Coating method for hydrogen atomic clock storage bubbles

By preparing and sintering poly(perfluoroethylene) propylene resin particles for coating, the problem of unstable performance indicators in the coating process of hydrogen atomic clock storage bubbles was solved, and the high stability and consistency of hydrogen atomic clocks were achieved.

CN117960525BActive Publication Date: 2026-01-06BEIJING INST OF RADIO METROLOGY & MEASUREMENT
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Patent Information

Application Number
CN202311822819.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-27
Publication Date
2026-01-06
Estimated Expiration
2043-12-27

AI Technical Summary

Technical Problem

Existing hydrogen atomic clock storage bubble coating processes are insufficient to improve the consistency of hydrogen atomic clock performance indicators, especially the instability of indicators such as atomic transition amplitude, daily stability, and drift.

Method used

A coating material is prepared by mixing poly(perfluoroethylene) propylene resin particles, a co-solvent, and water in a predetermined ratio. The coating is then formed on the inner wall of the storage bubble by rotating the storage container, cleaning with an acidic solution and distilled water, spraying, dipping, or brushing, and sintering multiple times until the desired thickness is achieved.

Benefits of technology

The atomic transition amplitude of the hydrogen atomic clock was achieved in the range of -104 dBm to -108 dBm, with daily stability on the order of 10⁻¹⁵ and drift on the order of 10⁻¹⁶, ensuring the stability and consistency of the performance indicators of the hydrogen atomic clock.

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Abstract

The application discloses a coating method for a hydrogen atomic clock storage bubble. The coating method comprises steps S1 to S4. Step S1 is mixing polyfluoroethylene propylene resin particles, a cosolvent and water in a predetermined proportion to prepare a coating material, and storing the coating material in a rotating storage container; step S2 is sequentially cleaning the inner wall surface of the storage bubble with an acid solution and distilled water, and drying the cleaned storage bubble in an oven; step S3 is coating the coating material in the storage container to the inner wall surface of the storage bubble by using a spraying, dipping or brushing coating method, and rotating the storage bubble; and step S4 is sintering the coated storage bubble, repeating steps S3 to S4 N times until the coating on the inner wall surface of the storage bubble reaches a required coating thickness. The application can solve the problem of unstable atomic transition amplitude, daily stability and drift of the hydrogen atomic clock in the prior art.
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Description

Technical Field

[0001] This application relates to the field of atomic clock technology, and more specifically, to a coating method for a hydrogen atomic clock storage bubble. Background Technology

[0002] A hydrogen atomic clock is a key device for generating and maintaining standard time, requiring excellent long-term operational reliability and stability during timekeeping. F =0→F=0,m F =0) The frequency accuracy and stability of a quantum frequency standard system depend on the transition frequency stability and phase stability of a large number of hydrogen atoms, and are subject to various constraints. Among them, the maintenance of atomic state has a direct impact on improving the system's performance. Currently, by using hydrogen atomic clock storage bubble coating technology, a long-chain molecular film of high molecular polymer material is added to the inner wall of the storage bubble, and then the coating material is sintered into a film at a certain temperature and time. This molecular film is inert to hydrogen atoms, so that the atoms do not change their state when colliding with the wall, thereby improving the performance of the hydrogen atomic clock.

[0003] In a hydrogen atomic clock, the energy level transitions of atoms occur during the storage time within the storage bubble. Atoms collide multiple times with the bubble wall. To minimize changes in the hyperfine energy level states of atoms during these transitions, the film formation on the inner wall of the hydrogen clock's storage bubble directly determines the generation and indicators of the transition signals. To improve the performance of the hydrogen atomic clock, relatively high requirements are placed on the quality of the long-chain molecular film on the inner wall of the storage bubble, considering both its smoothness and integrity. Therefore, the coating process for the storage bubble has become a key technology in the development of hydrogen clocks. However, existing coating processes for storage bubbles are insufficient to improve the performance of hydrogen atomic clocks and cannot guarantee the consistency of the hydrogen atomic clock's performance when the coated storage bubble is used. Summary of the Invention

[0004] The main objective of this application is to provide a coating method for hydrogen atomic clock storage bubbles, so as to solve the problems of instability in the atomic transition amplitude, daily stability and drift of hydrogen atomic clocks in the prior art.

[0005] According to one aspect of this application, a coating method for a hydrogen atomic clock storage bubble is provided, comprising:

[0006] Step S1: Prepare a coating material by mixing poly(perfluoroethylene propylene) resin particles, co-solvent and water in a predetermined ratio, and store the coating material in a rotating storage container.

[0007] Step S2: The inner wall of the storage bubble is cleaned with acidic solution and distilled water in sequence, and the cleaning is performed at least once. The cleaned storage bubble is then dried in an oven.

[0008] Step S3: Apply the coating material in the storage container to the inner wall surface of the storage bubble by spraying, dipping, or brushing, and rotate the storage bubble at least once.

[0009] Step S4: Sinter the coated storage bubble, repeat steps S3 to S4 for N times, until the coating on the inner wall of the storage bubble reaches the required coating thickness.

[0010] Further, in step S1, the mass ratio of the poly(fluoroethylene propylene) resin particles, the co-solvent, and the water is (45-55):(5-10):(35-50).

[0011] Furthermore, the co-solvent includes sodium dodecyl sulfate or polyoxyethylene stearate.

[0012] Further, in step S1, the storage container is a sealed container; the rotation speed of the storage container is 20 r / min to 30 r / min; and the storage temperature of the storage container is 20°C to 30°C.

[0013] Furthermore, in step S2, the acidic solution is hydrofluoric acid; and the number of cleaning cycles is three.

[0014] Furthermore, in step S2, the drying temperature of the oven is 50°C to 60°C; the drying time of the oven is 55 min to 65 min.

[0015] Furthermore, in step S3, the number of rotations is three.

[0016] Furthermore, in step S4, when N=2, the storage bubble is sintered three times;

[0017] The sintering temperature for the first and second sintering is 170℃ to 180℃, and the sintering time is 25min to 35min.

[0018] The sintering temperature for the third sintering is 360℃ to 370℃, and the sintering time is 85 min to 95 min.

[0019] Further, in step S3, the coated storage bubble is placed in a fixture and left to stand for 20 to 30 minutes.

[0020] In this application, the coating method described in steps S1 to S4 can be used when actually coating the storage bubble. In step S1, a coating material needs to be selected. The coating material in this application is a mixture of polytetrafluoroethylene propylene resin particles, a co-solvent, and water in a predetermined ratio. This coating material can be placed in a storage container for storage. After the coating material is placed, the storage container needs to be kept rotating to ensure that the coating material can be accessed at any time during the coating process. Before coating begins, the inner wall of the storage bubble needs to be cleaned in step S2. An acidic solution can be poured into the storage bubble and allowed to flow fully on the inner wall. Then, distilled water can be poured into the storage bubble to clean the inner wall. This operation should be repeated at least once to ensure the cleanliness of the inner wall of the storage bubble. After cleaning, the storage bubble is dried in an oven to keep the inner wall of the storage bubble dry. In step S3, the coating material is first removed from the storage container, and then applied to the inner wall of the storage bubble using spraying, dipping, or brushing methods. When the coating material enters the storage bubble, it is rotated at least once to ensure sufficient flow of the material on the inner wall, effectively guaranteeing a complete coating. In step S4, the coated storage bubble is sintered, allowing the coating material to form and adhere to the inner wall. After sintering, steps S3 to S4 can be repeated N times, depending on the required coating thickness, until the coating on the inner wall of the storage bubble reaches the desired thickness. Compared to existing coating methods, the coating method in this application is more feasible and ensures the stability of the atomic transition amplitude, daily stability, and drift of the hydrogen atomic clock, while also guaranteeing the consistency of the hydrogen atomic clock's performance indicators. Attached Figure Description

[0021] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments of this application and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings:

[0022] Figure 1 This is a flowchart of the coating method for the hydrogen atomic clock storage bubble disclosed in this application;

[0023] Figure 2 This is a flowchart illustrating the specific implementation process of the coating method for the hydrogen atomic clock storage bubble disclosed in this application. Detailed Implementation

[0024] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. This application will now be described in detail with reference to the accompanying drawings and embodiments.

[0025] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0026] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps described in these embodiments do not limit the scope of this application. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following drawings denote similar items; therefore, once an item is defined in one drawing, it need not be further discussed in subsequent drawings.

[0027] See Figures 1 to 2 As shown, this application provides a coating method for a hydrogen atomic clock storage bubble, hereinafter referred to as the coating method, which includes steps S1 to S4.

[0028] Step S1 involves preparing a coating material by mixing poly(perfluoroethylene propylene) resin particles, a co-solvent, and water in a predetermined ratio, and storing the coating material in a rotating storage container. Step S2 involves cleaning the inner wall of the storage bubble with an acidic solution and distilled water at least once, and then drying the cleaned storage bubble in an oven. Step S3 involves applying the coating material from the storage container to the inner wall of the storage bubble using a spraying, dipping, or brushing method, and rotating the storage bubble at least once. Step S4 involves sintering the coated storage bubble, and repeating steps S3 to S4 N times until the coating on the inner wall of the storage bubble reaches the required coating thickness.

[0029] In this embodiment, the coating method described in steps S1 to S4 can be used when actually coating the storage bubble. In step S1, a coating material needs to be selected first. In this embodiment, the coating material is a mixture of polytetrafluoroethylene propylene resin particles, a co-solvent, and water in a predetermined ratio. The coating material is then placed in a storage container for storage. After the coating material is placed, the storage container needs to be kept rotating to ensure that the coating material can be accessed at any time during the coating process. Before coating begins, the inner wall of the storage bubble needs to be cleaned in step S2. An acidic solution can be poured into the storage bubble and allowed to flow fully on the inner wall. Then, distilled water can be poured into the storage bubble to clean the inner wall. This operation should be repeated at least once to ensure the cleanliness of the inner wall of the storage bubble. After cleaning, this embodiment uses an oven to dry the cleaned storage bubble to keep the inner wall of the storage bubble dry. In step S3, the coating material is first removed from the storage container, and then applied to the inner wall of the storage bubble using spraying, dipping, or brushing methods. When the coating material enters the storage bubble, it needs to be rotated at least once to ensure sufficient flow of the material on the inner wall, effectively guaranteeing a complete coating. In step S4, the coated storage bubble is sintered to form and adhere the coating material to the inner wall. After sintering, steps S3 to S4 can be repeated N times according to the required coating thickness until the coating on the inner wall of the storage bubble reaches the desired thickness. Compared to existing coating methods, the coating method in this embodiment is more feasible and ensures the stability of the atomic transition amplitude, daily stability, and drift of the hydrogen atomic clock, while maintaining the consistency of its performance indicators. Specifically, the atomic transition amplitude is between -104 dBm and -108 dBm, and the daily stability reaches 10... -15 On the order of magnitude, the drift can reach 10. -16 Magnitude.

[0030] Further, in step S1, the mass ratio of poly(perfluoroethylene propylene) resin particles, co-solvent, and water in this embodiment is (45-55):(5-10):(35-50), thereby obtaining a poly(perfluoroethylene propylene) suspension. The performance indicators of this suspension are closely related to the coating method in this embodiment, and the performance indicators of the poly(perfluoroethylene propylene) suspension are shown in Table 1. Specifically, this embodiment contains 54% poly(perfluoroethylene propylene) resin particles and 46% a mixture of co-solvent and water.

[0031] Table 1 Performance Indicators of Poly(Fluoroethylene) Propylene Dispersion

[0032] Serial Number Performance indicators Required value 1 density <![CDATA[1.41g / cm 3 ]]> 2 Viscosity 25 mPa·s 3 Solid content 54% 4 Average particle size 180nm 5 Melting temperature 260℃

[0033] Furthermore, the co-solvent in this embodiment includes sodium dodecyl sulfate or polyoxyethylene stearate. The coating material in this embodiment is composed of poly(perfluoroethylene propylene) resin particles, a co-solvent, and water. Water is a common solvent, and the poly(perfluoroethylene propylene) resin particles are soluble in water. However, due to the low polarity of water, its ability to dissolve poly(perfluoroethylene propylene) resin particles is relatively weak. To improve the dissolution rate and efficiency of poly(perfluoroethylene propylene) resin particles in water, a certain amount of surfactant, such as sodium dodecyl sulfate or polyoxyethylene stearate, is usually added as a co-solvent.

[0034] Further, in step S1, the storage container in this embodiment is a sealed container; the rotation speed of the storage container is 20 r / min to 30 r / min, for example, 20 r / min, 22 r / min, 24 r / min, 26 r / min, 28 r / min, or 30 r / min; the storage temperature of the storage container is 20°C to 30°C, for example, 20°C, 22°C, 24°C, 25°C, 27°C, or 30°C. Since the coating material in this embodiment is a polytetrafluoroethylene propylene suspension, if the coating material is stored using conventional static storage methods, polytetrafluoroethylene propylene resin particles will precipitate, and the viscosity will change, directly affecting the thickness, smoothness, and integrity of the film. Therefore, the coating material needs to be stored under certain temperature and continuous solution dispersion conditions.

[0035] Experimental verification showed that when the stirring paddle is placed in the suspension and the coating material is stored using open mechanical stirring and ultrasonic dispersion, both methods involve direct contact with the coating material. In this case, both methods cause shear force damage to the particles in the coating material, affecting its size. However, the storage container in this embodiment is horizontally placed. When the coating material is placed in this container, it remains sealed. The container is rotated at a speed of 20 to 30 r / min and a storage temperature of 20°C to 30°C, thereby achieving continuous dispersion of the coating material and effectively preventing precipitation and aggregation in the polytetrafluoroethylene (PTFE) suspension.

[0036] Specifically, when the rotation speed of the storage container is below 20 r / min, the lower rotation speed reduces the dispersion effect of the coating material, easily leading to sedimentation and agglomeration, which in turn affects the integrity and uniformity of the film. When the rotation speed of the storage container is above 30 r / min, it can easily damage the particles in the coating material. When the storage temperature of the storage container is not within the range of 20℃ to 30℃, the coating material is extremely prone to sedimentation and agglomeration.

[0037] Further, in step S2, the acidic solution in this embodiment is preferably hydrofluoric acid; the cleaning is performed three times. This embodiment uses hydrofluoric acid and distilled water to clean the inner wall of the storage bubble, ensuring the cleanliness of the inner wall and effectively preventing the formation and peeling of subsequent coating materials. In addition, in this embodiment, hydrofluoric acid is first poured into the storage bubble and the bubble is shaken to allow the hydrofluoric acid to flow fully on the inner wall, then distilled water is poured in for rinsing, and this operation is repeated three times. Experimental verification shows that three cleaning cycles are sufficient to ensure optimal cleanliness of the inner wall.

[0038] Furthermore, in step S2, the drying temperature of the oven in this embodiment is 50°C to 60°C, for example, 50°C, 52°C, 54°C, 56°C, 58°C, or 60°C; the drying time of the oven is 55 min to 65 min, for example, 55 min, 57 min, 60 min, 63 min, or 65 min. When the drying temperature is below 50°C, the evaporation time of moisture in the inner wall surface is prolonged, and the drying time is increased, which easily reduces the drying efficiency. When the drying temperature is above 60°C and remains at a high temperature for a long time (drying temperature above 100°C), the storage bubbles are easily damaged.

[0039] Specifically, the drying time of the oven in this embodiment is 60 minutes. It can be understood that the drying time is affected by the drying temperature. When the drying temperature of the oven in this embodiment is 50°C to 60°C, the drying time of the oven is 60 minutes.

[0040] Furthermore, in step S3, the number of rotations in this embodiment is three. Considering the structural shape characteristics of the storage bubble in this application, since the bubble opening is small, this embodiment preferably uses an dip-coating method to pour the coating material into the storage bubble and rotates the storage bubble three times. This allows the coating material to flow fully on the inner wall surface of the storage bubble, effectively ensuring the integrity of the coating material on the inner wall surface of the storage bubble.

[0041] Furthermore, in step S4, when N=2 in this embodiment, the storage bubble is sintered three times. Figure 2It can be seen that when N=0, this embodiment does not perform the cycle of steps S3 to S4, that is, it only includes the first coating and the first sintering; when N=1, this embodiment performs the cycle of steps S3 to S4 once, in which case the coating method includes the first coating, the first sintering, the second coating, and the second sintering; when N=2, this embodiment performs the cycle of steps S3 to S4 twice, in which case the coating method includes the first coating, the first sintering, the second coating, the second sintering, the third coating, and the third sintering. That is to say, steps S3 and S4 in this embodiment only need to be repeated twice to ensure the integrity of the coating material on the inner wall of the storage bubble, while N>2 is an invalid operation, which reduces the coating efficiency to a certain extent.

[0042] Optionally, in this embodiment, the sintering temperature for the first and second sintering is 170°C to 180°C, for example, 170°C, 172°C, 174°C, 176°C, 178°C, and 180°C, and the sintering time is 25 min to 35 min, for example, 25 min, 27 min, 30 min, 33 min, and 35 min. That is to say, the sintering temperature and sintering time for the first and second sintering are consistent. In this embodiment, the purpose of the first and second sintering is to remove water and co-solvent from the coating material to ensure that the coating material can adhere to the inner wall surface of the storage bubble and form a film. When the sintering temperature of the storage bubble is less than 170°C, the film-forming effect of the coating material on the inner wall surface of the storage bubble is easily deteriorated, resulting in the film falling off the inner wall surface and prolonging the sintering time of the storage bubble; when the sintering temperature of the storage bubble is greater than 180°C, the excessively high temperature causes high-temperature damage to the inner wall surface and the film on the inner wall surface. Therefore, in this embodiment, the sintering temperature of the storage bubble is 170°C to 180°C.

[0043] Specifically, in this embodiment, the sintering time for the first and second sintering of the storage bubble is preferably 30 minutes. It is understood that the sintering time is affected by the sintering temperature. When the sintering temperature of the storage bubble in this embodiment is 170°C to 180°C, a sintering time of 30 minutes is sufficient to ensure the film-forming effect of the coating material on the inner wall of the storage bubble, and to a certain extent avoid film peeling, cracking, and porosity defects.

[0044] Optionally, in this embodiment, the sintering temperature for the third sintering is 360°C to 370°C, for example, 360°C, 362°C, 364°C, 366°C, 368°C, or 370°C, and the sintering time is 85 min to 95 min, for example, 85 min, 87 min, 90 min, 93 min, or 95 min. That is to say, the sintering temperature and time for the third sintering differ from those for the first and second sintering. The third sintering intensifies the movement of resin molecules in the coating material, leading to the disappearance of the interfaces between the polytetrafluoroethylene propylene resin particles. At this point, the coating material forms a continuous and dense whole on the inner wall surface, effectively ensuring the integrity of the film formation. However, when the sintering temperature of the storage bubble is not within the range of 360°C to 370°C, it will severely affect the length of the polytetrafluoroethylene propylene resin molecular chains, reducing the film formation effect to some extent. Therefore, in this embodiment, the sintering temperature of the storage bubble is 360°C to 370°C.

[0045] Specifically, in this embodiment, the sintering time of the storage bubble is 90 minutes. It can be understood that when the sintering temperature of the storage bubble in this embodiment is 360°C to 370°C, the sintering time of the storage bubble is 90 minutes.

[0046] Further, in step S3, in this embodiment, the coated storage bubble is placed in a fixture and left to stand for 20 to 30 minutes, for example, 20 minutes, 22 minutes, 24 minutes, 26 minutes, 28 minutes, or 30 minutes. In this embodiment, the coated storage bubble is placed in the fixture with the bubble opening facing down and left to stand for 20 to 30 minutes, and the bubble opening is visually inspected to ensure that no excess coating material flows out. Then, the fixture and the storage bubble are placed together in an oven for sintering, during which the bubble opening must be kept facing down.

[0047] Combination Figure 2 As shown, the coating method for hydrogen atomic clock storage bubbles in this application includes the following specific embodiments:

[0048] (1) Storage foam cleaning

[0049] The inner wall of the storage bubble was cleaned three times using hydrofluoric acid and distilled water. First, hydrofluoric acid was poured into the storage bubble and shaken to allow it to flow freely on the inner wall. Then, distilled water was poured in for rinsing. This process was repeated three times. Finally, the storage bubble was placed in an oven to dry the inner wall. The oven temperature was 50°C to 60°C, and the drying time was 60 minutes.

[0050] (2) Storage of dispersion

[0051] The dispersion is a suspension of perfluoroethylene propylene (PFEP), stored under constant temperature and continuous dispersion conditions to prevent sedimentation and stratification of the PFEP resin particles, ensuring readily available dispersibility during coating. A horizontally placed storage container is used, with both ends clamped and rotated uniformly to continuously disperse the PFEP suspension. The storage container remains sealed, and the rotation speed is 20 to 30 r / min. The temperature of the storage container is maintained at a constant 25℃ ± 5℃.

[0052] (3) First coating

[0053] Pour the dispersion into the storage bubble and use the dip-coating method. Rotate the storage bubble three times to prevent the dispersion from flowing completely inside, ensuring that the inner wall of the storage bubble is completely coated with the dispersion.

[0054] (4) First sintering

[0055] After the first coating is completed, place the storage bubble with the bubble opening facing down in the fixture and let it stand for 20 to 30 minutes. Visually inspect the bubble opening for any excess dispersion flowing out. Then, place the storage bubble in the fixture into the oven for sintering. During this process, keep the bubble opening facing down. The temperature for the first sintering is 170°C to 180°C, and the sintering time is 30 minutes.

[0056] (5) Second coating

[0057] Pour the dispersion into the storage bubble and use the dip-coating method. Rotate the storage bubble three times to prevent the dispersion from flowing completely inside, ensuring that the inner wall of the storage bubble is completely coated with the dispersion.

[0058] (6) Second sintering

[0059] After the second coating is completed, place the storage bubble with the bubble opening facing down in the fixture and let it stand for 20 to 30 minutes. Visually inspect the bubble opening for any excess dispersion flowing out. Then, place the storage bubble in the fixture into the oven for sintering. During this process, keep the bubble opening facing down. The temperature for the second sintering is 170°C to 180°C, and the sintering time is 30 minutes.

[0060] (7) Third coating

[0061] Pour the dispersion into the storage bubble and use the dip-coating method. Rotate the storage bubble three times to prevent the dispersion from flowing completely inside, ensuring that the inner wall of the storage bubble is completely coated with the dispersion.

[0062] (8) Third sintering

[0063] After the third coating is completed, place the storage bubble with the bubble opening facing down in the fixture and let it stand for 20 to 30 minutes. Visually inspect the bubble opening for any excess dispersion flowing out. Then, place the storage bubble in the fixture into the oven for sintering. During this process, keep the storage bubble opening facing down. The temperature for the third sintering is 360°C to 370°C, and the sintering time is 90 minutes.

[0064] As can be seen from the above description, the embodiments of this application achieve the following technical effects: Compared with the coating method of hydrogen atomic clock storage bubble in the prior art, the coating method of this application selects polytetrafluoroethylene propylene suspension as coating material and adopts a three-coating and sintering method to ensure the integrity of the coating material film on the inner wall surface of the storage bubble. Moreover, this coating method has been verified in the self-developed sapphire hydrogen atomic clock and has feasibility, consistency of indicators and excellent performance.

[0065] For ease of description, spatial relative terms such as "above," "on top of," "on the upper surface of," "above," etc., are used herein to describe the spatial positional relationship of a device or feature as shown in the figures to other devices or features. It should be understood that spatial relative terms are intended to encompass different orientations in use or operation beyond the orientation of the device as described in the figures. For example, if the device in the figures were inverted, a device described as "above" or "on top of" other devices or structures would subsequently be positioned as "below" or "under" other devices or structures. Thus, the exemplary term "above" can include both "above" and "below." The device may also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatial relative descriptions used herein will be interpreted accordingly.

[0066] Furthermore, it should be noted that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore cannot be construed as limiting the scope of protection of this application.

[0067] The above are merely preferred embodiments of this application and are not intended to limit this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. A film coating method for a hydrogen atomic clock storage bubble, characterized by, The application relates to a method for preparing a polytetrafluoroethylene coating film. Step S1: mixing polytetrafluoroethylene resin particles, a cosolvent and water in a predetermined ratio to prepare a coating film material, and storing the coating film material in a rotating storage container; Step S2: sequentially cleaning the inner wall surface of the storage bubble with an acid solution and distilled water, the cleaning being performed at least once, and drying the cleaned storage bubble in an oven; Step S3: coating the coating film material in the storage container onto the inner wall surface of the storage bubble by spraying, dipping or brushing, and rotating the storage bubble at least once; Step S4: sintering the coated storage bubble, repeating the steps S3 to S4 N times until the coating film on the inner wall surface of the storage bubble reaches a required coating film thickness; when N=2, the sintering of the storage bubble is performed three times; The sintering temperature of the first sintering and the second sintering is 170-180 DEG C, and the sintering time is 25-35 min; The sintering temperature of the third sintering is 360-370 DEG C, and the sintering time is 85-95 min.

2. The coating film forming method for a hydrogen atomic clock storage cell according to claim 1, characterized by, In the step S1, the mass ratio of the polytetrafluoroethylene resin particles, the cosolvent and the water is (45-55):(5-10):(35-50).

3. The coating film forming method for a hydrogen atomic clock storage cell according to claim 2, characterized by, The cosolvent includes sodium dodecyl sulfate or polyoxyethylene stearate.

4. The coating film forming method for a hydrogen atomic clock storage cell according to claim 1, characterized by, In the step S1, the storage container is a sealed container, the rotating speed of the storage container is 20-30 r / min, and the storage temperature of the storage container is 20-30 DEG C.

5. The coating film forming method for a hydrogen atomic clock storage cell according to claim 1, characterized by, In the step S2, the acid solution is hydrofluoric acid, and the cleaning is performed three times.

6. The coating film forming method for a hydrogen atomic clock storage cell according to claim 1, characterized by, In the step S2, the drying temperature of the oven is 50-60 DEG C, and the drying time of the oven is 55-65 min.

7. The coating film forming method for a hydrogen atomic clock storage cell according to claim 1, characterized by, In the step S3, the rotating is performed three times.

8. The coating film forming method for a hydrogen atomic clock storage cell according to claim 1, characterized by, In the step S3, the coated storage bubble is placed in a fixed tool and kept for 20-30 min.