CN116288598A - Device and method for preparing uranium film on tubular outer wall by electroplating method - Google Patents
Device and method for preparing uranium film on tubular outer wall by electroplating method Download PDFInfo
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- CN116288598A CN116288598A CN202310097257.2A CN202310097257A CN116288598A CN 116288598 A CN116288598 A CN 116288598A CN 202310097257 A CN202310097257 A CN 202310097257A CN 116288598 A CN116288598 A CN 116288598A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/04—Tubes; Rings; Hollow bodies
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The application relates to the technical field of uranium film preparation, in particular to a device and a method for preparing a tubular outer wall uranium film by an electroplating method, wherein the device comprises a base, a ball screw device, an anode fixing rod, a water bath and a direct-current stabilized power supply, and the device comprises the following components: the water bath is fixed on the base, and an electroplating bath is arranged in the water bath; the ball screw device is fixed on the base and is arranged at one side of the water bath; the anode fixing rod is connected with the ball screw device and can slide up and down through the ball screw device; the direct current stabilized power supply is used for providing direct current required by electroplating for the electroplating bath. The method uses the absolute ethyl alcohol as the electroplating solution, improves and optimizes the electroplating efficiency and the quality of the coating film by adjusting the conditions such as the cathode treatment process, the pH value of the electroplating solution, the current density, the electroplating time, the concentration of uranyl ions in the electroplating solution and the like, has the advantages of simple operation and convenient use, has strong bonding force with the surface of a base material, is easy to control the conditions, and can be used for uranium plating on the upper surface of the base body with different specifications and sizes.
Description
Technical Field
The application relates to the technical field of uranium film preparation, in particular to a device and a method for preparing a tubular outer wall uranium film by utilizing an electroplating method.
Background
Uranium (U) is an important natural sourceThe presence of the actinide of jettance, wherein, the liquid crystal display device comprises a liquid crystal display device, 235 the low-energy neutron fission section of the U isotope is larger, and the energy generated by the nuclear fission reaction is large, so that the U isotope is mainly used as a nuclear fuel in the nuclear reaction and is also one of main fissionable materials for manufacturing a fission ionization chamber detector.
The fission ionization chamber detector has higher n-gamma discrimination capability and can be widely applied to the fields of nuclear reaction data measurement, reactor neutron flux monitoring, nuclear fusion research, medical accelerator monitoring and the like. Fission ionization chamber electrodes are key components of neutron detectors, with surfaces coated with high enrichment 235 U (abundance of 90% or more), is generally required 235 The U-shaped membrane has large area, uniform membrane layer and controllable thickness, and the manufacturing process level directly influences key performances such as sensitivity of the fission ionization chamber.
The electroplating method has the advantages of high deposition efficiency, uniform and firm plating layer, simple equipment, easy control of conditions, uniform deposition on a substrate with a complex structure and the like, and is widely applied to the aspect of preparing films from actinides at present. In the electroplating method, an organic solvent is used as an electrolyte carrier, and a relatively stable electric field is formed by applying voltage. Uranyl ions in solvent
And under the action of an electric field, migrating to the cathode and depositing on the surface of the cathode plating piece to form a film. />
The density, firmness, uniformity and deposition quality of the electrodeposit are closely related to the parameters of the electroplating process (such as current density, deposition time, solvent pH value, etc.). However, the uranium deposition amount prepared by the current electroplating method is limited, and the film thickness is generally 1mg/cm 2 On the left and right sides, the deposition thickness internal stress is large, easy to crack and fall off, and the device and the method are not used for the film coating of the tubular outer wall of the ionization chamber electrode, which clearly limit the application range and the neutron detection efficiency of the fission ionization chamber detector. Therefore, the determination of optimal plating process conditions, the mass thickness of uranium electrode plating and the increase of the area of the fission sensitive area of the ionization chamber electrode are key works.
Disclosure of Invention
The application provides a device and a method for preparing a uranium film on a tubular outer wall by an electroplating method, wherein an anodic oxidation treatment method is adopted to pretreat a piece to be plated, an oxide film with a certain thickness and a special structure is formed on the surface of the piece to be plated, and the binding force of the uranium film and a pipe is improved.
In order to achieve the above-mentioned purpose, the application provides a utilize device of electroplating process preparation tubulose outer wall uranium film, including base, ball screw device, positive pole dead lever, water bath and DC regulated power supply, wherein: the water bath is fixed on the base, and an electroplating bath is arranged in the water bath; the ball screw device is fixed on the base and is arranged at one side of the water bath; the anode fixing rod is connected with the ball screw device and can slide up and down through the ball screw device; the direct current stabilized power supply is used for providing direct current required by electroplating for the electroplating bath.
Further, be provided with negative pole in the plating bath and wait that aluminize alloy pipe, positive pole spring platinum silk and seal structure, wherein: the anode spring platinum wire is arranged around the cathode to-be-aluminized alloy tube; the sealing structure comprises a sealing pressing block, a rubber gasket and a double-head threaded rod; the sealing press blocks are arranged at the upper end and the lower end of the cathode to-be-aluminized alloy pipe, the rubber gasket is arranged between the sealing press blocks and the cathode to-be-aluminized alloy pipe, and the double-headed threaded rod is connected with the sealing press blocks at the upper end of the cathode to-be-aluminized alloy pipe; the side wall of the bottom of the electroplating bath is provided with an electroplating liquid outlet.
Further, the positive pole of the direct current stabilized voltage supply is connected with an anode spring platinum wire through an anode wire, and the negative pole is connected with a double-head threaded rod through a cathode wire.
Further, the ball screw device includes step motor, ball screw supporting seat, ball screw, linear guide and ball screw slip table, wherein: the ball screw supporting seat is connected with the base through a fixed plate; the ball screw and the linear guide rail are fixed on the ball screw supporting seat; the stepping motor is fixed on the base and connected with the ball screw; the ball screw sliding table passes through the ball screw and is connected with the linear guide rail, and the ball screw sliding table slides up and down along the linear guide rail through the rotation of the ball screw; limit switches are arranged at the upper end and the lower end of the linear guide rail; the anode fixing rod is fixed in the middle of the ball screw sliding table.
Further, an anode wire through hole is arranged in the middle of the anode fixing rod.
Further, the plating tank is made of polytetrafluoroethylene.
In addition, the application also provides a method for applying the device for preparing the uranium film on the tubular outer wall by using the electroplating method, which comprises the following steps: step 1: preparing uranium-containing electroplating solution, taking an absolute ethyl alcohol organic solution containing uranyl nitrate as the electroplating solution, and adjusting the pH value of the electroplating solution; step 2: preparing a pretreatment electroplating solution and an activating solution, weighing phosphorous acid solid, adding the phosphorous acid solid into distilled water to prepare the pretreatment electroplating solution, and diluting an HF solution to obtain the activating solution; step 3: pretreating the outer wall of the alloy tube to be aluminized by adopting the pretreatment electroplating solution and the activation solution in the step 2; step 4: and (2) placing the uranium-containing electroplating solution in the step (1) into an electroplating bath, taking the to-be-aluminized alloy tube as a cathode, taking an anode spring platinum wire as an anode, and electroplating uranium, so that a uranium-containing coating film is formed on the outer wall surface of the to-be-aluminized alloy tube.
Further, in the step 3, when the outer wall of the alloy to be aluminized is pretreated, the following steps are adopted: step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall; step 3.2: cleaning by adopting HCl to remove oxide impurities on the surface of the pipe wall; step 3.3: performing anodic oxidation treatment by pretreating the electroplating solution; step 3.4: activating the to-be-aluminized alloy tube subjected to anodic oxidation treatment by adopting an activating solution, and forming an oxide film on the surface of the outer wall; step 3.5: distilled water is used for flushing.
The device and the method for preparing the uranium film on the tubular outer wall by using the electroplating method provided by the invention have the following beneficial effects:
the application uses absolute ethyl alcohol as the electroplating solution, and improves and optimizes the electroplating efficiency and the quality of the coating film by adjusting the conditions of a cathode treatment process, the pH value of the plating solution, the current density, the electroplating time, the concentration of uranyl ions in the plating solution and the likeThe efficiency is up to more than 90%, and the film thickness is even and can reach 6mg/cm 2 The bonding force with the surface of the substrate is strong, the conditions are easy to control, and the method can be used for uranium plating on the upper surfaces of substrates with different specifications and sizes.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, are included to provide a further understanding of the application and to provide a further understanding of the application with regard to the other features, objects and advantages of the application. The drawings of the illustrative embodiments of the present application and their descriptions are for the purpose of illustrating the present application and are not to be construed as unduly limiting the present application. In the drawings:
FIG. 1 is a schematic cross-sectional view of an apparatus for preparing a tubular outer wall uranium film using an electroplating method according to an embodiment of the present application;
fig. 2 is a schematic structural view of an apparatus for preparing a uranium film on a tubular outer wall by electroplating according to an embodiment of the present application;
FIG. 3 is a process diagram of steps for preparing a tubular outer wall uranium film according to an embodiment of the present application;
in the figure: the plating equipment comprises a plating tank 1, a plating tank 2, a cathode alloy pipe to be plated with aluminum, a spring platinum wire 3, a water bath 4, a direct current stabilized voltage supply 5, a stepping motor 6, a ball screw sliding table 7, a linear guide rail 8, an anode fixing rod 9, a double-headed threaded rod 10, a sealing pressing block 11, an anode lead 12, a ball screw supporting seat 13, an electroplating liquid outlet 14, a base 15, a cathode lead 16, a limit switch 17 and a through hole 18.
Detailed Description
In order to make the present application solution better understood by those skilled in the art, the following description will be made in detail and with reference to the accompanying drawings in the embodiments of the present application, it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate in order to describe the embodiments of the present application described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In the present application, the terms "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal" and the like indicate an azimuth or a positional relationship based on that shown in the drawings. These terms are used primarily to better describe the present application and its embodiments and are not intended to limit the indicated device, element or component to a particular orientation or to be constructed and operated in a particular orientation.
Also, some of the terms described above may be used to indicate other meanings in addition to orientation or positional relationships, for example, the term "upper" may also be used to indicate some sort of attachment or connection in some cases. The specific meaning of these terms in this application will be understood by those of ordinary skill in the art as appropriate.
In addition, the term "plurality" shall mean two as well as more than two.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As shown in fig. 1-2, the application provides a device for preparing a uranium film with a tubular outer wall by using an electroplating method, which comprises a base 15, a ball screw device, an anode fixing rod 9, a water bath 4 and a direct current stabilized power supply 5, wherein: the water bath 4 is fixed on the base 15, and the electroplating bath 1 is arranged inside; the ball screw device is fixed on the base 15 and is arranged on one side of the water bath 4; the anode fixing rod 9 is connected with a ball screw device, and can slide up and down through the ball screw device; the dc stabilized power supply 5 is used to supply dc current required for plating to the plating tank 1.
In particular, due to 238 U and 235 u belongs to isotope, has similar chemical properties and is relatively cheap and easily obtained, so the embodiment of the application utilizes 238 U substitution 235 And U, carrying out research on electroplating devices and processes on the outer wall surface of the tubular aluminum alloy, and systematically inspecting influence of current density, electroplating time, pH value, polar distance and surface treatment process of a plated part on electroplating efficiency and plating quality. In the embodiment of the present application, the base 15 mainly plays a role of a fixed support; the water bath 4 is used for placing distilled water and cooling heat generated by the plating solution in the electroplating process; the electroplating bath 1 is arranged in the water bath 4 and is used for electroplating uranium; the ball screw device is arranged on the side surface of the water bath tank 4, and the anode fixing rod 9 is fixed on the ball screw device and can slide up and down under the drive of the ball screw device, so that the anode spring platinum wire 3 in the electroplating tank 1 is driven to move up and down; the dc regulated power supply 5 is connected to the anode lead 12 and the cathode lead 16 for supplying a stable dc current.
Further, be provided with negative pole in plating bath 1 wait that aluminizing alloy pipe 2, positive pole spring platinum silk 3 and seal structure, wherein: the anode spring platinum wire 3 is arranged around the cathode alloy tube 2 to be aluminized; the sealing structure comprises a sealing pressing block 11, a rubber gasket and a double-head threaded rod 10; the sealing press blocks 11 are arranged at the upper end and the lower end of the cathode to-be-aluminized alloy pipe 2, the rubber gaskets are arranged between the sealing press blocks 11 and the cathode to-be-aluminized alloy pipe 2, and the double-headed threaded rod 10 is connected with the sealing press blocks 11 at the upper end of the cathode to-be-aluminized alloy; the bottom side wall of the plating tank 1 is provided with a plating solution outlet 14. The cathode to-be-plated aluminum alloy tube 2 is used as a cathode in an electroplating process, after electroplating is finished, uranium-containing plating layers are formed on the surface, sealing pressing blocks 11 and rubber gaskets are arranged at the upper end and the lower end of the cathode to-be-plated aluminum alloy tube 2, a double-head threaded rod 10 is arranged at the upper end sealing block, fastening sealing of the cathode to-be-plated aluminum alloy tube 2 is achieved, and a cathode lead 16 is connected with the cathode to-be-plated aluminum alloy tube 2 through the double-head threaded rod 10. The anode spring platinum wire 3 is used as an anode in the electroplating process, is arranged around the cathode to-be-aluminized alloy tube 2, and is sleeved in the middle of the cathode to-be-aluminized alloy tube 2, and the anode spring platinum wire 3 is connected with the anode lead 12.
Further, the positive electrode of the direct current stabilized voltage power supply 5 is connected with the anode spring platinum wire 3 through the anode wire 12, and the negative electrode is connected with the double-head threaded rod 10 through the cathode wire 16, so as to provide stable direct current for electroplating, and the current magnitude and the duration of current supply can be adjusted according to actual electroplating conditions.
Further, the ball screw device includes step motor 6, ball screw supporting seat 13, ball screw, linear guide 8 and ball screw slip table 7, wherein: the ball screw supporting seat 13 is connected with the base 15 through a fixed plate; the ball screw and the linear guide rail 8 are fixed on the ball screw supporting seat 13; the stepping motor 6 is fixed on the base 15 and is connected with the ball screw; the ball screw sliding table 7 penetrates through the ball screw and is connected with the linear guide rail 8, and the ball screw sliding table 7 slides up and down along the linear guide rail 8 through rotation of the ball screw; limit switches 17 are arranged at the upper end and the lower end of the linear guide rail 8; the anode fixing rod 9 is fixed in the middle of the ball screw sliding table 7. The ball screw supporting seat 13 is mainly used for fixedly supporting the ball screw and the linear guide rail 8, the stepping motor 6 drives the ball screw to rotate, the ball screw sliding table 7 on the ball screw can slide up and down along the linear guide rail 8 under the action of the rotation of the ball screw, so that the anode fixing rod 9 on the ball screw sliding table 7 is driven to slide up and down, the upper end and the lower end of the linear guide rail 8 are provided with the high-sensitivity induction limit switch 17 for limiting the range interval of the upper and lower sliding of the ball screw sliding table 7, and the specific positions of the upper limit switch 17 and the lower limit switch 17 are set according to the height of the alloy tube 2 to be aluminized by the cathode.
Further, an anode wire through hole 18 is provided in the middle of the anode fixing rod 9. The anode wire through hole 18 in the middle of the anode fixing rod 9 is used for the anode wire 12 to pass through, the positive electrode of the direct current stabilized power supply 5 is connected with the anode wire 12, the anode wire 12 passes through the anode wire through hole 18 to be connected with the anode spring platinum wire 3 in the electroplating bath 1, and the anode spring platinum wire 3 can be driven to reciprocate up and down along with the up and down sliding of the anode fixing rod 9. The anode spring platinum wire 3 moves up and down at a uniform speed, so as to provide a path for electroplating scanning, the electroplating area is not limited to the area covered by the anode spring platinum wire 3, large-area scanning electroplating can be realized according to actual conditions, and the anode spring platinum wire 3 moves up and down at a uniform speed for scanning electroplating, so that the anode spring platinum wire has more uniform current density and good liquid phase mass transfer effect.
Further, the plating tank 1 is made of polytetrafluoroethylene. The polytetrafluoroethylene has the characteristics of heat resistance, acid resistance, alkali resistance and organic solvent resistance, is insoluble in absolute ethyl alcohol, avoids introducing impurities, has excellent electrical insulation, and is not afraid of contacting with an anode spring platinum wire 3 in the electroplating process, so that a circuit is short-circuited or an electric field line is changed.
In addition, as shown in fig. 3, the embodiment of the application also provides a method for applying the device for preparing the uranium film with the tubular outer wall by using the electroplating method, which comprises the following steps: step 1: preparing uranium-containing electroplating solution, taking an absolute ethyl alcohol organic solution containing uranyl nitrate as the electroplating solution, and adjusting the pH value of the electroplating solution; step 2: preparing a pretreatment electroplating solution and an activating solution, weighing phosphorous acid solid, adding the phosphorous acid solid into distilled water to prepare the pretreatment electroplating solution, and diluting an HF solution to obtain the activating solution; step 3: pretreating the outer wall of the alloy tube to be aluminized by adopting the pretreatment electroplating solution and the activation solution in the step 2; step 4: and (3) putting the uranium-containing electroplating solution in the step (1) into an electroplating bath (1), and electroplating uranium by taking the to-be-aluminized alloy tube as a cathode and taking the anode spring platinum wire (3) as an anode, so that a uranium-containing coating film is formed on the outer wall surface of the to-be-aluminized alloy tube.
Further, in the step 3, when the outer wall of the alloy to be aluminized is pretreated, the following steps are adopted: step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall; step 3.2: cleaning by adopting HCl to remove oxide impurities on the surface of the pipe wall; step 3.3: performing anodic oxidation treatment by pretreating the electroplating solution; step 3.4: activating the to-be-aluminized alloy tube subjected to anodic oxidation treatment by adopting an activating solution, and forming an oxide film on the surface of the outer wall; step 3.5: distilled water is used for flushing.
Specifically, the method for applying the device for preparing the uranium film on the tubular outer wall by using the electroplating method provided by the embodiment of the application is that the electroplating solution is an absolute ethyl alcohol organic system, and in order to maintain that uranium in the electroplating solution mainly exists in the form of uranyl ions
Proper amount of hydrochloric acid is required to be added to the plating solution.
Since the standard reduction potential sequence of uranium (U) and hydrogen (H) is:
therefore, U (VI) has a weaker electron-withdrawing ability than hydrogen ions, which preferentially precipitate in large amounts on the cathode, uranyl ions
It is difficult to deposit in metallic form from solution on the cathode, but in low valence form (UO) in the appropriate pH range 2 , +4), hydrolysate (UO 2 (OH) 2 ) Or->
Is deposited on the outer wall surface of the aluminum alloy pipe.
The reactions that occur at the cathode during electroplating are:
2H + +2e＝H 2 ∈ (side reaction)
2H 2 O+2e＝2OH - +H 2 ∈ (side reaction)
The method of the present application using an apparatus for preparing a uranium film on a tubular outer wall by electroplating is further described below with reference to specific examples:
example 1
Step 1: preparing uranium-containing electroplating solution, weighing a certain amount of uranyl nitrate (UO) 2 (NO 3 ) 2 ) Adding the solid into absolute ethyl alcohol to prepare uranium-containing solution with the concentration of about 5mg/mL, and adjusting the pH of the solution to 2-3;
step 2: preparing a pretreated plating solution and an activating solution, and weighing a certain amount of phosphorous acid (H) 3 PO 3 ) Adding the solid into distilled water to prepare 30-50% of H 3 PO 3 A solution (pretreatment plating solution) in which the HF solution is diluted to a diluted HF solution (activation solution) of 0.5 to 1%;
step 3: the pretreatment electroplating solution and the activation solution in the step 2 are adopted to pretreat the outer wall of the alloy tube to be aluminized:
step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall;
step 3.2: cleaning by adopting HCl with the concentration of 1mol/L to remove oxide impurities on the surface of the pipe wall;
step 3.3: by 30% -50% H 3 PO 3 Solution (pretreatment plating solution) solution is subjected to anodic oxidation treatment;
step 3.4: activating the anodized alloy tube to be plated with aluminum by using 0.5-1% of HF activating solution, forming an oxide film with a certain thickness and a special structure on the surface of the outer wall, and improving the binding force of the uranium plating film;
step 3.5: distilled water is used for flushing.
Step 4: the uranium-containing electroplating solution in the step 1 is put into an electroplating bath 1, the liquid level is over an alloy pipe to be plated, the alloy pipe to be plated is taken as a cathode, an anode spring platinum wire 3 is taken as an anode, electroplating of uranium is carried out, a ball screw sliding device module is opened, the rotating speed of a stepping motor 6 is regulated, a ball screw sliding table 7 drives the anode spring platinum wire 3 to slide up and down at a constant speed along a linear guide rail 8, the speed is kept to be 0.5cm/s, heat generated in the electroplating process is reduced by adopting a water bath cooling mode, a direct-current stabilized power supply 5 is connected, and electroplating treatment is carried out for 1h by maintaining current of 60mA, so that a uranium-containing coating film is formed on the outer wall surface of the alloy pipe to be plated.
Determining the concentration of uranium in a uranium-containing coating film formed on the outer wall surface of an alloy pipe to be aluminized by adopting an ultraviolet spectrophotometry, and determining that the electroplating efficiency is 90% and the coating film thickness is 6mg/cm by calculation 2 。
Example 2
Step 1: preparing uranium-containing electroplating solution, weighing a certain amount of uranyl nitrate (UO) 2 (NO 3 ) 2 ) Adding the solid into absolute ethyl alcohol to prepare uranium-containing solution with the concentration of about 5mg/mL, and adjusting the pH of the solution to 2-3;
step 2: preparing a pretreated plating solution and an activating solution, and weighing a certain amount of phosphorous acid (H) 3 PO 3 ) Adding the solid into distilled water to prepare 30-50% of H 3 PO 3 A solution (pretreatment plating solution) in which the HF solution is diluted to a diluted HF solution (activation solution) of 0.5 to 1%;
step 3: the pretreatment electroplating solution and the activation solution in the step 2 are adopted to pretreat the outer wall of the alloy tube to be aluminized:
step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall;
step 3.2: cleaning by adopting HCl with the concentration of 1mol/L to remove oxide impurities on the surface of the pipe wall;
step 3.3: by 30% -50% H 3 PO 3 Solution (pretreatment plating solution) solution is subjected to anodic oxidation treatment;
step 3.4: activating the anodized alloy tube to be plated with aluminum by using 0.5-1% of HF activating solution, forming an oxide film with a certain thickness and a special structure on the surface of the outer wall, and improving the binding force of the uranium plating film;
step 3.5: distilled water is used for flushing.
Step 4: the uranium-containing electroplating solution in the step 1 is put into an electroplating bath 1, the liquid level is over an alloy pipe to be plated, the alloy pipe to be plated is taken as a cathode, an anode spring platinum wire 3 is taken as an anode, electroplating of uranium is carried out, a ball screw sliding device module is opened, the rotating speed of a stepping motor 6 is regulated, a ball screw sliding table 7 drives the anode spring platinum wire 3 to slide up and down at a constant speed along a linear guide rail 8, the speed is kept to be 0.5cm/s, heat generated in the electroplating process is reduced by adopting a water bath cooling mode, a direct-current stabilized power supply 5 is connected, and electroplating treatment is carried out for 1h by keeping current of 20mA, so that a uranium-containing coating film is formed on the surface of the outer wall of the alloy pipe to be plated.
Determining the concentration of uranium in a uranium-containing coating film formed on the outer wall surface of an alloy pipe to be aluminized by adopting an ultraviolet spectrophotometry, and determining that the electroplating efficiency is 24% and the thickness of the coating film is 1.5mg/cm by calculation 2 。
Example 3
Step 1: preparing uranium-containing electroplating solution, weighing a certain amount of uranyl nitrate (UO) 2 (NO 3 ) 2 ) Adding the solid into absolute ethyl alcohol to prepare uranium-containing solution with the concentration of about 5mg/mL, and adjusting the pH of the solution to 2-3;
step 2: preparing a pretreated plating solution and an activating solution, and weighing a certain amount of phosphorous acid (H) 3 PO 3 ) Adding the solid into distilled water to prepare 30-50% of H 3 PO 3 A solution (pretreatment plating solution) in which the HF solution is diluted to a diluted HF solution (activation solution) of 0.5 to 1%;
step 3: the pretreatment electroplating solution and the activation solution in the step 2 are adopted to pretreat the outer wall of the alloy tube to be aluminized:
step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall;
step 3.2: cleaning by adopting HCl with the concentration of 1mol/L to remove oxide impurities on the surface of the pipe wall;
step 3.3: by 30% -50% H 3 PO 3 Solution (pretreatment plating solution) solution is subjected to anodic oxidation treatment;
step 3.4: activating the anodized alloy tube to be plated with aluminum by using 0.5-1% of HF activating solution, forming an oxide film with a certain thickness and a special structure on the surface of the outer wall, and improving the binding force of the uranium plating film;
step 3.5: distilled water is used for flushing.
Step 4: the uranium-containing electroplating solution in the step 1 is put into an electroplating bath 1, the liquid level is over an alloy pipe to be plated, the alloy pipe to be plated is taken as a cathode, an anode spring platinum wire 3 is taken as an anode, electroplating of uranium is carried out, a ball screw sliding device module is opened, the rotating speed of a stepping motor 6 is regulated, a ball screw sliding table 7 drives the anode spring platinum wire 3 to slide up and down at a constant speed along a linear guide rail 8, the speed is kept to be 0.5cm/s, heat generated in the electroplating process is reduced by adopting a water bath cooling mode, a direct-current stabilized power supply 5 is connected, and electroplating treatment is carried out for 2 hours by maintaining current of 60mA, so that a uranium-containing coating film is formed on the outer wall surface of the alloy pipe to be plated.
Determining the concentration of uranium in a uranium-containing coating film formed on the outer wall surface of an alloy pipe to be aluminized by adopting an ultraviolet spectrophotometry, and determining that the electroplating efficiency is 92% and the thickness of the coating film is 6.1mg/cm by calculation 2 。
Example 4
Step 1: preparing uranium-containing electroplating solution, weighing a certain amount of uranyl nitrate (UO) 2 (NO 3 ) 2 ) Adding the solid into absolute ethyl alcohol to prepare uranium-containing solution with the concentration of about 10mg/mL, and adjusting the pH of the solution to 2-3;
step 2: preparing a pretreated plating solution and an activating solution, and weighing a certain amount of phosphorous acid (H) 3 PO 3 ) Adding the solid into distilled water to prepare 30-50% of H 3 PO 3 A solution (pretreatment plating solution) in which the HF solution is diluted to a diluted HF solution (activation solution) of 0.5 to 1%;
step 3: the pretreatment electroplating solution and the activation solution in the step 2 are adopted to pretreat the outer wall of the alloy tube to be aluminized:
step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall;
step 3.2: cleaning by adopting HCl with the concentration of 1mol/L to remove oxide impurities on the surface of the pipe wall;
step 3.3: by 30% -50% H 3 PO 3 Solution (pretreatment plating solution) solution is subjected to anodic oxidation treatment;
step 3.4: activating the anodized alloy tube to be plated with aluminum by using 0.5-1% of HF activating solution, forming an oxide film with a certain thickness and a special structure on the surface of the outer wall, and improving the binding force of the uranium plating film;
step 3.5: distilled water is used for flushing.
Step 4: the uranium-containing electroplating solution in the step 1 is put into an electroplating bath 1, the liquid level is over an alloy pipe to be plated, the alloy pipe to be plated is taken as a cathode, an anode spring platinum wire 3 is taken as an anode, electroplating of uranium is carried out, a ball screw sliding device module is opened, the rotating speed of a stepping motor 6 is regulated, a ball screw sliding table 7 drives the anode spring platinum wire 3 to slide up and down at a constant speed along a linear guide rail 8, the speed is kept to be 0.5cm/s, heat generated in the electroplating process is reduced by adopting a water bath cooling mode, a direct-current stabilized power supply 5 is connected, and electroplating treatment is carried out for 1h by maintaining current of 60mA, so that a uranium-containing coating film is formed on the outer wall surface of the alloy pipe to be plated.
Determining the concentration of uranium in a uranium-containing coating film formed on the outer wall surface of an alloy pipe to be aluminized by adopting an ultraviolet spectrophotometry, and determining that the electroplating efficiency is 68% and the coating film thickness is 8.8mg/cm by calculation 2 。
Example 5
Step 1: preparing uranium-containing electroplating solution, weighing a certain amount of uranyl nitrate (UO) 2 (NO 3 ) 2 ) Adding the solid into absolute ethyl alcohol to prepare uranium-containing solution with the concentration of about 5mg/mL, and adjusting the pH of the solution to 4-5;
step 2: preparing a pretreated plating solution and an activating solution, and weighing a certain amount of phosphorous acid (H) 3 PO 3 ) Adding the solid into distilled water to prepare 30-50% of H 3 PO 3 A solution (pretreatment plating solution) in which the HF solution is diluted to a diluted HF solution (activation solution) of 0.5 to 1%;
step 3: the pretreatment electroplating solution and the activation solution in the step 2 are adopted to pretreat the outer wall of the alloy tube to be aluminized:
step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall;
step 3.2: cleaning by adopting HCl with the concentration of 1mol/L to remove oxide impurities on the surface of the pipe wall;
step 3.3: by 30% -50% H 3 PO 3 Solution (pretreatment plating solution) solution is subjected to anodic oxidation treatment;
step 3.4: activating the anodized alloy tube to be plated with aluminum by using 0.5-1% of HF activating solution, forming an oxide film with a certain thickness and a special structure on the surface of the outer wall, and improving the binding force of the uranium plating film;
step 3.5: distilled water is used for flushing.
Step 4: the uranium-containing electroplating solution in the step 1 is put into an electroplating bath 1, the liquid level is over an alloy pipe to be plated, the alloy pipe to be plated is taken as a cathode, an anode spring platinum wire 3 is taken as an anode, electroplating of uranium is carried out, a ball screw sliding device module is opened, the rotating speed of a stepping motor 6 is regulated, a ball screw sliding table 7 drives the anode spring platinum wire 3 to slide up and down at a constant speed along a linear guide rail 8, the speed is kept to be 0.5cm/s, heat generated in the electroplating process is reduced by adopting a water bath cooling mode, a direct-current stabilized power supply 5 is connected, and electroplating treatment is carried out for 1h by maintaining current of 60mA, so that a uranium-containing coating film is formed on the outer wall surface of the alloy pipe to be plated.
Determining the concentration of uranium in a uranium-containing coating film formed on the outer wall surface of an alloy pipe to be aluminized by adopting an ultraviolet spectrophotometry, and determining that the electroplating efficiency is 72% and the thickness of the coating film is 4.8mg/cm by calculation 2 。
In summary, compared with example 1 and example 2, the plating current is different, so that the plating effect is different, the current is small, the cathode polarization effect is small, the plating crystallization is thick, the plating thickness is thin, the cathode polarization effect is increased with the increase of the current, the plating crystal grain is thinner and thinner, and when the current is continuously increased, the plating quality is deteriorated, and the phenomena of scorching and blackening occur, so that the current is controlled between 50mA and 70 mA; compared with the embodiment 1 and the embodiment 3, the electroplating time is different, so that the plating effect is not much, the electroplating time is prolonged, the effect of improving the electroplating efficiency and the plating thickness is not obvious, however, the electroplating time is prolonged, the electroplating heating is obvious, and the quality of a plating layer can be influenced; example 1 and example 4 phasesCompared with the prior art, the concentration of the uranium-containing electroplating solution is different, so that the plating effect is different, the plating efficiency is reduced along with the increase of the concentration of the uranium-containing electroplating solution, but the total plating deposition amount can be increased, however, the firmness of a plating layer is reduced along with the increase of the preparation plating degree, and the plating effect is reduced instead; in example 1, the uranium-containing plating solution had a different pH than in example 5, so that the plating effect was different, and the pH of the plating solution was increased, resulting in
The formation of hydroxides or negatively charged complexes is detrimental to electromigration and electrodeposition of uranium, resulting in reduced plating efficiency and reduced film thickness.
In addition, in the embodiment of the application, besides changing the above parameters, the size of the workpiece to be plated, the distance between the cathode and the anode, the pitch of the anode spring platinum wire 3, the rotation speed of the stepper motor 6, and the like can be changed according to the actually required coating effect, so as to regulate and control the uranium plating process on the outer wall in a combined manner.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (8)
1. The utility model provides an utilize device of electroplating process preparation tubulose outer wall uranium film which characterized in that includes base, ball screw device, positive pole dead lever, water bath and direct current constant voltage power supply, wherein:
the water bath is fixed on the base, and an electroplating bath is arranged in the water bath;
the ball screw device is fixed on the base and is arranged on one side of the water bath;
the anode fixing rod is connected with the ball screw device and can slide up and down through the ball screw device;
the direct-current stabilized power supply is used for providing direct current required by electroplating for the electroplating bath.
2. The apparatus for preparing a uranium film with a tubular outer wall by an electroplating method according to claim 1, wherein a cathode alloy tube to be aluminized, an anode spring platinum wire and a sealing structure are arranged in the electroplating tank, and wherein:
the anode spring platinum wire is arranged around the cathode to-be-aluminized alloy tube;
the sealing structure comprises a sealing pressing block, a rubber gasket and a double-head threaded rod;
the sealing press blocks are arranged at the upper end and the lower end of the cathode to-be-aluminized alloy pipe, the rubber gaskets are arranged between the sealing press blocks and the cathode to-be-aluminized alloy pipe, and the double-head threaded rod is connected with the sealing press blocks at the upper end of the cathode to-be-aluminized alloy pipe;
and an electroplating liquid outlet is formed in the side wall of the bottom of the electroplating bath.
3. The apparatus for preparing a uranium film with a tubular outer wall by an electroplating method according to claim 2, wherein an anode of the direct current stabilized power supply is connected to the anode spring platinum wire through an anode wire, and a cathode is connected to the double-ended threaded rod through a cathode wire.
4. The apparatus for preparing a uranium film having a tubular outer wall by an electroplating method according to claim 3, wherein the ball screw apparatus includes a stepper motor, a ball screw support base, a ball screw, a linear guide rail, and a ball screw sliding table, and wherein:
the ball screw supporting seat is connected with the base through a fixing plate;
the ball screw and the linear guide rail are fixed on the ball screw supporting seat;
the stepping motor is fixed on the base and is connected with the ball screw;
the ball screw sliding table passes through the ball screw and is connected with the linear guide rail, and the ball screw sliding table slides up and down along the linear guide rail through rotation of the ball screw;
limit switches are arranged at the upper end and the lower end of the linear guide rail;
the anode fixing rod is fixed in the middle of the ball screw sliding table.
5. The apparatus for preparing a uranium film having a tubular outer wall by an electroplating method according to claim 4, wherein an anode wire through hole is provided in the middle of the anode fixing rod.
6. The apparatus for preparing a uranium film having a tubular outer wall by an electroplating method according to claim 5, wherein the material of the electroplating tank is polytetrafluoroethylene.
7. A method of applying the apparatus for producing a uranium film on a tubular outer wall according to any one of claims 1 to 6, comprising the steps of:
step 1: preparing uranium-containing electroplating solution, taking an absolute ethyl alcohol organic solution containing uranyl nitrate as the electroplating solution, and adjusting the pH value of the electroplating solution;
step 2: preparing a pretreatment electroplating solution and an activating solution, weighing phosphorous acid solid, adding the phosphorous acid solid into distilled water to prepare the pretreatment electroplating solution, and diluting an HF solution to obtain the activating solution;
step 3: pretreating the outer wall of the alloy tube to be aluminized by adopting the pretreatment electroplating solution and the activation solution in the step 2;
step 4: and (2) placing the uranium-containing electroplating solution in the step (1) into an electroplating bath, taking the to-be-aluminized alloy tube as a cathode, taking an anode spring platinum wire as an anode, and electroplating uranium, so that a uranium-containing coating film is formed on the outer wall surface of the to-be-aluminized alloy tube.
8. The method of claim 7, wherein in the step 3, when the outer wall of the alloy to be aluminized is pretreated, the following steps are adopted:
step 3.1: carrying out ultrasonic treatment on the alloy pipe to be aluminized by adopting acetone to remove organic impurities on the surface of the pipe wall;
step 3.2: cleaning by adopting HCl to remove oxide impurities on the surface of the pipe wall;
step 3.3: performing anodic oxidation treatment by pretreating the electroplating solution;
step 3.4: activating the to-be-aluminized alloy tube subjected to anodic oxidation treatment by adopting an activating solution, and forming an oxide film on the surface of the outer wall;
step 3.5: distilled water is used for flushing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310097257.2A CN116288598A (en) | 2023-01-27 | 2023-01-27 | Device and method for preparing uranium film on tubular outer wall by electroplating method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310097257.2A CN116288598A (en) | 2023-01-27 | 2023-01-27 | Device and method for preparing uranium film on tubular outer wall by electroplating method |
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