Plating solution dispersion method

Abstract

The present invention provides a method for dispersing a plating solution, which relates to the technical field of electroplating. The method according to the present invention promotes uniform dispersion of the plating solution and ensures the stability of the plating solution during the electroplating process. [Solution] The method includes the steps of performing electroplating while intermittently introducing gas bubbles into the plating solution, intermittently ultrasonicating the plating solution while introducing the gas bubbles, and placing at least some of the gas bubbles within the range of influence of the ultrasonic waves.

Description

[Technical Field]

[0001] The present invention relates to the technical field of electroplating, and more particularly to a method for dispersing a plating solution. [Background technology]

[0002] Current technologies for improving the thermal conductivity, electrical conductivity, and wear resistance of plating films involve adding materials such as graphene to the plating solution during the electroplating process to form composite plating films, thereby meeting the required plating film performance. However, solid particles such as graphene easily aggregate to form graphite during the electroplating process. If this graphite is electroplated onto the surface of the plating film instead of graphene, it can adversely affect the electroplating process. Therefore, conventional techniques typically involve adding a dispersant to the plating solution to prevent the solid particles from forming large particles. While adding a dispersant can somewhat reduce the aggregation of solid particles such as graphene in the plating solution, conventional dispersants do not facilitate the movement and diffusion of solid particles such as graphene in the plating solution. Therefore, composite plating films manufactured using the addition of a dispersant often fail to achieve the desired performance. Furthermore, although mechanical stirring and ultrasonic dispersion can also be used to some extent to disperse solid granules such as graphene, the plating solution must be kept stable during the electroplating process. However, conventional mechanical stirring and simple ultrasonic dispersion increase the flow and vibration of the plating solution, adversely affecting the plating film. Therefore, conventional mechanical stirring and simple ultrasonic dispersion are difficult to apply to the electroplating process.

[0003] In summary, how to promote uniform dispersion of solid particles such as graphene in the plating solution while ensuring the stability of the electroplating solution is a challenge that must be resolved with current technology. Summary of the Invention [Problem to be solved by the invention]

[0004] An object of the present invention is to provide a plating solution dispersion method that can promote uniform dispersion of graphene in the plating solution and simultaneously ensure the stability of the plating solution during the electroplating process. [Means for solving the problem]

[0005] In order to solve the above technical problems, the technical means adopted in the present invention are: A method for dispersing a plating solution, comprising: a step of intermittently feeding bubbles into the plating solution while performing electroplating; a step of intermittently ultrasonically treating the plating solution while feeding the bubbles; and a step of placing at least some of the bubbles within the range of influence of the ultrasonic waves.

[0006] Optionally, in some embodiments, the sonication is performed once for each single injection of the air bubbles.

[0007] Optionally, in some embodiments, the duration of the single gas bubble injection is set to 0.1 to 6 minutes, and the duration of the single ultrasonic treatment is set to 1 to 6 minutes.

[0008] Optionally, in some embodiments, the interval for injecting air bubbles is set to 5 to 20 minutes, and the interval for ultrasonic treatment is set to 1 to 20 minutes.

[0009] Optionally, in some embodiments, the ultrasonic treatment is performed from 10 to 50 seconds after the start of the blowing of the air bubbles during the single blowing of the air bubbles.

[0010] Optionally, in some embodiments, the solid granular material contained in the plating solution is selected from one or more of graphene, a metal oxide, and a non-metal oxide.

[0011] Optionally, in some embodiments, the diameter of the bubbles is limited to 0.01 to 1000 μm; or Limiting the diameter of the bubbles to 1 to 150 μm, or The diameter of the bubbles is controlled to 30 to 80 μm.

[0012] Optionally, in some embodiments, the ultrasonic frequency of the sonication is limited to 40-50 kHz.

[0013] Optionally, in some embodiments, injecting the gas bubbles into the plating solution via a gas bubble inlet, and placing the plating solution in a container containing a cathode and an anode spaced apart; The bubble inlet is located between the cathode and the anode, with the bubble inlet located closer to the anode and farther from the cathode; or The cathode is located on one side of the anode away from the side wall of the container, and the bubble inlet is located between the anode and the side wall, with the bubble inlet being located close to the side wall and away from the anode.

[0014] Optionally, in some embodiments, the bubble inlet faces in the direction where the cathode is located.

[0015] Optionally, in some embodiments, a plurality of the bubble inlets are arranged, and there is a difference in vertical height between each of the bubble inlets.

[0016] Optionally, in some embodiments, the number of the bubble inlets is two, and the two bubble inlets are respectively arranged in a first region and a second region, wherein the first region is a region between a horizontal plane on which a middle portion of the cathode is located and a horizontal plane on which a lower portion of the cathode is located, and the second region is a region between a horizontal plane on which a lower portion of the cathode is located and a horizontal plane on which a bottom of the container is located.

[0017] Optionally, in some embodiments, the bubble inlet located in the first region is a first inlet, and the bubble inlet located in the second region is a second inlet, the first inlet facing a portion above the horizontal plane on which the first inlet is located, and the second inlet facing a portion below the horizontal plane on which the second inlet is located.

[0018] Optionally, in some embodiments, the angle between the axis on which the first inlet is located and a horizontal plane is 30 to 80 degrees; and the angle between the axis on which the second inlet is located and a horizontal plane is 30 to 80 degrees.

[0019] Optionally, in some embodiments, the sonication is accomplished using an ultrasonic device located in the first zone.

[0020] Optionally, in some embodiments, the ultrasonic device is located between the bubble inlet and the cathode, with the ultrasonic device positioned close to the bubble inlet and away from the cathode.

[0021] Optionally, in some embodiments, the total amount of gas pumped per minute when pumping the bubbles is limited to 10 to 80 L.

[0022] Optionally, in some embodiments, when the gas bubbles are injected, the injected gas is selected from one or more of hydrogen gas, nitrogen gas, and air. [Effects of the Invention]

[0023] The present invention has the following advantageous effects compared to the prior art.

[0024] The present invention intermittently introduces bubbles into the plating solution during the electroplating process and intermittently ultrasonicates the plating solution. This method, on the one hand, strengthens the diffusion and expansion of the bubbles under the action of ultrasound. When the bubbles reach their bursting point and then burst, a momentary driving force is generated locally at the moment of bubble bursting. This driving force micro-agitates the localized portion of the plating solution, subsequently forming a localized microcirculation in the plating solution, promoting uniform dispersion of the plating solution. On the other hand, the diffusion movement of the bubbles in the plating solution also micro-agitates the plating solution, thereby contributing to dispersion. Furthermore, by intermittently introducing bubbles and ultrasonicating the plating solution, the present invention can suppress the introduction of bubbles and ultrasonication, thereby ensuring the relative stability of the plating solution during the electroplating process.

[0025] The plating solution dispersion method provided by the present invention is particularly suitable for plating solutions containing solid granules such as graphene, and the dispersion method can sufficiently disperse the solid granules such as graphene and effectively prevent the solid granules such as graphene from agglomerating to form larger granules, thereby improving the quality of electroplating.

[0026] In summary, the plating solution dispersion method provided by the present invention can promote uniform dispersion of the plating solution, particularly dispersion of solid granules such as graphene in the plating solution, as well as ensure the stability of the electroplating solution, compared to current technologies. [Brief explanation of the drawings]

[0027] In order to more clearly explain the technical solutions of the embodiments of the present invention, the drawings necessary for describing the embodiments are outlined as follows. Obviously, the drawings described below are some embodiments of the present invention, but those skilled in the art may obtain other drawings according to these drawings without exerting ordinary creative abilities.

[0028] FIG. 1 is a schematic diagram of the plating solution provided by Example 1. DETAILED DESCRIPTION OF THE INVENTION

[0029] In the following, the technical means in the embodiments of the present invention will be clearly and completely described with reference to the drawings in the embodiments of the present invention, and it is to be understood that the described embodiments are not all the embodiments but only some of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without any creative efforts fall within the protection scope of the present invention.

[0030] We will now describe in detail the technical solutions provided by the present invention. It is necessary to explain that the order in which the following examples are described does not limit the order in which the examples are used. Furthermore, in describing the present invention, "comprises" is interpreted as "includes, but is not limited to." Terms such as "first" and "second" are used only as modifiers and do not impose numerical or sequential meanings. Various embodiments of the present invention can be described in ranges, and it should be understood that the embodiments are described in ranges merely for the convenience and brevity of the present invention, but should not be construed as a strict limitation on the scope of the invention. Therefore, the description of a range should be considered to have specifically disclosed all possible subranges and single values ​​within that range.

[0031] The plating solution dispersion method provided by the present invention comprises the steps of: The method includes a step of intermittently feeding bubbles into the plating solution while performing electroplating, a step of intermittently ultrasonically treating the plating solution while feeding the bubbles, and a step of placing at least some of the bubbles within the range of influence of the ultrasonic waves.

[0032] We will explain the present invention using an example of a process in which air bubbles are intermittently introduced into a plating solution. The term "intermittent" here refers to the periodic repetition of introducing and stopping air bubbles, with the time interval between the cessation of air bubble introduction corresponding to the intermittent period of air bubble introduction. More specifically, the intermittent period of air bubble introduction is the length of time between the introduction of one air bubble and the start of the next air bubble introduction. The concepts of "intermittent" and "intermittent period" in ultrasonic processing are similar to those explained above and will not be repeated here.

[0033] It should be understood that "at least some of the bubbles are placed within the range of influence of the ultrasonic waves" is interpreted as meaning that at least some of the bubbles introduced into the plating solution burst under the action of the ultrasonic waves, causing micro-agitation in the local plating solution.

[0034] The plating solution dispersion method provided by the present invention can ensure the stability of the electroplating solution and promote uniform dispersion of the plating solution.

[0035] What is necessary for explanation is that "the plating solution is ultrasonically treated intermittently while air bubbles are being fed in" is to be interpreted as meaning that the ultrasonic treatment is carried out intermittently while air bubbles are being fed in, so that the air bubbles are fed in simultaneously with the ultrasonic treatment. Furthermore, it is to be interpreted as meaning that the air bubbles are fed in each time and the ultrasonic treatment is carried out, or that the air bubbles are fed in once and the ultrasonic treatment is carried out, as long as the plating solution is sufficiently dispersed.

[0036] Preferably, ultrasonic treatment is performed once each time air bubbles are fed in, thereby further improving the dispersion effect of solid granules such as graphene in the plating solution.

[0037] In some embodiments, the duration of a single gas bubble injection may be 0.1 to 6 minutes, and the duration of a single ultrasonic treatment may be 1 to 6 minutes.

[0038] In some embodiments, the interval between the injection of air bubbles may be 5 to 20 minutes, and the interval between the ultrasonic treatment may be 1 to 20 minutes.

[0039] When the length of time for a single supply of air bubbles, the length of time for a single ultrasonic treatment, the intermittent period for supplying air bubbles, and the intermittent period for ultrasonic treatment are within the above-mentioned ranges, the stability of the plating solution is better maintained, which is advantageous for carrying out electroplating.

[0040] Furthermore, when setting and adjusting the length of time and the intermittent period for the air bubble injection and ultrasonic treatment, it is necessary to perform the air bubble injection and ultrasonic treatment simultaneously each time the air bubbles are injected. To achieve this, the ultrasonic treatment can be started simultaneously with each air bubble injection, or the air bubbles can be injected first each time and the ultrasonic treatment can be performed before the single air bubble injection is completed. Furthermore, when air bubbles are injected and ultrasonic treatment is performed each time, the air bubble injection and ultrasonic treatment can be completed simultaneously, or the air bubble injection can be completed before the ultrasonic treatment, or the ultrasonic treatment can be completed before the air bubble injection.

[0041] Preferably, air bubbles are first fed each time and ultrasonic treatment is carried out before the single feeding of air bubbles is completed, and the feeding of air bubbles is completed before the ultrasonic treatment.

[0042] In some embodiments, the ultrasonic treatment begins 10 to 50 seconds after the start of the air bubble injection process during a single air bubble injection process. That is, during each air bubble injection and ultrasonic treatment process, the air bubble injection is first performed, and the air bubble injection continues for 10 to 50 seconds, after which the ultrasonic treatment begins. In this case, since the air bubble injection and the ultrasonic treatment are performed simultaneously, it can be understood that the air bubble injection does not end when the ultrasonic treatment begins.

[0043] In some embodiments, the solid granular material contained in the plating solution is selected from one or more of graphene, a metal oxide, and a non-metal oxide.

[0044] The plating solution dispersion method provided by the present invention is particularly suitable for plating solutions containing solid granules such as graphene, etc. The plating solution dispersion method provided by the present invention effectively prevents the solid granules such as graphene (e.g., graphene, zinc oxide, silicon dioxide) from agglomerating to form larger granules, thereby ensuring smooth operation of the related plating process.

[0045] Preferably, the plating solution dispersion method provided by the present invention is suitable for a plating solution containing graphene, and effectively prevents aggregation of graphene in the plating solution by using the plating solution dispersion method provided by the present invention.

[0046] In some embodiments, the diameter of the bubbles may be 0.01 to 1000 μm; preferably, the diameter of the bubbles may be 1 to 150 μm; preferably, the diameter of the bubbles may be 30 to 80 μm. When the diameter of the bubbles is within the above range, the stability of the plating solution can be ensured.

[0047] In some embodiments, the ultrasonic frequency of the sonication is 40-50 kHz.

[0048] In some embodiments, the injection of gas bubbles into the plating solution is accomplished through a gas bubble inlet, which can be located between the cathode and the anode in a vessel containing a spaced apart cathode and anode, with the gas bubble inlet located near the anode and far from the cathode.

[0049] To explain, to ensure that bubbles bursting under the action of ultrasound impart micro-agitation to the local plating solution, the placement of the bubble inlet must satisfy the prerequisite that at least some of the bubbles are within the range of ultrasound influence. When the bubble inlet is installed between the cathode and the anode, bubbles burst between the cathode and the anode, imparting targeted micro-agitation to the plating solution between the cathode and the anode. This promotes the diffusion of substances in the plating solution between the cathode and the anode, replenishing substances (including cations and solid particles) consumed by electroplating near the cathode and maintaining stable concentrations of related substances in the plating solution near the cathode. Taking a plating solution containing solid particles such as graphene as an example, a bubble inlet placed between the cathode and the anode can enhance the diffusion of graphene between the cathode and the anode, promoting the migration of graphene to the surface of the cathode and maintaining a certain level of graphene concentration on the surface.

[0050] Furthermore, the cathode may be located on one side of the anode away from the sidewall of the vessel, and the bubble inlet may be located between the anode and the sidewall, with the bubble inlet located closer to the sidewall and further away from the anode. This may reduce the perturbation of large bubbles into the plating solution near the cathode and improve plating quality. For example, in some embodiments, the bubble inlet may be located on one side of the anode away from the cathode, so that bubbles remain at least 5 cm away from the surface of the cathode when they burst.

[0051] In some embodiments, the container holding the plating solution may be a plating tank.

[0052] In some embodiments, the bubble inlet may face the cathode, which may favor migration of materials in the plating solution toward the cathode, thereby maintaining a relatively stable concentration of the plating solution near the cathode.

[0053] In some embodiments, a plurality of bubble inlets are arranged, and there is a difference in vertical height between each of the bubble inlets.

[0054] When the plating solution dispersion method provided by the present invention includes multiple bubble inlets positioned at different heights along the vertical direction, the bubbles injected into the plating solution burst at different depths in the plating solution under the action of ultrasound, causing localized micro-agitation in the plating solution at different depths and promoting dispersion of the plating solution at different depths. Furthermore, the number of bubble inlets can be two, three, four, or five. Preferably, the number of bubble inlets can be two.

[0055] In some embodiments, the number of bubble inlets is two, and the bubble inlets may be located in a first zone and a second zone, respectively. Here, the first zone is the zone between the horizontal plane where the middle part of the cathode is located and the horizontal plane where the lower part of the cathode is located, and the second zone is the zone between the horizontal plane where the lower part of the cathode is located and the horizontal plane where the bottom of the container is located. The first zone may be understood as the middle-lower region of the plating solution, and the second zone may be understood as the bottom region of the plating solution. The first zone may be understood as being above the second zone, with the plating solution still present above the first zone, and a portion of the cathode being located in the plating solution above the first zone. In some embodiments, the zone between the horizontal plane where the middle part of the cathode is located and the horizontal plane where the upper part of the cathode is located may be named a third zone, and the third zone may be understood as the middle-upper region of the plating solution.

[0056] When two bubble inlets are located in the first and second zones, bubbles introduced into the plating solution through the bubble inlet located in the second zone first micro-agitate the plating solution at the bottom by moving the bubbles. Then, bubbles introduced through the bubble inlet located in the second zone move upward to the first zone under the action of buoyancy and burst under the action of ultrasound, thereby locally micro-agitating the plating solution between the cathode and anode in the first zone and improving the local micro-circulation of the plating solution between the cathode and anode in the first zone. Therefore, bubbles introduced into the plating solution through the bubble inlet located in the second zone primarily micro-agitate the plating solution in both the first and second zones. Furthermore, bubbles introduced into the plating solution through the bubble inlet located in the first zone can also move upward under the action of buoyancy. When bubbles introduced into the plating solution through the bubble inlet located in the first zone move upward to the third zone, the bubbles that have moved to the third zone also burst under the action of the ultrasound, thereby providing localized micro-agitation of the plating solution in the third zone. Furthermore, when bubbles introduced into the plating solution through the bubble inlet located in the second zone burst near the bubble inlet located in the first zone to form smaller bubbles, the formed smaller bubbles merge with and become part of the bubbles introduced into the plating solution through the bubble inlet located in the first zone, and a secondary burst then occurs, enhancing the localized micro-circulation and agitation of the plating solution.

[0057] Therefore, when two bubble inlets are arranged in the first and second zones, respectively, the bubbles may simultaneously impart localized micro-agitation to the plating solution in the bottom, lower middle, and upper middle parts of the zones, dispersing the plating solution in the bottom, lower middle, and upper middle parts.

[0058] In some embodiments, the two bubble inlets are located on the same vertical axis along the vertical direction, where the axis refers to the vertical axis along the vertical direction, not the axis along which the bubble inlets face.

[0059] In some embodiments, the bubble inlet located in the first region is a first inlet, and the bubble inlet located in the second region is a second inlet, the first inlet facing a portion above the horizontal plane on which the first inlet is located, and the second inlet facing a portion below the horizontal plane on which the second inlet is located.

[0060] When the second inlet faces a portion below the horizontal plane, the air bubbles fed into the plating solution through the second inlet move downward for a certain distance before moving upward under the action of buoyancy, causing some of the air bubbles fed into the plating solution through the second inlet to burst in the second zone, thereby applying local circulatory micro-agitation to the plating solution in the second zone.

[0061] In some embodiments, the angle between the axis of the bubble inlet located in the first section and the horizontal plane may be 30 to 80°; the angle between the axis of the bubble inlet located in the second section and the horizontal plane may be 30 to 80°. The axis of the bubble inlet may be understood to refer to the central axis of the bubble inlet.

[0062] Preferably, the angle between the axis of the bubble inlet located in the first zone and the horizontal plane may be 30 to 60°; the angle between the axis of the bubble inlet located in the second zone and the horizontal plane may be 30 to 60°.

[0063] In some embodiments, the sonication may be accomplished using an ultrasonic device located in the first zone, and a bubble inlet in the first zone can ensure that at least some of the bubbles are within the range of the ultrasonic waves when the ultrasonic device is positioned in the first zone.

[0064] In some embodiments, an ultrasonic device may be located between the bubble inlet and the cathode, with the ultrasonic device positioned near the bubble inlet and away from the cathode.

[0065] When the ultrasonic device is located between the bubble inlet and the cathode, and the ultrasonic device is located close to the bubble inlet and away from the cathode, the ultrasonic device is located near the bubble inlet, which allows many bubbles to be within the range of ultrasonic influence, thereby ensuring the local micro-agitation effect of bubble bursting on the plating solution.In addition, the ultrasonic device is located away from the cathode, which reduces the ultrasonic disturbance to the plating solution near the cathode, ensures the relative stability of the plating solution near the cathode, and thus improves plating quality.

[0066] Furthermore, if the plating solution dispersion method requires a plurality of bubble inlets, the ultrasonic device can be disposed between any of the bubble inlets and the cathode.

[0067] In some embodiments, the distance between the ultrasound device and the cathode may be at least 40 cm.

[0068] In some embodiments, when pumping bubbles, the total amount of gas pumped per minute can be 10 to 80 L.

[0069] The total amount of gas pumped per minute corresponds to the amount of gas actually pumped per minute to overcome the pressure of the plating solution. When the total amount of gas pumped per minute is within the above range, the bubble size is controlled so that the number of bubbles in the plating solution, the burst frequency, and the flow rate are all within the optimal range, and the stirring strength of the bubbles added to the plating solution is appropriate.

[0070] Furthermore, the diameter and injection amount of the bubbles are determined depending on the depth of the bubble inlet in the plating solution and the content of solid granules such as graphene in the plating solution. For example, the deeper the position of the bubble inlet in the plating solution, the larger the injection amount of the bubbles can be set, and the smaller the bubble diameter can be set. For example, at the same depth in the plating solution, the higher the concentration of solid granules such as graphene in the plating solution, the larger the injection amount of the bubbles can be set, and the smaller the bubble diameter can be set.

[0071] Furthermore, when the number of bubble inlets is two and the two bubble inlets are located in the first and second zones, respectively, the total amount of gas delivered per minute through the two bubble inlets may be the same or different. Specifically, the total amount of gas delivered per minute through the bubble inlet located in the second zone may be greater than the total amount of gas delivered per minute through the bubble inlet located in the first zone.

[0072] In some embodiments, when gas bubbles are injected, the injected gas may be selected from one or more of hydrogen gas, nitrogen gas, and air.

[0073] The present invention selects different gases depending on the type of plating film, thereby achieving various additional effects. For example, when plating copper, air is introduced to promote a smooth plating process of the copper film. For example, when plating silver, hydrogen gas is introduced to utilize the reducing properties of hydrogen, thereby making the surface of the silver film more uniform and bright.

[0074] In some embodiments, the gas introduced can be a gas mixture such as nitrogen and hydrogen, without limitation thereto.

[0075] Example 1 The present invention provides a method for dispersing graphene-silver plating solution. A schematic diagram of the plating solution is shown in Figure 1. The method includes the following steps:

[0076] Electroplating is performed in an electroplating tank 101 using a graphene-silver plating solution. The opening size of the plating tank 101 is set to 2 m × 2 m, the vertical depth of the plating solution is set to 1.2 m, and the graphene concentration in the plating solution is set to 10 g / L. Hydrogen gas is intermittently fed into the plating solution during the electroplating process. A single injection of hydrogen gas takes 4 min, the diameter of the injected bubbles is set to 20 μm, and the intermittent period for feeding bubbles is set to 10 min. After the start of bubble feeding for 6 s, the graphene-silver plating solution is ultrasonically treated. A single ultrasonic treatment takes 5 min and the intermittent period for ultrasonic treatment is set to 8 min.

[0077] In the plating tank 101, air bubbles are fed through two air bubble inlets 102. The two air bubble inlets 102 are located between the cathode 105 and the anode 104 and face the cathode 105. The two air bubble inlets 102 are located in a first zone 106 and a second zone 107 of the plating solution, respectively, and are arranged on the same vertical axis. The distance between the air bubble inlet 102 located in the first zone 106 and the bottom of the plating tank 101 is set to 0.3 m. The air bubble inlet 102 located in the first zone 106 faces in a direction above the horizontal direction where it is located. The included angle between the axis of the air bubble inlet 102 located in the first zone 106 and the horizontal plane is set to 45°. 20 L of air is fed per minute through the air bubble inlet 102 located in the first zone 106. The distance between the gas bubble inlet 102 located in the second zone 107 and the bottom of the plating tank 101 is set to 0.1 m, the gas bubble inlet 102 located in the second zone 107 faces downward in the horizontal direction in which it is located, the included angle between the axis of the gas bubble inlet 102 located in the second zone 107 and the horizontal plane is set to 45°, and a gas rate of 20 L per minute is fed through the gas bubble inlet 102 located in the second zone 107. The horizontal distance between the gas bubble inlet 102 and the cathode 105 is set to 0.75 m.

[0078] Ultrasonic treatment is performed via an ultrasonic device 103, which is located between the bubble inlet 102 and the cathode 105, with the horizontal distance between the ultrasonic device 103 and the cathode 105 set to 0.5 m and the ultrasonic frequency set to 42 kHz.

[0079] Example 2 The present invention provides a method for dispersing a graphene-silver plating solution, which includes the following steps:

[0080] Electroplating was performed in an electroplating tank using a graphene-silver plating solution. The opening size of the plating tank was set to 2m x 2m, the vertical depth of the plating solution was set to 1.5m, and the graphene concentration in the plating solution was set to 10g / L. Hydrogen gas was intermittently introduced into the plating solution during the electroplating process. A single injection of hydrogen gas took 0.1 min, the diameter of the injected bubbles was set to 0.01μm, and the intermittent period for introducing bubbles was set to 5 min. The graphene-silver plating solution was ultrasonicated as soon as the injection of bubbles began. A single ultrasonic treatment took 1 min, and the intermittent period for ultrasonic treatment was set to 4.1 min.

[0081] In this system, air bubbles are introduced through two air bubble inlets. The two air bubble inlets are located on one side of the anode away from the cathode and face the cathode. The two air bubble inlets are located in the first and second zones of the plating solution, respectively, and are arranged on the same vertical axis. The distance between the air bubble inlet located in the first zone and the bottom of the plating tank is set to 0.4 m. The air bubble inlet located in the first zone faces in a direction above the horizontal where it is located. The included angle between the axis of the air bubble inlet located in the first zone and the horizontal plane is set to 80°. 5 L of air is introduced per minute through the air bubble inlet located in the first zone. The distance between the gas bubble inlet in the second zone and the bottom of the plating tank is set to 0.2 m, the gas bubble inlet in the second zone faces downward in the horizontal direction, the included angle between the axis of the gas bubble inlet in the second zone and the horizontal plane is set to 80°, and 5 L of gas is fed per minute through the gas bubble inlet in the second zone. The horizontal distance between the gas bubble inlet and the cathode is set to 1.25 m.

[0082] The ultrasonic treatment is carried out via an ultrasonic device, which is located in the first zone and between the bubble inlet and the cathode, with the horizontal distance between the ultrasonic device and the cathode set to 0.5 m and the ultrasonic frequency set to 40 kHz.

[0083] Example 3 The present invention provides a method for dispersing a graphene-silver plating solution, which includes the following steps:

[0084] Electroplating was performed in an electroplating tank using a graphene-silver plating solution. The opening size of the plating tank was set to 2m x 2m, the vertical depth of the plating solution was set to 1.5m, and the graphene concentration in the plating solution was set to 10g / L. Hydrogen gas was intermittently pumped into the plating solution during the electroplating process. A single injection of hydrogen gas took 6 minutes, the diameter of the injected bubbles was set to 1000μm, and the intermittent period for bubble injection was set to 20 minutes. After the bubbles were injected for 10 seconds, the graphene-silver plating solution was ultrasonicated. A single ultrasonic treatment took 6 minutes, and the intermittent period for ultrasonic treatment was set to 20 minutes.

[0085] In this system, air bubbles are introduced through two air bubble inlets. The two air bubble inlets are located on one side of the anode away from the cathode and face the cathode. The two air bubble inlets are located in the first and second zones of the plating solution, respectively, and are arranged on the same vertical axis. The distance between the air bubble inlet located in the first zone and the bottom of the plating tank is set to 0.4 m. The air bubble inlet located in the first zone faces in a direction above the horizontal where it is located. The included angle between the axis of the air bubble inlet located in the first zone and the horizontal plane is set to 60°. 40 L of air is introduced per minute through the air bubble inlet located in the first zone. The distance between the gas bubble inlet located in the second zone and the bottom of the plating tank is set to 0.2 m, the gas bubble inlet located in the second zone faces downward in the horizontal direction, the included angle between the axis of the gas bubble inlet located in the second zone and the horizontal plane is set to 60°, and 40 L of gas is fed per minute through the gas bubble inlet located in the second zone. The horizontal distance between the gas bubble inlet and the cathode is set to 1.25 m.

[0086] The ultrasonic treatment is carried out via an ultrasonic device, which is located in the first zone and between the bubble inlet and the cathode, with the horizontal distance between the ultrasonic device and the cathode set to 0.5 m and the ultrasonic frequency set to 50 kHz.

[0087] Example 4 The present invention provides a method for dispersing a graphene-silver plating solution, which includes the following steps:

[0088] Electroplating was performed in an electroplating tank using a graphene-silver plating solution. The opening size of the plating tank was set to 1m x 1m, the vertical depth of the plating solution was set to 1m, and the graphene concentration in the plating solution was set to 15g / L. Hydrogen gas was intermittently pumped into the plating solution during the electroplating process. A single injection of hydrogen gas took 6 minutes, the diameter of the injected bubbles was set to 50μm, and the intermittent period for bubble injection was set to 10 minutes. After the bubbles were injected for 50 seconds, the graphene-silver plating solution was ultrasonicated. A single ultrasonic treatment took 6 minutes, and the intermittent period for ultrasonic treatment was set to 10 minutes.

[0089] In the plating tank, air bubbles are fed through one air bubble inlet. The air bubble inlet is located on one side of the anode away from the cathode and faces the cathode. The air bubble inlet is located in the second zone of the plating solution. The distance between the air bubble inlet and the bottom of the plating tank is set to 0.1 m, and 40 L of gas is fed per minute through the air bubble inlet. The horizontal distance between the air bubble inlet and the cathode is set to 1.25 m.

[0090] The ultrasonic treatment is carried out via an ultrasonic device, which is located in the first zone and between the bubble inlet and the cathode, with the horizontal distance between the ultrasonic device and the cathode set to 0.25 m and the ultrasonic frequency set to 45 kHz.

[0091] Although the technical solutions provided by the embodiments of the present invention have been described in detail above, and the principles and embodiments of the present invention are described in the text using specific examples, the explanations of the above examples are only used to help understand the method of the present invention and its spirit. Moreover, those skilled in the art can make changes to the specific embodiments and application scope according to the spirit of the present invention, and in summary, the contents of this specification should not be understood as limitations on the present invention. [Explanation of symbols]

[0092] 101 - electroplating bath; 102-Bubble inlet; 103-Ultrasonic device; 104-anode; 105 - cathode; 106-First area; 107-Second area.

Claims

1. The method includes the steps of: performing electroplating while intermittently feeding bubbles into a plating solution; feeding the bubbles while intermittently subjecting the plating solution to ultrasonic treatment; and placing at least some of the bubbles within an influence range of the ultrasonic waves. A method for dispersing a plating solution.

2. 2. The plating solution dispersion method according to claim 1, wherein the ultrasonic treatment is performed once each time the air bubbles are fed once.

3. The length of time for which the bubbles are fed once is set to 0.1 to 6 minutes, and the length of time for which the ultrasonic treatment is performed once is set to 1 to 6 minutes; and the total amount of gas fed per minute when the bubbles are fed is limited to 10 to 80 L.

2. The plating solution dispersion method according to claim 1.

4. The intermittent period for injecting the bubbles is set to 5 to 20 minutes, and the intermittent period for the ultrasonic treatment is set to 1 to 20 minutes.

2. The plating solution dispersion method according to claim 1.

5. The ultrasonic treatment is carried out from 10 to 50 seconds after the start of the blowing of the air bubbles during the single blowing of the air bubbles.

2. The plating solution dispersion method according to claim 1.

6. the solid granular material contained in the plating solution is selected from one or more of graphene, metal oxides, and non-metal oxides; and when the gas bubbles are introduced, the introduced gas is selected from one or more of hydrogen gas, nitrogen gas, and air.

2. The plating solution dispersion method according to claim 1.

7. The diameter of the bubbles is limited to 0.01 to 1000 μm, or Limiting the diameter of the bubbles to between 1 and 150 μm, or The diameter of the bubbles is kept to 30 to 80 μm.

2. The plating solution dispersion method according to claim 1.

8. 2. The plating solution dispersion method according to claim 1, wherein the ultrasonic frequency of the ultrasonic treatment is controlled to 40 to 50 kHz.

9. Injecting the gas bubbles into the plating solution through a gas bubble inlet, and placing the plating solution in a container containing a cathode and an anode spaced apart from each other; The bubble inlet is located between the cathode and the anode, with the bubble inlet located closer to the anode and farther from the cathode; or the cathode is located on one side of the anode away from a side wall of the container, and the bubble inlet is located between the anode and the side wall, and the bubble inlet is located close to the side wall and away from the anode; 2. The plating solution dispersion method according to claim 1.

10. 10. The plating solution dispersion method according to claim 9, wherein the bubble inlet faces the cathode.

11. A plurality of the air bubble inlets are arranged, and there is a difference in height between the air bubble inlets along the vertical direction.

11. The plating solution dispersion method according to claim 9 or 10.

12. the number of the bubble inlets is two, and the two bubble inlets are respectively arranged in a first region and a second region, wherein the first region is a region between a horizontal plane on which an intermediate portion of the cathode is located and a horizontal plane on which a lower portion of the cathode is located, and the second region is a region between a horizontal plane on which the lower portion of the cathode is located and a horizontal plane on which a bottom of the container is located; The plating solution dispersion method according to claim 11 .

13. The air bubble inlet located in the first area is a first inlet, the air bubble inlet located in the second area is a second inlet, the first inlet faces a part above the horizontal plane where the first inlet is located, and the second inlet faces a part below the horizontal plane where the second inlet is located.

13. The plating solution dispersion method according to claim 12.

14. The angle between the axis of the first inlet and a horizontal plane is 30 to 80°; the angle between the axis of the second inlet and a horizontal plane is 30 to 80°.

14. The plating solution dispersion method according to claim 13.

15. the ultrasonic treatment is performed using an ultrasonic device located in the first zone; the ultrasonic device is located between the bubble inlet and the cathode, and the ultrasonic device is positioned close to the bubble inlet and away from the cathode.

15. The plating solution dispersion method according to claim 14.

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