawings used in the embodiments will be briefly described below. Obviously, the drawings described below are merely some embodiments of the present invention, and those skilled in the art can obtain other drawings based on these drawings without any creative effort.
[0022] In describing embodiments of the present invention, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer" express orientations or positional relationships based on the orientations or positional relationships shown in the relevant drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, the above terms should not be construed as limitations on the present invention.
[0023] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. The embodiments cannot be described in detail here, but the embodiments of the present invention are not limited to the following embodiments.
[0024] like Figure 1 As shown, according to one embodiment of the present invention, a method for preparing an atomic gas chamber for sapphire coating is provided. The present invention utilizes atomic layer deposition (ALD) technology to prepare a sapphire material vapor precursor, which is injected into the atomic gas chamber via alternating pulses. By controlling the flow rate of each vapor precursor, an ordered, surface-self-saturated chemical reaction occurs between the sapphire material vapor precursor and the wall (mainly the inner wall) of the atomic gas chamber. Heating during the reaction process ensures stable adhesion of the sapphire material. Then, alkali metal atoms are filled using a high-vacuum system. After quantitative filling, the chamber is encapsulated, ultimately completing the preparation of the sapphire coating atomic gas chamber. Specifically, it includes the following steps: S1. Place the cleaned atomic gas chamber on the heating base of the reaction chamber, and fill the reaction chamber with replacement gas to remove the residual gas; S2. Aluminum source gas is introduced into the reaction chamber, and chemical adsorption occurs on the wall of the atomic gas chamber based on atomic layer deposition technology to form the first film layer; S3. Purge the reaction chamber with replacement gas to remove any residual aluminum source gas. S4. Introduce oxide gas into the reaction chamber to oxidize the first film layer and transform it into an aluminum oxide film layer; S5. Purge the reaction chamber with replacement gas to remove residual oxide gases; S6. Repeat steps S2 to S5 to form an aluminum oxide film layer with a preset number of layers and a preset thickness on the wall surface of the atomic gas chamber, so as to form an atomic gas chamber with a sapphire coating.
[0025] According to one embodiment of the present invention, a method for preparing an atomic gas chamber for sapphire coating further includes: S7. Remove the atomic gas cell and fill it with alkali metal.
[0026] According to one embodiment of the present invention, in step S1, where the cleaned atomic gas chamber is placed on the heating platform of the reaction chamber, the atomic gas chamber to be coated is cleaned with solutions such as acetone, methanol, and deionized water to ensure that its surface reaches a preset cleanliness level. After being dried and cleaned by blowing nitrogen gas through the walls (especially the inner walls), it is placed on the heating platform of the reaction chamber. In this embodiment, the internal space of the reaction chamber is a pre-cleaned ultra-clean room to ensure that the walls of the atomic gas chamber to be coated remain clean during the coating process.
[0027] In this embodiment, the atomic gas chamber can be a glass structure with an inlet pipe, and its material is usually high borosilicate or quartz, used to fill alkali metal atomic gas after the film coating is completed.
[0028] Furthermore, in step S1, the step of placing the cleaned atomic gas chamber on the heating platform of the reaction chamber, the working temperature of the heating platform is set to 250℃~300℃; the heating effect of the heating platform effectively ensures the stable and reliable adhesion of the sapphire material during the coating process, making the finished product of the present invention more effective.
[0029] In this embodiment, when the atomic gas chamber is installed on the heating base, the orientation of the gas inlet of the atomic gas chamber is perpendicular to the orientation of the gas inlet of the reaction chamber. This arrangement ensures that the gas inlet direction of the atomic gas chamber is perpendicular to the gas inlet direction of the reaction chamber, effectively preventing direct scouring of the atomic gas chamber by the gas entering from the reaction chamber. This allows the gas flow to be evenly distributed into the atomic gas chamber through dispersion, achieving uniform distribution on the surface of the atomic gas chamber. Furthermore, this method allows for a faster replacement rate of the pre-existing gas in the reaction chamber, enabling complete replacement of the pre-existing gas before full filling of the atomic gas chamber, which is more beneficial in minimizing the influence of the pre-existing gas.
[0030] Furthermore, in step S1, the step of filling the reaction chamber with replacement gas to remove residual gas can use high-purity nitrogen gas. The gas flow rate of the replacement gas is controlled at 300 sccm for about 30 seconds, thereby completely removing the residual gas from the reaction chamber and filling the entire reaction chamber with replacement gas. This also effectively avoids the influence of residual gas on the subsequent coating process and ensures the surface quality of the coated film.
[0031] According to one embodiment of the present invention, in step S2, the aluminum source gas is introduced into the reaction chamber using an alternating pulse gas inlet method; wherein the aluminum source is trimethylaluminum (TMA, Al(CH3)3). In this embodiment, a replacement gas is introduced simultaneously with the aluminum source gas, thereby allowing the trimethylaluminum to be introduced into the reaction chamber under the action of the replacement gas. Consequently, the aluminum source gas can adhere to the wall surface of the atomic gas chamber for chemical adsorption, thereby forming a single-sided first film layer (i.e., a trimethylaluminum film layer). In this embodiment, to facilitate the sufficient introduction of the aluminum source gas into the atomic gas chamber, the inlet of the atomic gas chamber can be positioned directly opposite the inlet of the aluminum source gas to achieve accurate filling of the atomic gas chamber.
[0032] In this embodiment, in step S2, the alternating pulse gas injection method used in the step of filling the reaction chamber with aluminum source gas has an injection time of 10 minutes or more for each pulse. This setting effectively ensures sufficient reaction between the reactant gas and the inner wall of the atomic gas chamber, resulting in a denser and more stable film layer, which is more beneficial for improving the performance of the atomic gas chamber.
[0033] According to one embodiment of the present invention, in step S3, in the step of introducing replacement gas into the reaction chamber to remove the residual aluminum source gas therein, after the quantitative supply of aluminum source gas into the reaction chamber is completed, the supply valve of aluminum source gas is closed while the continuous input of replacement gas is maintained, thereby achieving the removal of residual aluminum source gas in the reaction chamber under the action of replacement gas.
[0034] According to one embodiment of the present invention, in step S4, where an oxide gas is introduced into the reaction chamber to oxidize the first film layer and transform it into an alumina film layer, the thickness of the alumina film layer is 0.1 nm to 0.2 nm. In this embodiment, the oxide gas can be deionized water vapor (H2O), which is introduced simultaneously with a replacement gas to be carried into the reaction chamber under the action of the replacement gas. This allows the oxide gas to fully form an oxidizing atmosphere around the first film layer, thereby transforming the first film layer into an alumina film layer under the action of the oxide gas.
[0035] According to one embodiment of the present invention, in step S5, in the step of introducing displacement gas into the reaction chamber to discharge the residual oxide gas therein, after the quantitative delivery of oxide gas into the reaction chamber is completed, the oxide gas delivery valve is closed while the displacement gas is still continuously input, thereby achieving the discharge of residual oxide gas in the reaction chamber under the action of displacement gas.
[0036] According to one embodiment of the present invention, in step S6, steps S2 to S5 are repeated to form an alumina film layer of a predetermined number and predetermined thickness on the wall surface of the atomic gas chamber. The predetermined number of layers on the wall surface of the atomic gas chamber can be determined according to actual performance requirements, and will not be elaborated further here. Similarly, the predetermined thickness of each alumina film layer is also determined based on actual performance requirements. A thicker predetermined thickness simply requires a corresponding increase in the coating time. Through the above settings, each alumina film layer can achieve its actual coating thickness determined by the corresponding coating time. Therefore, this solution flexibly controls the corresponding coating time according to different actual needs to achieve the coating of any number of alumina film layers, exhibiting excellent adaptability and scalability.
[0037] According to one embodiment of the present invention, step S7, the step of removing the atomic gas cell and filling it with alkali metals, includes: S71. Connect an alkali metal source and at least one atomic gas chamber to the same gas filling pipe; wherein the alkali metal source is a glass structure with an outlet pipe, and the corresponding alkali metal is pre-encapsulated therein, and the alkali metal in the alkali metal source is cesium metal (Cs) or rubidium metal (Rb). In this embodiment, a glass cylindrical tube is used to weld the sealed ends of the gas filling pipe and the alkali metal source together, wherein a movable iron block can be pre-arranged in the glass cylindrical tube, and then the iron block can be lifted by a magnet outside the glass cylindrical tube and the magnet can be detached so that the iron block falls freely in the glass cylindrical tube to break the seal of the alkali metal source, thereby achieving communication between the alkali metal source and the gas filling pipe.
[0038] Correspondingly, the atomic gas chambers are also connected to the gas filling pipe by welding; the atomic gas chambers can be arranged along the length of the gas filling pipe, so that the connection of different numbers of atomic gas chambers can be achieved based on the length of the gas filling pipe.
[0039] S72. A vacuum is evacuated from the atomic gas chamber via a gas filling pipe, and the atomic gas chamber, alkali metal source, and at least a portion of the gas filling pipe are placed in a heating oven; in this embodiment, a vacuum device is used to extract residual gas from the gas filling pipe and the atomic gas chamber, thereby achieving a vacuum level better than 10 in the connected gas filling pipe and atomic gas chamber. -5 Pa.
[0040] S73. Open the sealing structure between the alkali metal source and the gas filling pipe, and start the heating oven to perform coating heating according to the preset heating scheme. In this embodiment, the sealing structure is the closed port of the alkali metal source. Therefore, based on the aforementioned movable iron block between the alkali metal source and the gas filling pipe, the sealing structure can be opened by the action of a magnet. In this embodiment, the heating sequence of the preset heating scheme is as follows: heating from room temperature to 200°C for 1 hour; then maintaining the temperature at 200°C for 2 hours; and finally cooling from 200°C to room temperature for 1 hour. In this embodiment, the heating and cooling processes can be implemented using linear processes, thereby achieving a balanced filling process, which is more beneficial to ensuring the filling effect.
[0041] S74. After the heating oven completes heating based on the preset heating scheme, remove the heating oven, seal the atomic gas chamber and remove it from the gas filling pipe to complete the alkali metal filling of the atomic gas chamber.
[0042] like Figure 2As shown, according to one embodiment of the present invention, the present invention provides a system for the aforementioned preparation method of an atomic gas chamber for sapphire coating, comprising: a coating unit 1; wherein, the coating unit 1 is used to form a sapphire coating on the wall surface of the atomic gas chamber; specifically, the coating unit 1 includes: a reaction chamber 11 having a heating base, a first pipeline 12 connected to the reaction chamber 11, an aluminum source device 13, an oxide source device 14, and a displacement gas source device 15 connected to the first pipeline 12; in this embodiment, the reaction chamber 11 includes: a regular and hollow reaction chamber body 111, and a first perforated plate 112 and a second perforated plate 113 respectively provided at opposite ends of the reaction chamber body 111; wherein, the reaction chamber body 111 can be configured as a hollow regular box, and its entirety can be configured as a stainless steel box to ensure sufficient corrosion resistance and effectively avoid the influence on the coating process. In addition, to facilitate the arrangement and installation of each structure, an openable and closable door can be provided on the reaction chamber body 111, thereby facilitating the installation and disassembly of the atomic gas chamber.
[0043] In this embodiment, the aluminum source device 13 is loaded with an aluminum source (i.e., trimethylaluminum (TMA), etc.); the oxide source device 14 is loaded with deionized water vapor; and the displacement gas source device 15 is loaded with high-purity nitrogen gas.
[0044] In this embodiment, perforated plate mounting positions for arranging the first perforated plate 112 and the second perforated plate 113 are provided on the walls at opposite ends of the reaction chamber body 111. The first perforated plate 112 and the second perforated plate 113 are detachably or fixedly connected to the perforated plate mounting positions, and the connection points can be further sealed with seals to ensure airtightness of the mounting positions. Furthermore, the perforated plate mounting positions at opposite ends of the reaction chamber body 111 are coaxially arranged, thereby enabling the first perforated plate 112 and the second perforated plate 113 to be arranged coaxially.
[0045] In this embodiment, one end of the first pipeline 12 is connected to the position where the first orifice plate 112 is set on the reaction chamber body 111; thereby, the flow rate of the transported gas can be controlled through the first orifice plate 112.
[0046] In this embodiment, the first pipe 12 includes a horizontal pipe section 121 and a vertical pipe section 122. The horizontal pipe section 121 and the vertical pipe section 122 are connected at their ends perpendicular to each other. The end of the horizontal pipe section 121 away from the vertical pipe section 122 is connected to the first orifice plate 112. The end of the vertical pipe section 122 away from the horizontal pipe section 121 is closed, and the vertical pipe section 122 extends downwards. In this embodiment, the connection between the horizontal pipe section 121 and the vertical pipe section 122 is made with a rounded transition to ensure a smooth transition in airflow direction, which is beneficial to improving the airflow delivery stability of the present invention. In this embodiment, the first pipe 12 is a circular cross-section pipe and is made of stainless steel, thereby ensuring sufficient material stability to guarantee the plating effect of the present invention.
[0047] Furthermore, to ensure the flexibility of on / off control between the first pipeline 12 and the reaction chamber 11, a high-vacuum connection valve can be installed on the horizontal pipeline section 121 to achieve on / off control of the first pipeline 12.
[0048] In this embodiment, the aluminum source device 13, oxide source device 14, and displacement gas source device 15 are respectively connected to the vertical pipeline section 122. The aluminum source device 13, oxide source device 14, and displacement gas source device 15 are arranged sequentially from top to bottom. High-vacuum valves are installed at the connection points of the aluminum source device 13, oxide source device 14, and displacement gas source device 15 to the vertical pipeline section 122 to achieve individual control of each gas source. Furthermore, the output gas flow rate can be quantitatively controlled based on the opening degree of the high-vacuum valves. In this embodiment, the high-vacuum valves used can be electromagnetically controlled valves, thereby enabling more precise and sensitive control, making the film deposition process of this invention more accurate, and thus resulting in better film quality and precision.
[0049] like Figure 3As shown, in this embodiment, the first perforated plate 112 has a plurality of first through holes 112a penetrating its body, and the diameters of some of the first through holes 112a on the first perforated plate 112 are different; wherein, the first perforated plate 112 can be configured as a circular plate, and the diameters of the first through holes 112a in the first perforated plate 112 can be configured as three types. Specifically, the largest diameter first through hole 112a can be configured as one, and it is arranged at the center position of the first perforated plate 112; the second diameter first through holes 112a can be configured as a plurality of them, and they can be arranged at equal intervals around the largest diameter first through hole 112a along the circumference of the first perforated plate 112 to realize the second diameter The first through hole 112a surrounds the first through hole 112a with the largest central diameter; multiple first through holes 112a with the smallest diameter can be provided, and they can be arranged at equal intervals around the first through hole 112a with the second diameter along the circumference of the first orifice plate 112, so as to realize the first through hole 112a with the smallest diameter surrounding the first through hole 112a with the second diameter; furthermore, since the opening areas of the three types of first through holes 112a with different diameters are different, the number of first through holes 112a with different diameters can be gradually increased from the center to the edge of the first orifice plate 112, so as to realize the flexible control of gas flow by different first through holes 112a. Of course, the aperture of the first through hole 112a in the first orifice plate 112 can be set to four, five or more types to achieve the distribution of first through holes 112a of different sizes. Moreover, the first through holes 112a are arranged according to the law of decreasing diameter and increasing number in the direction from the center to the outer edge of the first orifice plate 112, so that the first orifice plate 112 of this solution has excellent flow control effect.
[0050] In this embodiment, the first through holes 112a of the second aperture are arranged in an equally spaced annular array using a first ring; the first through holes 112a of the smallest aperture are arranged in an equally spaced annular array using a second ring; wherein, the interval between the center of the first ring and the center of the first through hole 112a of the largest aperture is the first interval, and the interval between the first ring and the second ring is the second interval, and the first interval and the second interval are either equal or different. In this embodiment, the number of first through holes 112a of the second aperture can be 4, 6, 8 or more, and the number of first through holes 112a of the smallest aperture can be 10, 12, 14, 16 or more.
[0051] In this embodiment, the diameter of the first through hole 112a is at least 1 mm.
[0052] In this embodiment, the distribution of the first perforated plate 112 and the first through holes 112a thereon is obtained based on the following steps; wherein, taking the first through holes 112a with three different diameters as an example, the specific steps include: Perform fluid dynamics modeling and simulation: A three-dimensional model of the first perforated plate 112 is constructed, wherein two concentric rings are constructed on the first perforated plate 112: a first ring for arranging the first through hole 112a of the second diameter and a second ring for arranging the first through hole 112a of the smallest diameter. Further, first through holes 112a are respectively set at the center of the first perforated plate 112, along the circumference of the first ring, and along the circumference of the second ring. Specifically, there is one first through hole 112a at the center, eight first through holes 112a on the first ring, and sixteen first through holes 112a on the third ring. The initial diameter of each first through hole 112a is set to 1 mm.
[0053] Perform gas flow analysis: An atomic gas chamber is placed in the same direction as the first orifice plate 112, with the gas inlet of the atomic gas chamber facing the first orifice plate 112 and 100mm away from it. The gas flow rate at the gas inlet is observed.
[0054] Optimize the diameter of the first through hole 112a, the diameter of the first annulus, and the diameter of the second annulus: To ensure that the diameter of each first through hole 112a remains unchanged, the diameters of the first ring and the second ring are sequentially combined within the range of 1mm to 5mm. The gas flow rate at the inlet of the atomic gas chamber is measured. After the maximum value is reached, the diameters of the first ring and the second ring are determined.
[0055] Keeping the diameters of the first and second rings unchanged, the diameters of the first through hole 112a located at the center of the first orifice plate 112, the first through hole 112a on the first ring, and the first through hole 112a on the second ring are sequentially combined and traversed within the range of 1mm to 5mm. The gas flow rate at the inlet of the atomic gas chamber is measured. After reaching the maximum value, the diameter of the first through hole 112a is determined.
[0056] The simulation results after completing the gas flow analysis are as follows: Figure 4 As shown.
[0057] The first orifice plate 112 was prepared and tested: The first orifice plate 112 is prepared and installed at the corresponding position in the reaction chamber 11 for nitrogen flow test. The effect is judged by the flow meter. If the flow rate does not reach the preset condition, the above arrangement is repeated to optimize the setting position and distribution pattern of the first through hole 112a on it, so as to further optimize the first orifice plate 112.
[0058] like Figure 5As shown, in this embodiment, to facilitate the experimental preparation of the first perforated plate 112, the first perforated plate 112 is configured as a combined structure to improve efficiency during repeated experiments. Specifically, the first perforated plate 112 includes: a perforated plate body 1121 and multiple through-hole structural components 1122 with adjustable apertures; wherein, the perforated plate body 1121 is provided with multiple structural component mounting positions 1121a penetrating its body, and the distribution of the structural component mounting positions 1121a is set based on the distribution pattern determined during the modeling and simulation process; wherein the dimensions of each structural component mounting position 1121a are consistent to facilitate the processing consistency and reusability of the perforated plate body 1121, and to meet the requirements of repeated use under the same hole position distribution but different hole diameter distribution, effectively improving the ease of use of this solution.
[0059] In this embodiment, the perforated plate body 1121 may be made of stainless steel.
[0060] Furthermore, the through-hole structure 1122 has a hollow portion to form a first through-hole 112a, and the radial dimension of this hollow portion is adjustable. This allows for precise adjustment of the output port diameter of the first through-hole 112a, enabling fine-tuning of any discrepancies between the actual and simulated effects, and achieving precise control of the precursor gas flow rate and stable, uniform distribution of the precursor gas input. Combined with... Figure 6 and Figure 7As shown, in this embodiment, the through-hole structure 1122 includes: an outer cylindrical body 1122a, a first annular elastic element 1122b, a second annular elastic element 1122c, and a bore diameter adjustment element 1122d; wherein, the outer cylindrical body 1122a is generally a hollow cylindrical body with openings at both ends, and along the radial direction from the outside to the inside of the through-hole structure 1122, the outer cylindrical body 1122a, the first annular elastic element 1122b, and the second annular elastic element 1122c are sequentially nested together; wherein, the end of the outer cylindrical body 1122a facing the first pipe 12 is defined as the inlet end, and the end facing away from the first pipe 12 is defined as the outlet end, and thus... The first end of the first annular elastic member 1122b is coaxially fixed to the inner side of the inlet end of the outer cylinder 1122a of the structural member. The first end of the second annular elastic member 1122c is coaxially fixed to the inner side of the first end of the first annular elastic member 1122b. Furthermore, the second end of the first annular elastic member 1122b and the outlet end of the outer cylinder 1122a of the structural member are radially spaced. Thus, the aperture adjustment member 1122d can be disposed between the second end of the first annular elastic member 1122b and the outlet end of the outer cylinder 1122a of the structural member. In this embodiment, the aperture adjustment component 1122d is an annular structure, and the outer cylinder 1122a of the structural component and the aperture adjustment component 1122d are connected by threads. Therefore, based on the abutment between the inner side of the aperture adjustment component 1122d and the outer side of the first annular elastic component 1122b, the position of the aperture adjustment component 1122d can be adjusted along the direction from the outlet end to the inlet end of the outer cylinder 1122a of the structural component. This allows the second end of the first annular elastic component 1122b to press radially inward against the second end of the second annular elastic component 1122c, thereby reducing the outlet diameter of the first through hole 112a formed by the combination of the second ends of the first annular elastic component 1122b and the second ends of the second annular elastic component 1122c. Conversely, by rotating the aperture adjustment component 1122d to move in the opposite direction, the outlet diameter of the first through hole 112a can be increased. Based on this control method, the outlet diameter of the first through hole 112a can be controlled more flexibly and accurately to achieve precise flow control and match the simulation effect.
[0061] In this embodiment, the outer surface of the outer cylinder 1122a can be either cylindrical or conical, while the inner surface is cylindrical to facilitate installation of the various structures. When the outer surface of the outer cylinder 1122a is a straight cylinder, it is connected to the mounting position 1121a using a matching connection structure (such as a thread). When the outer surface of the outer cylinder 1122a is a conical cylinder, the inner surface of the mounting position 1121a is also conical. This allows for self-positioning installation based on the matching of the outer surface of the outer cylinder 1122a and the inner surface of the mounting position 1121a, facilitating accurate installation of the through-hole structure 1122, ensuring airtightness of the installation position, and facilitating disassembly during replacement.
[0062] In this embodiment, when the outer surface of the outer cylinder 1122a of the structural component is set as a conical cylinder, the inlet end of the outer cylinder 1122a of the structural component is the large diameter end. Thus, the installation direction of the through hole structural component 1122 can be determined, making it more stable in use and effectively preventing it from coming off due to airflow.
[0063] In this embodiment, at the inlet end of the outer cylinder 1122a of the structural component, to facilitate the installation of the first annular elastic element 1122b, an annular connector for installing the end of the first annular elastic element 1122b can be provided on the inner side of the inlet end. The annular connector and the first annular elastic element 1122b can be coaxially connected by nesting installation, and can be fixed at the connection point by welding, bonding, or other methods. Of course, to achieve axial positioning and abutment of the first annular elastic element 1122b and the second annular elastic element 1122c, the inner annular surface of the annular connector can be set as a stepped surface. Positioning is achieved based on the stepped structure, and the height of the step is made to be the same as the total thickness of the first annular elastic element 1122b and the second annular elastic element 1122c to achieve flush connection at the connection point.
[0064] like Figure 7 As shown, in this embodiment, the first end of the second annular elastic member 1122c and the first end of the first annular elastic member 1122b are also installed in a nested manner, and are fixed by welding or bonding at the installation position to effectively ensure tight installation.
[0065] In this embodiment, the outer cylinder 1122a, the first annular elastic element 1122b, the second annular elastic element 1122c, and the aperture adjustment element 1122d are all made of stainless steel to ensure the stability of their material properties.
[0066] Combination Figure 7 and Figure 8As shown, according to one embodiment of the present invention, the first annular elastic member 1122b includes: a first connecting ring 1122b1 disposed at a first end of the first annular elastic member 1122b, and a first elastic plate 1122b2 disposed on the first connecting ring 1122b1; wherein, the first elastic plate 1122b2 is a long strip plate with an arc-shaped cross-section, and a plurality of first elastic plates 1122b2 are disposed at equal intervals along the circumference of the first connecting ring 1122b1. In this embodiment, the radial thickness of the first elastic plate 1122b2 gradually increases along the direction close to the first connecting ring 1122b1, and the radial inner surface of the first elastic plate 1122b2 is a cylindrical surface portion with the same diameter as the inner annular surface of the first connecting ring 1122b1, while the radial outer surface of the first elastic plate 1122b2 is a conical surface portion of a truncated cone.
[0067] Combination Figure 7 and Figure 8 As shown, according to one embodiment of the present invention, the second annular elastic member 1122c includes: a second connecting ring 1122c1 disposed at a first end of the second annular elastic member 1122c, and a second elastic plate 1122c2 disposed on the second connecting ring 1122c1; wherein, the second elastic plate 1122c2 is a long strip plate with an arc-shaped cross-section, and a plurality of second elastic plates 1122c2 are disposed at equal intervals along the circumference of the second connecting ring 1122c1. In this embodiment, the radial thickness of the second elastic plate 1122c2 is uniform along the direction close to the second connecting ring 1122c1, thereby, the radial inner surface of the second elastic plate 1122c2 is a cylindrical surface portion with the same diameter as the inner annular surface of the second connecting ring 1122c1, and the radial outer surface of the second elastic plate 1122c2 is a cylindrical surface portion parallel to the radial inner surface of the second elastic plate 1122c2.
[0068] Combination Figure 7 and Figure 8As shown, according to one embodiment of the present invention, when the second elastic plate 1122c2 and the first annular elastic member 1122b are nested together, the second elastic plate 1122c2 and the first elastic plate 1122b2 are misaligned, so that the second elastic plate 1122c2 blocks the gap between adjacent first elastic plates 1122b2, and the first elastic plate 1122b2 can also block the gap between adjacent second elastic plates 1122c2. Thus, by fixing the first end of the first annular elastic member 1122b and the first end of the second annular elastic member 1122c together, the assembly can be enclosed to form a sidewall seal. The closed annular cylinder has only abutting contact between the first elastic plate 1122b2 and the second elastic plate 1122c2. Therefore, based on the movement of the aperture adjustment member 1122d along the axial direction of the first annular elastic member 1122b, the radial thickness of the first elastic plate 1122b2 can be used to achieve the contraction and pressing of the first elastic plate 1122b2 under the abutting action. Thus, based on the force transmission effect of the first elastic plate 1122b2, the second elastic plate 1122c2 can produce a corresponding elastic contraction, thereby realizing the continuous and flexible adjustment of the outlet end opening diameter of the outer cylinder 1122a of the structural member.
[0069] Combination Figure 7 and Figure 8 As shown, according to one embodiment of the present invention, on the second annular elastic member 1122c, and along the direction away from the second connecting ring 1122c1, the interval between adjacent second elastic plates 1122c2 can be gradually increased. Thus, by setting its larger interval, sufficient space for movement between adjacent second elastic plates 1122c2 is effectively ensured when the opening diameter of the outlet end is reduced, so as to effectively avoid mutual interference.
[0070] In this embodiment, to avoid the impact of the step position caused by the direct stacking of the first elastic plate 1122b2 and the second elastic plate 1122c2 on the accuracy of the orifice size, the thickness of the second elastic plate 1122c2 can be reduced to significantly improve the accuracy of the orifice size, thereby achieving precise and effective flow control. Furthermore, reducing the thickness of the second elastic plate 1122c2 also allows it to have better elasticity, making it easier to be driven by the first elastic plate 1122b2, effectively improving the convenience of the drive adjustment process.
[0071] Combination Figure 9 , Figure 10 and Figure 11As shown, in another embodiment, to reduce the impact of the thickness of the second elastic plate 1122c2 on the dimensional accuracy of the aperture, a receiving groove for accommodating the second elastic plate 1122c2 can be provided on the adjacent first elastic plate 1122b2. Thus, the second elastic plate 1122c2 can be arranged in the receiving groove to block the gap between the adjacent first elastic plates 1122b2. Moreover, by using the method of stacking concave cavities, a mechanical seal can be achieved between the interconnected positions based on the mutual cooperation between the mechanical structures, effectively ensuring the overall sealing performance when the aperture of the first annular elastic member 1122b and the second annular elastic member 1122c changes.
[0072] In this embodiment, to avoid mutual interference between structures during the change of aperture, a certain gap can be set at the position where they cooperate to achieve a sufficient range of aperture change. For example, the interval between adjacent receiving slots on the same first elastic plate 1122b2 is smaller than the interval between adjacent second elastic plates 1122c2, thereby facilitating the movement of the second elastic plate 1122c2.
[0073] This configuration allows for more flexible adjustment of the thickness of the second elastic plate 1122c2, enabling more flexible adjustment of its elasticity and providing the solution with greater usability.
[0074] like Figure 7 As shown, according to one embodiment of the present invention, the aperture adjustment member 1122d can be configured as an annular structure, and its inner annular surface can be configured as a conical surface. The end with the smallest diameter of the inner annular surface can realize the control of the maximum aperture of the combination of the first annular elastic member 1122b and the second annular elastic member 1122c. Then, as the aperture adjustment member 1122d moves, based on the abutment of the end with the smallest diameter of its inner annular surface with the outer surface of the first annular elastic member 1122b, the aperture of the combination of the first annular elastic member 1122b and the second annular elastic member 1122c can be controlled.
[0075] like Figure 12As shown, in this embodiment, the second perforated plate 113 has a plurality of second through holes 113a penetrating its body, and the diameters of some of the second through holes 113a on the second perforated plate 113 are different. The second perforated plate 113 can be configured as a circular plate, and the diameters of the second through holes 113a in the second perforated plate 113 can be configured as three types. Specifically, the second through hole 113a with the largest diameter can be one, and it is arranged at the center of the second perforated plate 113; the second through holes 113a with a second diameter can be multiple, and they can be arranged at equal intervals around the second through hole 113a with the largest diameter along the circumference of the second perforated plate 113, so as to achieve the enclosure of the second through holes 113a with the second diameter around the central second through hole 113a; the smallest diameter... Multiple second through holes 113a can be provided, and they can be arranged at equal intervals around the second through holes 113a of the second aperture along the circumference of the second orifice plate 113, so as to realize the enclosure of the second through hole 113a of the second aperture by the second through hole 113a of the smallest aperture; furthermore, since the opening areas of the three apertures of the second through holes 113a are different, the number of second through holes 113a of different apertures can be gradually increased from the center to the edge of the second orifice plate 113, so as to realize the flexible control of gas flow by different second through holes 113a.
[0076] In this embodiment, the second through holes 113a with the second aperture are arranged in an equally spaced annular array using a first ring; the second through holes 113a with the smallest aperture are arranged in an equally spaced annular array using a second ring; wherein, the interval between the center of the first ring and the center of the second through hole 113a with the largest aperture is the first interval, and the interval between the first ring and the second ring is the second interval, and the first interval and the second interval are either equal or different. In this embodiment, there can be 8 second through holes 113a with the second aperture, and 16 second through holes 113a with the smallest aperture.
[0077] In this embodiment, the diameter of the second through hole 113a is at least 1 mm.
[0078] In this embodiment, the second perforated plate 113 is obtained based on the following steps: Perform fluid dynamics modeling and simulation: A three-dimensional model of the second perforated plate 113 is constructed, wherein two concentric rings are constructed on the second perforated plate 113: a first ring for arranging the second through holes 113a of the second diameter and a second ring for arranging the second through holes 113a of the minimum diameter. Further, second through holes 113a are respectively set at the center of the second perforated plate 113, circumferentially on the first ring, and circumferentially on the second ring. Specifically, there is one second through hole 113a at the center, eight second through holes 113a on the first ring, and sixteen second through holes 113a on the third ring. The initial diameter of each second through hole 113a is set to 1 mm.
[0079] Perform gas flow analysis: An atomic gas chamber is placed in the same direction as the second orifice plate 113, with the gas inlet of the atomic gas chamber facing the second orifice plate 113 and 100 mm away from it. The gas flow rate at the gas inlet is observed.
[0080] Optimize the diameter of the second through hole 113a, the diameter of the first annulus, and the diameter of the second annulus: To ensure that the diameter of each second through hole 113a remains unchanged, the diameters of the first and second rings are sequentially combined within the range of 1mm to 5mm. The gas flow rate at the inlet of the atomic gas chamber is measured. After the maximum value is reached, the diameters of the first and second rings are determined.
[0081] Keeping the diameters of the first and second rings unchanged, the diameters of the second through hole 113a located at the center of the second orifice plate 113, the second through hole 113a on the first ring, and the second through hole 113a on the second ring are sequentially combined and traversed within the range of 1mm to 5mm. The gas flow rate at the inlet of the atomic gas chamber is measured. After reaching the maximum value, the diameter of the second through hole 113a is determined.
[0082] With the parameters set the same as the aforementioned first orifice plate 112, the simulation results after completing the gas flow analysis are as follows: Figure 4 As shown.
[0083] The second well plate 113 was prepared and experiments were conducted: The second orifice plate 113 is prepared and installed at the corresponding position in the reaction chamber 11 for nitrogen flow test. The effect is judged by the flow meter. If the flow rate does not reach the preset condition, the above arrangement is repeated to optimize the setting position and distribution pattern of the second through hole 113a on it, so as to further optimize the second orifice plate 113.
[0084] In this embodiment, the second through hole 113a in the second perforated plate 113 is at least partially open during the deposition process of the atomic gas chamber. Thus, the open opening allows for controlled gas discharge during the process of filling the reaction chamber with gas, effectively ensuring sufficient coating on the walls of the atomic gas chamber.
[0085] In this embodiment, the heating platform provided in the reaction chamber 11 can be an electric heating platform, thereby enabling controlled heating and precise temperature control, which greatly ensures high stability and high precision in the film deposition process.
[0086] It should be noted that the second orifice plate 113 also adopts the same combination configuration as the first orifice plate 112 mentioned above, which will not be described again here.
[0087] Through the above settings, this scheme, based on simulation and experimental testing, optimizes the diameter of the circular holes at different positions of the first orifice plate 112 and the second orifice plate 113 at both ends, causing the gas transported from the outer periphery to converge towards the center, thereby increasing the gas flow rate at the gas inlet of the atomic gas chamber and improving coating efficiency and reliability. To simplify the design, the first orifice plate 112 and the second orifice plate 113 are set to the same specifications. According to requirements and the concept of this scheme, the shape and distribution of the circular hole diameters of the first orifice plate 112 and the second orifice plate 113 can be adjusted to achieve different forms of atomic gas chamber coating.
[0088] like Figure 13 As shown, according to one embodiment of the present invention, the system for preparing a sapphire coated atomic gas chamber further includes an alkali metal filling unit 2; wherein the alkali metal filling unit 2 includes a gas filling pipe 21, an alkali metal source 22, a heating oven 23, and a vacuum unit. In this embodiment, to facilitate reliable connection with the alkali metal source 22 and the coated atomic gas chamber, the gas filling pipe 21 can be made of glass, thereby enabling fusion welding between them, greatly ensuring the reliability and convenience of the connection. Furthermore, it also facilitates reliable sealing of the atomic gas chamber after the alkali metal filling.
[0089] Furthermore, the gas filling pipe 21 is partially disposed inside the heating oven 23, and the alkali metal source 22 is connected to the portion of the gas filling pipe 21 inside the heating oven 23. Thus, it is convenient to fuse the alkali metal source 22 and the atomic gas chamber into the gas filling pipe 21 inside the heating oven 23, and it is convenient to achieve overall heating after connection, which greatly improves the ease of use of the present invention.
[0090] Furthermore, the vacuum unit is connected to the end of the gas filling pipe 21 located outside the heating oven 23; thereby, it is convenient to remove the residual air inside before alkali metal filling, so as to effectively ensure the high purity filling effect of the present invention.
[0091] like Figure 13 As shown, according to one embodiment of the present invention, the heating oven 23 includes a hollow upper cover 231 and a bottom plate 232; wherein the upper cover 231 and the bottom plate 232 are closable. In this embodiment, the heating oven 23 can be configured as a rectangular structure, wherein the upper cover 231 is a hollow rectangular box body with an opening at the lower end, and the bottom plate 232 is a rectangular plate that matches the lower opening of the upper cover 231; wherein both the upper cover 231 and the bottom plate 232 are provided with heaters to achieve controlled heating. In this embodiment, a linear groove is provided on one side of the upper cover 231, which allows the air filling pipe 21 to pass through the linear groove of the upper cover 231 to facilitate the vertical movement of the upper cover 231.
[0092] The above description is merely an example of a specific solution of the present invention. For any devices and structures not described in detail herein, it should be understood that they are implemented using common devices and methods already available in the art.
[0093] The above description is merely one embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the invention by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A method for preparing atomic gas cells for sapphire coating, characterized in that, Includes the following steps: S1. Place the cleaned atomic gas chamber on the heating base of the reaction chamber, and fill the reaction chamber with replacement gas to remove the residual gas therein; S2. Aluminum source gas is introduced into the reaction chamber, and chemical adsorption occurs on the wall of the atomic gas chamber based on atomic layer deposition technology to form a first film layer; S3. The reaction chamber is filled with replacement gas to remove the residual aluminum source gas therein; S4. Oxide gas is introduced into the reaction chamber to oxidize the first film layer and transform it into an aluminum oxide film layer; S5. A displacement gas is introduced into the reaction chamber to remove residual oxide gases therein; S6. Repeat steps S2 to S5 to form an aluminum oxide film layer with a predetermined number of layers and a predetermined thickness on the wall surface of the atomic gas chamber, so as to form an atomic gas chamber with a sapphire coating.
2. The method for preparing atomic gas cells for sapphire coating according to claim 1, characterized in that, Also includes: S7. Remove the atomic gas chamber and fill it with alkali metal.
3. The method for preparing atomic gas cells for sapphire coating according to claim 2, characterized in that, In step S1, the step of placing the cleaned atomic gas chamber on the heating platform of the reaction chamber, wherein the operating temperature of the heating platform is 250℃~300℃; The gas inlet of the atomic gas chamber is oriented perpendicularly to the gas inlet of the reaction chamber.
4. The method for preparing atomic gas cells for sapphire coating according to claim 3, characterized in that, In step S2, the aluminum source gas is introduced into the reaction chamber using an alternating pulse gas intake method; wherein, in the alternating pulse gas intake method, the gas intake time of each pulse is greater than or equal to 10 minutes.
5. The method for preparing atomic gas cells for sapphire coating according to claim 4, characterized in that, In step S4, where oxide gas is introduced into the reaction chamber to oxidize the first film layer and transform it into an alumina film layer, the thickness of the alumina film layer is 0.1 nm to 0.2 nm.
6. The method for preparing atomic gas cells for sapphire coating according to claim 5, characterized in that, Step S7, the step of removing the atomic gas chamber and filling it with alkali metals, includes: S71. Connect the alkali metal source and at least one of the atomic gas cells to the same gas filling pipe; S72. Vacuum the atomic gas chamber based on the gas filling pipe, and place the atomic gas chamber, the alkali metal source and at least part of the gas filling pipe in a heating oven; S73. Open the sealing structure between the alkali metal source and the gas filling pipe, and start the heating oven to perform wrapping heating according to the preset heating scheme; wherein, the preset heating scheme is: heating from room temperature to 200°C for 1 hour, maintaining at 200°C for 2 hours, and cooling from 200°C to room temperature for 1 hour. S74. After the heating oven completes heating based on the preset heating scheme, the heating oven is removed, and the atomic gas chamber is sealed and taken off from the gas filling pipe to complete the alkali metal filling of the atomic gas chamber.
7. The method for preparing atomic gas cells for sapphire coating according to claim 6, characterized in that, In step S72, during the step of evacuating the atomic gas chamber based on the gas filling pipe, the vacuum level evacuated is better than 10. -5 Pa.
8. The method for preparing atomic gas cells for sapphire coating according to claim 7, characterized in that, The atomic gas chamber is a high borosilicate glass gas chamber or a quartz gas chamber; The aluminum source gas is trimethylaluminum gas; The oxide gas is deionized water vapor; The alkali metal source is either cesium or rubidium.
9. A system applied to the method for preparing atomic gas cells for sapphire coating according to any one of claims 1 to 8, characterized in that, include: Coating unit (1); The coating unit (1) includes: a reaction chamber (11) with a heating base, a first pipeline (12) connected to the reaction chamber (11), an aluminum source device (13), an oxide source device (14) and a displacement gas source device (15) connected to the first pipeline (12). The reaction chamber (11) includes: a regular and hollow reaction chamber body (111), and a first perforated plate (112) and a second perforated plate (113) respectively provided at opposite ends of the reaction chamber body (111); One end of the first pipeline (12) is connected to the position where the first perforated plate (112) is located on the main body of the reaction chamber (111); The first perforated plate (112) has a plurality of first through holes (112a) penetrating its body, and the diameter of some of the first through holes (112a) on the first perforated plate (112) is different; The second perforated plate (113) has a plurality of second through holes (113a) penetrating its body, and the diameter of some of the second through holes (113a) on the second perforated plate (113) is different.
10. The system for preparing atomic gas cells for sapphire coating according to claim 9, characterized in that, Also includes: Alkali metal filling unit (2); The alkali metal filling unit (2) includes: a gas filling pipe (21), an alkali metal source (22), a heating oven (23), and a vacuum unit; The inflation pipe (21) is partially installed inside the heating oven (23); The alkali metal source (22) is connected to the portion of the gas filling pipe (21) located inside the heating oven (23); The vacuum unit is connected to the end of the gas filling pipe (21) located outside the heating oven (23); The heating oven (23) includes: a hollow upper cover (231) and a bottom plate (232); The upper cover (231) and the bottom plate (232) are designed to be openable and closable.
Citation Information
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