Anodic oxidation electrolytic bath prepared from titanium dioxide nanotubes

Abstract

The anodic oxidation electrolytic bath comprises an electrolytic bath body made of a polytetrafluoroethylene material, and a stirring piece, a temperature control piece and a conductive system are arranged in the electrolytic bath body; wherein the stirring piece comprises double stirring rotors which rotate in opposite directions, the temperature control piece is a bow-shaped temperature control rod, the conductive system comprises a cathode conductive rod, an anode conductive rod and a cathode electrode plate with an adjustable distance, and meanwhile, the conductive system is provided with a liquid outlet and a transparent cover plate with a sealing function. The technical effects that the stability of the electrolysis process is optimized, the temperature control precision is improved, and the operation convenience is enhanced are achieved, and the quality and production efficiency of the titanium dioxide nanotubes are remarkably improved.

Description

Technical Field

[0001] This application relates to the field of anodic oxidation electrolytic cells, and more particularly to an anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes. Background Technology

[0002] Anodizing is a surface treatment process that involves electrochemical oxidation of metal or alloy surfaces, which is related to the subsequent finishing of the workpiece.

[0003] Currently, the most widely used equipment in the anodizing process is the electrolytic cell. The electrolytic cell mainly includes a water tank for storing the electrolyte solution, as well as electrode plates set inside the electrolytic cell. The electrode plates are respectively set on opposite sides of the electrolytic cell, and the electrode plates on the two sides of the electrolytic cell face each other. The electrolytic cell is equipped with a hanger, on which the product is hung and immersed in the electrolyte solution. Here, an external DC power supply is connected to the electrode plates and the hanger to form an electric field, with the workpiece as the anode, to achieve anodizing.

[0004] Anodizing can not only change the color of titanium and titanium alloy surfaces, but also form titanium dioxide nanotube-like structures. This process can obtain nanostructures with adjustable diameter, controllable length, and order, showing great promise for applications in photocatalysis, fuel-sensitized batteries, and surface modification of medical titanium and alloys.

[0005] To obtain nanotube arrays with controllable and regular morphology, they are usually prepared in organic electrolytes. However, the current organic electrolytes absorb moisture from the air, which affects the conductivity. The process is also a heat-generating process, and temperature changes will also affect the array and the anodic oxidation efficiency. Utility Model Content

[0006] To improve the anodic oxidation efficiency of titanium dioxide nanotubes, this application provides an anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes.

[0007] The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes provided in this application adopts the following technical solution:

[0008] An anodizing electrolytic cell prepared from titanium dioxide nanotubes includes an electrolytic cell base, an electrolytic cell body fixedly installed at the top of the electrolytic cell base, a stirring element and a temperature control element arranged at the bottom of the electrolytic cell body, and a cover plate arranged at the top of the electrolytic cell body.

[0009] By adopting the above technical solution and incorporating a stirring element, the electrolyte becomes more uniform, avoiding concentration gradients and thus improving electrolysis efficiency. Simultaneously, the temperature control element precisely regulates the temperature within the electrolytic cell, preventing temperature fluctuations caused by electrolyte components absorbing moisture from the air, further ensuring electrolysis stability and efficiency. This allows for the production of more uniform and high-quality titanium dioxide nanotubes. A stable electrolysis environment and temperature control facilitate nanotube formation and growth, thereby improving product performance and reliability. The cover plate prevents electrolyte splashing, protecting operators from chemical hazards, and also prevents the electrolyte from absorbing water and altering conductivity. Furthermore, the automated control of the temperature control and stirring elements reduces the complexity and risk of manual operation, thereby enhancing the anodizing efficiency and effect of titanium dioxide nanotubes.

[0010] Preferably, the stirring element is two stirring rotors arranged at equal intervals, and a first driving element is provided below the electrolytic cell base. The output shaft of the first driving element passes through the electrolytic cell base and is connected to the stirring rotor.

[0011] By employing the above technical solution, two equidistantly arranged stirring rotors can effectively agitate the electrolyte, ensuring uniform mixing. This helps avoid concentration gradients in the electrolyte, resulting in a more uniform and consistent anodizing process, thereby improving the quality and yield of titanium dioxide nanotubes. Continuous stirring increases the contact area between the electrolyte and the anode material, thus accelerating the electrolytic reaction. This design helps reduce polarization during electrolysis, further improving electrolysis efficiency. The movement of the stirring rotors facilitates electrolyte circulation and renewal, better coordinating with temperature control components to maintain temperature stability within the electrolytic cell. Simultaneously, stirring helps maintain a uniform electrolyte concentration, preventing localized excessively high or low concentrations. Continuous stirring reduces solid particle deposition and scaling in the electrolyte, keeping the electrolytic cell clean and operating efficiently. This helps extend the electrolytic cell's lifespan and reduce maintenance costs.

[0012] Preferably, the two stirring rotors rotate in opposite directions.

[0013] By adopting the above technical solution, the two stirring rotors rotate in opposite directions, which can generate stronger convection and shear force, thereby more effectively stirring and mixing the electrolyte. At the same time, stirring in opposite directions can eliminate dead corners in the electrolytic cell, prevent the electrolyte from accumulating or forming clumps in local areas, accelerate the mass transfer process in the electrolyte, make the anodic oxidation reaction more rapid and uniform, and further improve the anodic oxidation efficiency.

[0014] Preferably, the temperature control device is an arc-shaped temperature control rod consisting of two U-shaped tubes surrounding the stirring rotor and an intermediate tube connecting the two U-shaped tubes.

[0015] By adopting the above technical solution, the U-shaped tube surrounding the stirring rotor can evenly distribute heat as the rotor rotates, ensuring a uniform and stable electrolyte temperature. The combination of the U-shaped tube and the intermediate tube forms a continuous temperature control path, increasing the contact area with the electrolyte and thus improving heat exchange efficiency, further enhancing the anodizing efficiency. The combination of the bow-shaped temperature control rod and the stirring rotor significantly improves the performance and reliability of the anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes through advantages such as precise temperature control, efficient heat exchange, enhanced stirring effect, and simplified structure and maintenance.

[0016] Preferably, the electrolytic cell body is made of polytetrafluoroethylene.

[0017] By adopting the above technical solution, in the process of preparing titanium dioxide nanotubes, the selected electrolyte contains fluoride ions. Fluoride ions will corrode the glass and metal tanks through chemical reactions, resulting in a decrease in their mechanical strength and surface quality. Therefore, polytetrafluoroethylene material is selected to ensure the long-term stable operation of the electrolytic cell.

[0018] Preferably, the system further includes conductive rods disposed inside the electrolytic cell body. These conductive rods include cathode conductive rods disposed on both sides of the electrolytic cell body and anode conductive rods disposed in the middle of the electrolytic cell body. The cathode conductive rods are arranged parallel to the anode conductive rods and parallel to the sides and bottom surface of the electrolytic cell body. Cathode electrode plates perpendicular to the bottom surface of the electrolytic cell body are disposed on the two cathode conductive rods. The cathode electrode plates are detachably disposed from the cathode conductive rods.

[0019] By adopting the above technical solution, the cathode conductive rods are located on both sides of the electrolytic cell, while the anode conductive rods are located in the middle. This layout ensures a more uniform current density distribution within the electrolytic cell, thereby improving the efficiency and uniformity of the electrolysis process. The detachable design of the cathode electrode plates and cathode conductive rods not only facilitates installation and maintenance but also provides greater flexibility. This design allows the electrode plates to be quickly replaced or adjusted according to actual needs to adapt to different electrolysis conditions and requirements. Simultaneously, the detachable cathode electrode plate design simplifies daily cleaning and maintenance. When the electrode plates show wear or require cleaning, they can be easily disassembled and replaced, reducing downtime and maintenance costs. The optimized electric field distribution and adjustable electrode plate design work together to significantly improve electrolysis efficiency, thereby increasing the yield of titanium dioxide nanotubes. The uniform electric field reduces side reactions during the electrolysis process, improves current efficiency, and allows more electrical energy to be effectively converted into chemical energy.

[0020] Preferably, conductive rails parallel to the front and rear sides of the electrolytic cell are provided at both ends of the conductive rod. The conductive rails are slidably disposed with the cathode conductive rod, and the two cathode conductive rods are driven to move toward or away from the anode conductive rod by a second driving member disposed on the conductive rail.

[0021] By adopting the above technical solution, the electrolyte concentration and conductivity will change during the preparation process. By adjusting the electrode spacing, it can be adapted to electrolytic cells of different sizes or different electrolysis tasks. This flexibility improves the utilization rate of the equipment, enabling it to adapt to more types of electrolysis needs, while ensuring the uniformity of the electric field distribution, thereby improving electrolysis efficiency and product quality.

[0022] Preferably, a drain outlet is provided on the rear side of the electrolytic cell body, and the drain outlet is located at the middle position of the bottom rear side of the electrolytic cell body.

[0023] By adopting the above technical solution, after the preparation is completed and the electrolyte is used up, the waste liquid is discharged from the electrolytic cell. At this time, the drain port is opened to discharge the waste liquid from the electrolytic cell, simplifying the waste liquid treatment process and improving work efficiency. Since the drain port is located in the middle of the bottom, waste liquid and sediment at the bottom of the cell can be discharged more effectively, reducing the impact of residues on subsequent electrolysis processes. Setting the drain port at the rear of the electrolytic cell makes reasonable use of space, avoids conflicts with other equipment or pipelines, and makes the overall layout more compact and reasonable.

[0024] Preferably, the cover plate and the electrolytic cell body are movably disposed, and a sealing ring is provided on the side of the cover plate that abuts against the electrolytic cell body, thereby sealing the electrolytic cell body through the sealing ring.

[0025] By adopting the above technical solution, the movable design of the cover plate simplifies the opening and closing of the electrolytic cell, facilitating internal cleaning, maintenance, and repair by staff. It also makes it easier to add and remove electrolytic materials. The sealing ring ensures a good seal between the cover plate and the electrolytic cell when closed, preventing electrolyte leakage and ensuring the safety and stability of the electrolysis process. Furthermore, the good seal prevents the electrolyte from absorbing water and altering its conductivity, thereby improving the anodizing effect.

[0026] Preferably, the cover plate is made of a transparent material.

[0027] By adopting the above technical solution, the transparent cover allows operators to observe the reaction in the electrolytic cell in real time without opening the cover, which helps to identify problems and adjust parameters in a timely manner, ensuring the smooth progress of the preparation process.

[0028] In summary, this application includes at least one of the following beneficial technical effects:

[0029] 1. The addition of a stirring element ensures a more uniform electrolyte solution, preventing concentration gradients and improving electrolysis efficiency. Simultaneously, the temperature control element precisely regulates the temperature within the electrolytic cell, preventing temperature fluctuations caused by electrolyte components absorbing moisture from the air, further guaranteeing electrolysis stability and efficiency. This allows for the production of more uniform and high-quality titanium dioxide nanotubes. A stable electrolysis environment and temperature control contribute to nanotube formation and growth, thereby improving product performance and reliability. The cover plate prevents electrolyte splashing, protecting operators from chemical hazards, and also prevents the electrolyte from absorbing water and altering conductivity. Furthermore, the automated control of the temperature control and stirring elements reduces the complexity and risk of manual operation, thereby enhancing the anodizing efficiency and oxidation effect of titanium dioxide nanotubes.

[0030] 2. The bow-shaped temperature control rod and the stirring rotor work together to achieve precise control of electrolyte temperature and uniform mixing, avoiding abnormal nanotube array morphology caused by temperature fluctuations or concentration gradients.

[0031] 3. The adjustable-spacing dual-pair electrode system reduces edge effects and improves the regularity and uniformity of nanotube arrays on columnar or other non-planar substrates by optimizing the electric field distribution. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of an anodic oxidation electrolytic cell structure prepared from titanium dioxide nanotubes according to this application.

[0033] Figure 2 This is a cross-sectional view of this application.

[0034] Explanation of reference numerals in the attached drawings: 1. Base; 11. Support plate; 12. Support leg; 2. Electrolytic cell body; 3. Stirring component; 31. First driving component; 32. Stirring rotor; 4. Temperature control component; 41. Temperature control rod; 5. Cover; 51. Sealing ring; 6. Conductive rod; 61. Cathode conductive rod; 611. Cathode electrode plate; 62. Anode conductive rod; 63. Conductive slide rail. Detailed Implementation

[0035] The following is in conjunction with the appendix Figure 1-2 This application will be described in further detail.

[0036] The inventors of this application discovered that, in order to obtain nanotube arrays with controllable and regular morphology, they are typically prepared in organic electrolytes. However, current organic electrolytes easily absorb moisture from the air, which affects their conductivity. Furthermore, this process is heat-generating, and temperature changes also affect the array. Therefore, this application primarily employs an anodic oxidation electrolytic cell, including a cell base, cell body, stirring components, temperature control components, and a cover plate, etc., achieving the goals of solving the electrolyte water absorption problem, precisely controlling the temperature, and optimizing the electric field distribution, thereby significantly improving the quality and efficiency of titanium dioxide nanotube preparation.

[0037] This application discloses an anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes. (Refer to...) Figure 1 , Figure 2 The anodic oxidation electrolytic cell fabricated from titanium dioxide nanotubes includes a base 1, an electrolytic cell body 2, a stirrer 3, a temperature controller 4, and a transparent cover 5. The stirrer 3 and temperature controller 4 are located at the bottom of the cell, while the top is fitted with a movable transparent cover 5 equipped with a sealing ring 51. This design effectively avoids the problem of electrolyte hygroscopicity, achieves precise temperature control, and improves the uniformity of the electric field distribution.

[0038] Reference Figure 2 Specifically, the base 1 includes a support plate 11 and a support leg 12 located below the support plate 11.

[0039] The electrolytic cell body 2 is made of polytetrafluoroethylene (PTFE), a material with excellent corrosion resistance. Compared to glass or metal, this material is more suitable for long-term exposure to environments containing fluoride ions. PTFE does not suffer damage to its mechanical strength or surface integrity due to chemical reactions, thus ensuring stable operation of the equipment over a long period. A drain port is located at the bottom rear of the electrolytic cell body 2. After preparation is completed, the waste liquid is discharged from the electrolytic cell through the drain port.

[0040] The stirring component 3 includes two stirring rotors 32 arranged equidistantly along a center line and driven to rotate by an external first driving component 31. The first driving component 31 is a motor, located below the base 1. One or two motors can be used. When only one first driving component 31 is used, a gear transmission assembly is provided at the output shaft of the first driving component 31, which drives the stirring rotors 32 to rotate. When two first driving components 31 are used, they are connected to the two stirring rotors 32 respectively.

[0041] The two rotors rotate in opposite directions, creating a strong and uniform liquid flow pattern, effectively eliminating the local dead zones that may occur with traditional unidirectional stirring. This bidirectional stirring mechanism not only promotes thorough mixing of the electrolyte components but also enhances heat dissipation, creating favorable conditions for maintaining a constant temperature environment.

[0042] The temperature control element 4 is an arc-shaped temperature control rod 41, consisting of two U-shaped tubes surrounding the stirring rotor 32 and an intermediate connecting tube between them. This unique structure greatly expands the actual surface area in contact with the electrolyte, making the heat transfer process more efficient and stable. During system operation, the continuous disturbance brought about by the stirring action further enhances the energy exchange rate, thereby ensuring that the process parameters are always kept within the ideal range.

[0043] The lid, consisting of five parts, is made of polycarbonate material that combines strength and light transmittance, and is equipped with a flexible sealing rubber ring to enhance airtightness when closed. On the one hand, its excellent optical transmittance allows operators to directly observe internal dynamic changes without frequent opening and closing; on the other hand, its tight-fitting design successfully prevents external moisture intrusion, completely eliminating any adverse effects.

[0044] It also includes conductive rods 6, which include cathode conductive rods 61 and anode conductive rods 62. The cathode conductive rods 61 are arranged in two positions on both sides of the anode conductive rods 62 and are parallel to the sides and bottom of the electrolytic cell body 2. Two parallel conductive slide rails 63 are arranged on the front and rear sides inside the cell body. The conductive slide rails 63 are located at both ends of the conductive rods 6 and are driven by a second driving component to move the cathode conductive rods 61 toward or away from the anode conductive rods 62. The second driving component can be a bidirectional lead screw or a hydraulic cylinder. By changing the distance between the cathode conductive rods 61 and the anode conductive rods 62, the electric field distribution of the electrode system is optimized, and finally, the efficient preparation of high-quality titanium dioxide nanotube arrays is achieved.

[0045] Two cathode conductive rods 61 have cathode electrode plates 611 fixedly mounted at their lower ends, perpendicular to the bottom surface of the tank. The cathode electrode plates 611 and the cathode conductive rods 61 are connected in a modular, detachable manner, allowing for flexible adjustment or replacement according to different experimental needs. The anode conductive rod 62 supports the titanium substrate sample to be processed. Both the cathode conductive rods 61 and the anode conductive rod 62 are connected to an external power source to ensure stable and reliable current transmission.

[0046] The implementation principle of the anodic oxidation electrolytic cell for preparing titanium dioxide nanotubes in this application embodiment is as follows: The stirring element 3 ensures a more uniform electrolyte, preventing concentration gradients and thus improving electrolysis efficiency. Simultaneously, the temperature control element 4 precisely controls the temperature within the electrolytic cell, preventing temperature changes caused by the absorption of moisture from the air by the electrolyte components, further ensuring the stability and efficiency of electrolysis. This allows for the preparation of more uniform and high-quality titanium dioxide nanotubes. A stable electrolysis environment and temperature control contribute to the formation and growth of nanotubes, thereby improving product performance and reliability. The cover plate prevents electrolyte splashing, protecting operators from chemical hazards, and also prevents the electrolyte from absorbing water and altering conductivity. Furthermore, the automated control of the temperature control element 4 and the stirring element 3 reduces the complexity and risk of manual operation, thereby improving the anodic oxidation efficiency and effect of titanium dioxide nanotubes.

[0047] The above are all preferred embodiments of this application and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. An anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes, characterized in that: An electrolytic cell base (1) is provided, and an electrolytic cell body (2) is fixedly installed on the top of the electrolytic cell base (1). A stirring component (3) and a temperature control component (4) are provided at the bottom of the electrolytic cell body (2). A cover plate is provided on the top of the electrolytic cell body (2).

2. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 1, characterized in that: The stirring element (3) consists of two stirring rotors (32) arranged at equal intervals. A first driving element (31) is provided below the electrolytic cell base (1). The output shaft of the first driving element (31) passes through the electrolytic cell base (1) and is connected to the stirring rotor (32).

3. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 2, characterized in that: The two stirring rotors (32) rotate in opposite directions.

4. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 3, characterized in that: The temperature control element (4) is an arc-shaped temperature control rod (41) consisting of two U-shaped tubes surrounding the stirring rotor (32) and an intermediate tube connecting the two U-shaped tubes.

5. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 1, characterized in that: The electrolytic cell body (2) is made of polytetrafluoroethylene.

6. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 1, characterized in that: It also includes conductive rods (6), which are disposed inside the electrolytic cell body (2). The conductive rods (6) include cathode conductive rods (61) disposed on both sides of the electrolytic cell body (2) and anode conductive rods (62) disposed in the middle of the electrolytic cell body (2). The cathode conductive rods (61) and anode conductive rods (62) are disposed parallel to each other and parallel to the sides and bottom of the electrolytic cell body (2). Cathode electrode plates (611) perpendicular to the bottom of the electrolytic cell body (2) are disposed on the two cathode conductive rods (61). The cathode electrode plates (611) and cathode conductive rods (61) are detachably disposed.

7. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 6, characterized in that: The conductive rod (6) is also provided with conductive slide rails (63) at both ends, which are parallel to the front and rear sides of the electrolytic cell body (2). The conductive slide rails (63) are slidably disposed with the cathode conductive rod (61), and the two cathode conductive rods (61) are driven to move toward or away from the anode conductive rod (62) by a second driving member disposed on the conductive slide rails (63).

8. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 1, characterized in that: The electrolytic cell body (2) has a drain outlet on the rear side, which is located at the middle of the bottom of the rear side of the electrolytic cell body (2).

9. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 1, characterized in that: The cover plate is movably disposed from the electrolytic cell body (2). A sealing ring (51) is provided on the side of the cover plate that abuts against the electrolytic cell body (2), and the electrolytic cell body (2) is sealed by the sealing ring (51).

10. The anodic oxidation electrolytic cell prepared from titanium dioxide nanotubes according to claim 9, characterized in that: The cover plate is made of a transparent material.

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