Electrolytic copper foil production apparatus having temperature control and copper foil width adjustment functions

Abstract

The present invention relates to an electrolytic copper foil production apparatus and, more specifically, to an electrolytic copper foil production apparatus having temperature control and copper foil width adjustment functions for minimizing defect occurrence and producing a high-quality copper foil. The present invention for achieving the above purpose provides an electrolytic copper foil production apparatus having temperature control and copper foil width adjustment functions, the apparatus comprising: a water tank unit in which an electrolyte is accommodated; a drum unit provided inside the water tank unit and provided to electrodeposit a copper foil by using the electrolyte; a positive electrode unit provided inside the water tank unit and electrically connected to the drum unit through the electrolyte from under the drum unit; and a temperature control unit provided under the positive electrode unit.

Description

Electrolytic copper foil production device with temperature control and copper foil width adjustment functions

[0001] The present invention relates to an electrolytic copper foil production device, and more specifically, to an electrolytic copper foil production device having temperature control and copper foil width control functions for producing high-quality copper foil with minimized defect occurrence.

[0002]

[0003] Electrolytic copper foil is a product produced by forming copper into a thin foil form through an electroplating process. It is primarily used in the manufacture of electronic devices and batteries, and is particularly widely utilized as a core material for negative electrode current collectors in lithium-ion batteries or for printed circuit boards (PCBs). In particular, electrolytic copper foil is utilized as an important material in the advanced electronic device and battery industries due to its excellent conductivity and the advantage of being thin and capable of precise thickness control.

[0004] In the manufacture of such electrolytic copper foil, insoluble electrodes are used as anodes. Specifically, the electrode is responsible for the oxygen evolution reaction during the electrolysis process; it does not dissolve in the electrolyte and contributes to maintaining the stability of the reaction. In other words, the insoluble electrode enables the continuous participation of the electrochemical reaction without being consumed, thereby facilitating the smooth production of electrolytic copper foil.

[0005] However, conventional insoluble electrodes have limitations in terms of durability and efficiency. In particular, maintaining high electrode performance is crucial during the electrolytic copper foil manufacturing process, as electrode performance directly affects copper quality and the efficiency of electrochemical reactions. However, current electrodes degrade over time, leading to increased production costs and reduced overall production efficiency.

[0006] Furthermore, electrodes commonly used in the fabrication process struggle to maintain a uniform thickness during coating and plating, resulting in uneven activation of the electrode surface. This led to a decrease in the electrochemical reactivity of the electrodes, which in turn resulted in non-uniform electrode performance during production.

[0007] Furthermore, the electrochemical reactions occurring during the manufacturing process of electrolytic copper foil involve a complex process in which hydrogen is generated at the cathode and oxygen is generated at the anode. These reactions can cause corrosion or failure of the electrodes and reduce the reliability of the production process. In particular, conventional anode materials lacked resistance to oxygen generation, leading to performance degradation during prolonged use.

[0008] Furthermore, the temperature of the electrolyte during the electrolytic copper foil production process affects the plating speed and thickness. Higher temperatures increase the plating speed, but excessively high temperatures can lead to defects. Therefore, it is important to maintain the electrolyte temperature uniformly at an appropriate level during the production process.

[0009] However, conventional electrolytic copper foil manufacturing technology had a problem where defects occurred due to the difficulty in controlling these temperatures.

[0010]

[0011] <Prior Art Literature>

[0012] Korean Registered Patent No. 10-1409750

[0013]

[0014] The objective of the present invention, which is to solve the above-mentioned problems, is to provide an electrolytic copper foil production device having temperature control and copper foil width adjustment functions to minimize defect occurrence and produce high-quality copper foil.

[0015] The technical problems that the present invention aims to solve are not limited to those mentioned above, and other unmentioned technical problems will be clearly understood by those skilled in the art to which the present invention belongs from the description below.

[0016]

[0017] The present invention, for achieving the above-mentioned purpose, provides an electrolytic copper foil production device having temperature control and copper foil width adjustment functions, characterized by comprising: a tank portion containing an electrolyte inside; a drum portion provided inside the tank portion and configured to electrodeposit a copper foil using the electrolyte; an anode portion provided inside the tank portion and connected to the drum portion through the electrolyte at the bottom of the drum portion; and a temperature control portion provided at the bottom of the anode portion.

[0018] In an embodiment of the present invention, the temperature control unit may be characterized by comprising: a base formed as a curved surface so as to be coupled to the anode portion on its upper surface; a tube formed inside the base; an inlet formed on one side of the tube; and an outlet formed on the other side of the tube, wherein a heat medium is circulated inside the tube.

[0019] In an embodiment of the present invention, the temperature control unit may be characterized by including: a sensor module for measuring the temperature of the electrolyte; and a control module provided to control the temperature of a heat medium circulating through the tube so that the temperature of the electrolyte measured by the sensor module maintains a preset temperature.

[0020] In an embodiment of the present invention, the temperature control unit may be characterized by being provided as a pair spaced apart from each other, and by being configured so that the electrolyte is supplied between the drum unit and the anode unit through a hollow portion formed spaced apart from each other.

[0021] In an embodiment of the present invention, the drum portion and the anode portion may be characterized by being formed spaced apart from each other by a predetermined distance to allow the electrolyte to flow in.

[0022] In an embodiment of the present invention, the invention may be characterized by including an electrolyte supply unit provided to supply an electrolyte into the interior of the tank; and an electrolyte discharge unit provided on the side of the tank and provided to discharge the electrolyte overflowing from the tank to the outside.

[0023] In an embodiment of the present invention, the electrolyte discharge portion may be characterized by comprising: a discharge body provided on the outer perimeter of the water tank portion and receiving the electrolyte overflowing from the water tank portion; and an electrolyte discharge port provided at the bottom of the discharge body.

[0024] In an embodiment of the present invention, the invention may further include a winding unit configured to transfer the copper foil generated in the drum unit to a core and wind it.

[0025] In an embodiment of the present invention, the drum portion may be characterized by comprising: a cylindrical drum body arranged to rotate in one direction; a rotation axis formed penetrating the center of the drum body; and a cathode material formed along the outer surface of the drum body.

[0026] In an embodiment of the present invention, the anode portion may be characterized as being provided as an insoluble electrode formed by coating a coating solution of an anode material onto an electrode substrate made of titanium material.

[0027]

[0028] The effect of the present invention according to the above configuration is that the quality of the produced copper foil can be maintained uniformly by uniformly controlling the temperature of the electrolyte.

[0029] In addition, according to the present invention, by using an insoluble titanium substrate coated with a platinum compound, the speed and efficiency of the electrochemical reaction can be increased. This can improve productivity by increasing the electrodeposition rate of copper during the production of electrolytic copper foil.

[0030] In addition, according to the present invention, corrosion or performance degradation of the electrode can be minimized by coating the anode with iridium oxide, which has resistance to oxygen generation. This ensures the stability of the electrode during the electrolytic copper foil manufacturing process, enabling long-term use.

[0031] Furthermore, according to the present invention, the quality of the electrolytic copper foil produced is improved thanks to the high reactivity and stability of the insoluble electrode. High-quality copper foil enhances applicability in the electronic device and battery industries and contributes to maximizing the performance of the final product.

[0032] Furthermore, according to the present invention, in addition to the production of electrolytic copper foil, it can be applied to various fields such as brine electrolysis, wastewater treatment, and electrochemical cleaning. This versatility increases the potential for commercialization of the technology and can promote its utilization in various industrial sectors.

[0033]

[0034] The effects of the present invention are not limited to the effects described above, and should be understood to include all effects that can be inferred from the configuration of the invention described in the detailed description of the invention or the claims.

[0035]

[0036] FIG. 1 is an exemplary diagram of an electrolytic copper foil production apparatus according to an embodiment of the present invention.

[0037] FIG. 2 is a perspective view of an electrolytic copper foil production apparatus according to an embodiment of the present invention.

[0038] FIG. 3 is an exemplary diagram of a temperature control unit according to an embodiment of the present invention.

[0039] FIG. 4 is a perspective view of an anode portion having a barrier formed thereon according to an embodiment of the present invention.

[0040] FIG. 5 is a process example diagram of a method for manufacturing an insoluble electrode for manufacturing electrolytic copper foil according to an embodiment of the present invention.

[0041] FIG. 6 is a flowchart of a method for manufacturing an insoluble electrode for manufacturing electrolytic copper foil according to an embodiment of the present invention.

[0042] FIG. 7 is a flowchart of the steps for pre-processing an electrode substrate according to an embodiment of the present invention.

[0043] FIG. 8 is a flowchart of the steps for preparing a coating solution for coating a pretreated electrode substrate according to an embodiment of the present invention.

[0044] FIG. 9 is a flowchart of the steps for manufacturing an insoluble electrode by coating an electrode substrate with a coating solution prepared according to an embodiment of the present invention.

[0045] FIG. 10 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 200x magnification to confirm the microstructure and elemental composition of an insoluble substrate according to the present invention.

[0046] Figure 11 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 500x magnification to confirm the microstructure and elemental composition of an insoluble substrate according to the present invention.

[0047] FIG. 12 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 2,000x magnification to confirm the microstructure and elemental composition of an insoluble substrate according to the present invention.

[0048] FIG. 13 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 10,000x magnification to confirm the microstructure and elemental composition of the insoluble substrate according to the present invention.

[0049] FIG. 14 is a graph showing the qualitative or quantitative analysis of elements on the surface of a material using an Energy Dospersive Spectroscope for an insoluble substrate according to the present invention.

[0050] FIG. 15 is an image taken at a magnification of 5,000x with a scanning electron microscope to confirm the elemental composition of the insoluble substrate according to the present invention.

[0051] FIG. 16 is an image taken to confirm the molecular structure and crystal structure of a mixture of insoluble substrates according to the present invention.

[0052] Figures 17 and 18 are images taken to confirm the molecular structure and crystal structure of iridium and tantalum when mixed together.

[0053] Figures 19 to 21 are images of an insoluble substrate taken by an X-ray photoelectron spectrometer.

[0054] Figure 22 is a table to show the effect of pretreatment on the electrode substrate.

[0055] Figure 23 is a table to show the effect of the coating solution on the electrode substrate.

[0056] Figure 24 is a table to show the effects of drying and heat treatment on the electrode substrate.

[0057]

[0058] A most preferred embodiment according to the present invention is characterized by comprising: a tank portion containing an electrolyte inside; a drum portion provided inside the tank portion and configured to electrodeposit a copper foil using the electrolyte; an anode portion provided inside the tank portion and connected to the drum portion through the electrolyte at the bottom of the drum portion; and a temperature control portion provided at the bottom of the anode portion.

[0059]

[0060] The present invention will be described below with reference to the attached drawings. However, the present invention can be implemented in various different forms and is therefore not limited to the embodiments described herein. Furthermore, in order to clearly explain the present invention in the drawings, parts unrelated to the explanation have been omitted, and similar parts throughout the specification have been given similar reference numerals.

[0061] Throughout the specification, when it is stated that a part is "connected (connected, in contact, combined)" with another part, this includes not only cases where they are "directly connected," but also cases where they are "indirectly connected" with other members interposed between them. Furthermore, when it is stated that a part "includes" a certain component, this means that, unless specifically stated otherwise, it does not exclude other components but rather allows for the inclusion of additional components.

[0062] The terms used herein are merely for describing specific embodiments and are not intended to limit the invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this specification, terms such as “comprising” or “having” are intended to indicate the presence of the features, numbers, steps, actions, components, parts, or combinations thereof described in the specification, and should be understood as not precluding the existence or addition of one or more other features, numbers, steps, actions, components, parts, or combinations thereof.

[0063] Additionally, terms such as "...part," "...unit," and "...module" described in the specification refer to a unit that processes at least one function or operation, and this may be implemented in hardware, software, or a combination of hardware and software.

[0064] Additionally, in this specification, when a step is described as being located "before" or "after" another step, this includes not only cases where a step is in a direct chronological relationship with another step, but also cases where there is an indirect chronological relationship in which the chronological order of the two steps may change, such as a mixing step following each step.

[0065] Embodiments of the present invention will be described in detail below with reference to the attached drawings.

[0066] FIG. 1 is an exemplary diagram of an electrolytic copper foil production device having temperature control and copper foil width control functions according to an embodiment of the present invention, FIG. 2 is a perspective view of an electrolytic copper foil production device having temperature control and copper foil width control functions according to an embodiment of the present invention, and FIG. 3 is an exemplary diagram of a temperature control unit according to an embodiment of the present invention.

[0067] Referring to FIGS. 1 to 3, an electrolytic copper foil production device (100) having temperature control and copper foil width control functions may include a water tank section (110), a drum section (120), an anode section (130), a temperature control section (140), an electrolyte supply section (150), an electrolyte discharge section (160), and a winding section (170).

[0068] The above-mentioned tank portion (110) can be provided to accommodate an electrolyte (1) inside.

[0069] Here, the electrolyte (1) can be prepared as a copper sulfate solution.

[0070] The drum portion (120) is provided inside the water tank portion and can be provided to electrodeposit a copper foil (2) using the electrolyte (1).

[0071] The drum portion (120) may include a drum body (121), a rotating shaft (122), and a cathode material (123).

[0072] The drum body (121) is provided in a cylindrical shape and can be provided so that electrodeposition is performed on the outer surface of the drum. The drum body (121) can be provided so that the electrodeposited copper foil (2) is maintained at a constant level and so that the copper foil (2) can be continuously formed as it rotates.

[0073] The above-mentioned rotation axis (122) can be configured to pass through the center of the drum body (121) to enable rotational movement of the drum body (121).

[0074] The above-mentioned rotating shaft (122) rotates in conjunction with the drum body (121), thereby enabling a continuous copper foil electrodeposition process to be performed on the drum body (121).

[0075] The above cathode material (123) is formed along the outer surface of the drum body (121) and can be arranged to serve as a cathode for electrodepositing copper foil.

[0076] The above-mentioned cathode material (123) can form a copper foil (2) through a reaction with the electrolyte (1), and the electrodeposited copper foil (2) can be formed with a uniform thickness in accordance with the rotational movement of the drum body (121).

[0077] The drum portion (120) provided in this manner can induce electrical movement from the negative electrode to the positive electrode through an electric current within the electrolyte, thereby allowing the copper foil (2) to be electrodeposited on the drum portion (120).

[0078] The anode portion (130) is provided at the bottom of the drum portion (120) and can be formed to have a curvature corresponding to the curvature of the drum portion (120). Additionally, the upper surface of the anode portion (130) can be provided to be spaced apart from the outer surface of the drum portion (120) at a constant distance.

[0079] Additionally, the anode portion (130) is provided as a pair and may be formed spaced apart from each other so that the electrolyte (1) can flow between the drum portion (120) and the anode portion (130).

[0080] The anode portion (130) provided in this manner serves to supply current and can interact with the cathode material (123) of the drum portion (120) through the electrolyte (1) to allow the copper foil to be electrodeposited.

[0081] The above anode (130) may be made of an insoluble electrode (20) manufactured by coating an electrode substrate (10) made of titanium with a coating solution containing iridium.

[0082] The above temperature control unit (140) is provided as a pair at the bottom of the anode unit (130) and may include a base (141), a tube (142), a heat medium inlet (143), a heat medium outlet (144), a sensor module (145), and a control module (146).

[0083] The above base (141) may be provided with a curved surface having a curvature corresponding to the anode (130) so that the anode (130) is coupled to the upper surface.

[0084] The above tube (142) is provided inside the base (141) and may be formed to extend in a zigzag shape along the length or width direction of the base (141). At this time, the length or width direction spacing of the parallel tubes (142) may be provided uniformly so that heat exchange is performed uniformly.

[0085] Additionally, a heat transfer medium may be provided to flow inside the tube (142). Furthermore, the heat transfer medium may be provided to exchange heat with the electrolyte while moving along the tube (142).

[0086] Meanwhile, a plurality of heat exchange fins may be further provided on the lower surface of the base (141). The heat exchange fins provided in this manner increase the contact area between the electrolyte (1) and the temperature control unit (140), thereby allowing the heat transferred by the tube (142) to be exchanged more quickly and evenly.

[0087] The above heat medium inlet (143) is provided on one side of the tube (142) to allow the heat medium to flow into the tube (142).

[0088] The above heat medium discharge port (144) is provided on the other side of the tube (142) to allow the heat medium, after heat exchange of the tube (142) is completed, to be discharged.

[0089] The heat medium discharged through the heat medium outlet (144) can be heated or cooled to reach a preset temperature and then flow into the tube (142) through the heat medium inlet (143) to be circulated.

[0090] The sensor module (145) may be configured to measure the temperature of the electrolyte in real time. The sensor module (145) may be configured to provide data regarding the measured temperature change to the control module (146).

[0091] The control module (146) may be configured to control the temperature of the heat medium circulating through the tube (142) so that the temperature of the electrolyte (1) maintains a preset temperature based on temperature data measured by the sensor module (145).

[0092] For example, the temperature of the above electrolyte (1) can be controlled to 49.5 to 50.5 degrees.

[0093] The above temperature control unit (140) is provided as a pair spaced apart from each other, and can be configured so that the electrolyte (1) is supplied between the drum unit (120) and the anode unit (130) through a hollow portion formed spaced apart from each other.

[0094] The above electrolyte supply unit (150) may be connected to an electrolyte tank and configured to supply the electrolyte (1) into the interior of the water tank unit (110). The above electrolyte supply unit (150) may be configured to be located at the bottom of the water tank unit (110) and to supply the electrolyte between the drum unit (120) and the anode unit (130) inside the water tank unit (110).

[0095] The above electrolyte discharge section (160) is provided on the side of the above water tank section (110) and can be provided to discharge the electrolyte (1) overflowing from the above water tank section (110) to the outside.

[0096] The above electrolyte discharge section (160) may include a discharge body (161) and an electrolyte discharge port (162).

[0097] The above discharge body (161) is provided on the outer circumference of the above tank section (110) and can be provided to receive the electrolyte (1) overflowing outside the above tank section (110).

[0098] The above electrolyte discharge port (162) may be provided at the bottom of the discharge body (161) to discharge the electrolyte (1) contained in the discharge body (161) into the electrolyte tank.

[0099] At this time, the above electrolyte tank may be further provided with a configuration for pre-treating the discharged electrolyte by filtering and cooling it so that it can be recycled.

[0100] The above winding unit (170) may be configured to transfer the copper foil (2) generated in the drum unit (120) to the core and wind it. The copper foil (2) generated in the drum unit (120) is stably transferred through the winding unit (170), and can be wound while maintaining a constant tension so as not to damage the copper foil during this process.

[0101] Meanwhile, the winding unit (170) may additionally be equipped with a winding control system. The winding control system can control the tension of the copper foil to be maintained at a constant level when the winding unit (170) winds the copper foil. In particular, the winding control system may be configured to measure the thickness and condition of the copper foil (2) in real time and automatically adjust the winding speed. The winding control system configured in this way can prevent damage to the copper foil (2) and increase production efficiency.

[0102] The electrolytic copper foil production device (100) having the above-mentioned temperature control and copper foil width control functions has the effect of maintaining the quality of the produced copper foil (2) uniformly by uniformly controlling the temperature of the electrolyte (1).

[0103] FIG. 4 is a perspective view of an anode portion having a barrier formed thereon according to an embodiment of the present invention.

[0104] Meanwhile, referring to FIG. 4, a barrier (180) may be provided to be attached to the anode (130).

[0105] Specifically, in the past, while the length of the copper foil (2) formed could be easily adjusted, there was a difficulty in the past in that a separate facility had to be provided to adjust the width of the copper foil (2).

[0106] However, according to the present invention, as shown in FIG. 4, a barrier film (180) may be attached to the side of the anode (130) so that the anode (130) is exposed by a width equal to the width of the copper foil (2) to be produced.

[0107] In this way, the anode portion (130), which is partially covered by the barrier (180), can be made so that the copper foil (2) is generated by electrical reaction only in the exposed area.

[0108] Alternatively, the anode portion (130) may be provided by combining multiple anode segments (not shown) divided along the width direction in a modular manner.

[0109] The anode portion (130) provided in this manner can be controlled so that the electrode is activated only in the anode splitter corresponding to the width of the copper foil (2) to be manufactured.

[0110] For example, if the total width of the anode portion (130) is 1m and the width of the copper foil (2) to be manufactured is 80cm, the electrodes of the anode splitters located on both sides may be kept in an inactive state, and only the electrodes of the anode splitters corresponding to 40cm from the center on both sides may be activated to manufacture the copper foil (2).

[0111] The present invention, prepared in this manner, has the effect of flexibly responding to the width of the copper foil (2) requested by the customer and reducing equipment costs.

[0112] Hereinafter, a method for manufacturing the insoluble electrode (20) constituting the anode portion (130) will be explained with reference to the following drawings.

[0113] FIG. 5 is a process example diagram of a method for manufacturing an insoluble electrode for manufacturing electrolytic copper foil according to an embodiment of the present invention, and FIG. 6 is a flowchart of a method for manufacturing an insoluble electrode for manufacturing electrolytic copper foil according to an embodiment of the present invention.

[0114] Referring to FIGS. 5 and 6, a method for manufacturing an insoluble electrode for manufacturing electrolytic copper foil may include a step (S10) of pre-treating an electrode substrate, a step (S20) of preparing a coating solution for coating the pre-treated electrode substrate, and a step (S30) of coating the electrode substrate with the prepared coating solution to produce an insoluble electrode.

[0115] FIG. 7 is a flowchart of the steps for pre-processing an electrode substrate according to an embodiment of the present invention.

[0116] Referring to FIG. 7, the step (S10) of pre-treating the electrode substrate may include a step (S11) of sandblasting the electrode substrate to create an uneven surface (S11), a step (S12) of first washing the electrode substrate with the created uneven surface (S12), a step (S13) of etching the washed electrode substrate, a step (S14) of second washing the etched electrode substrate, and a step (S15) of drying the electrode substrate that has undergone second washing.

[0117] First, in the step (S11) where a sandblasting process is performed on the electrode substrate to create an uneven surface, the electrode substrate (10) may be made of titanium material. For example, the electrode substrate (10) may be made of ASME B265-Gr.1.

[0118] In addition, an uneven surface (20) can be created on the electrode substrate (10) by a sandblasting process. At this time, the sandblasting process can be performed using an alumina oxide abrasive. In addition, the brown alumina particle size can be #80, #100, and #150 so that a uniform roughness within an error range of 8 to 15 Ra can be applied to each substrate.

[0119] Next, in the step (S12) where a first cleaning is performed on the electrode substrate with the uneven surface, high-pressure water cleaning and ultrasonic cleaning of the electrode substrate (10) may be performed.

[0120] At this time, the ultrasonic cleaning may be arranged so that the electrode substrate (10) is immersed in a cleaning solution diluted with an alkaline cleaning agent and hot water, and the cleaning is performed at a frequency of 30 to 40 kHz for 30 to 60 minutes.

[0121] In addition, the above cleaning solution may be prepared by diluting an alkaline cleaning agent with hot water at a ratio of 1:30.

[0122] This primary cleaning can remove the alumina that has penetrated during the sandblasting process of the electrode substrate (10).

[0123] Next, in the step (S13) where etching is performed on the cleaned electrode substrate, the electrode substrate (10) may be etched.

[0124] In particular, etching is performed to create a pattern and structure of the electrode substrate (10), and appropriate temperature, chemical concentration, and pressure must be maintained in the etching chamber so that uniform and accurate etching is performed.

[0125] To this end, the electrode substrate (10) may be prepared to be etched for 10 to 25 minutes at a concentration of 25 to 30% in a temperature range of 30 to 80 degrees by an etching solution containing oxalic acid and hydrochloric acid (HCl) or sulfuric acid (H2SO4).

[0126] At this time, since the titanium metal surface may melt if the etching time is too long, a chemical reaction is induced between 10 and 25 minutes to obtain an appropriate roughness, and at the same time, a uniform roughness within an error range of 8 to 15 Ra can be obtained.

[0127] As such, the electrode substrate that has undergone acid etching is additionally given fine roughness along the roughness formed by sandblasting treatment, thereby improving the contact area between the electrode substrate and the coating layer.

[0128] Next, in the step (S14) where a second cleaning is performed on the electrode substrate that has been etched, high-pressure water cleaning and ultrasonic cleaning of the electrode substrate (10) may be performed.

[0129] At this time, the ultrasonic cleaning may be arranged so that the electrode substrate (10) is immersed in a cleaning solution diluted with an alkaline cleaning agent and hot water, and the cleaning is performed at a frequency of 30 to 40 kHz for 30 to 60 minutes.

[0130] In addition, the above cleaning solution may be prepared by diluting an alkaline cleaning agent with hot water at a ratio of 1:30.

[0131] As such, ultrasonic cleaning performed with a cleaning solution containing an alkaline cleaning agent can dissolve and remove contaminants.

[0132] Next, in the step (S15) where the electrode substrate that has undergone the second washing is dried, the electrode substrate (10) that has undergone the second washing can be completely dried. Specifically, the electrode substrate (10) that has undergone the second washing can be arranged to be completely dried in an oven at a temperature of 70 to 150 degrees for at least 20 minutes.

[0133] FIG. 8 is a flowchart of the steps for preparing a coating solution for coating a pretreated electrode substrate according to an embodiment of the present invention.

[0134] Referring to FIG. 8, the step (S20) of manufacturing an insoluble electrode by coating an electrode substrate with a manufactured coating solution may include a step (S21) of mixing two or more elements among platinum group elements, iridium oxide (Ir), ruthenium chloride (Ru), platinum (Pt), and tantalum chloride (Ta) to form a mixture, a step (S22) of stirring the mixture with alcohol and dissolving the elements, and a step (S23) of irradiating the dissolved elements with ultrasound to manufacture the coating solution.

[0135] First, in the step (S21) of forming a mixture by mixing two or more elements among the platinum group elements, iridium oxide (Ir), ruthenium chloride (Ru), platinum (Pt), and tantalum chloride (Ta), the method may be configured to form a mixture by mixing two or more elements among the platinum group elements, iridium oxide (Ir), ruthenium chloride (Ru), platinum (Pt), and tantalum chloride (Ta).

[0136] Here, when making electrodes with iridium chloride (IrCl3, IrCl4, IrCl5) and iridium oxide (IrO2, IrO3, IrO5), iridium can be used as a mixture of two or more of tantalum chloride (TaCl2, TaCl3, TaCl4, TaCl5), tantalum oxide (TaO2, TaO3, TaO4, TaO5) and ruthenium chloride (Ru) to increase the life of the electrode in a corrosive environment.

[0137] Iridium chlorides (IrCl3, IrCl4, IrCl5) are relatively resistant to corrosive environments and possess high electrochemical reactivity, characterized by oxygen generation and low voltage, allowing for both direct and indirect reactions with contaminants.

[0138] Next, in the step (S22) where the mixture is stirred with alcohol and the element is dissolved, the mixture may be stirred with alcohol to dissolve the element.

[0139] For example, iridium, which is the main catalyst of the coating solution, and tantalum, which is the binder, can be prepared to be dissolved in alcohol in weight ratios of 70:30, 60:40, and 50:50.

[0140] At this time, the mixture may be prepared to be dissolved by stirring at 260 to 550 RPM at a temperature of 30 to 50 degrees in the alcohol for 2 to 4 hours.

[0141] In addition, the above alcohol may be prepared as one or more of isopropyl alcohol, chlorine, butanol, and ethanol.

[0142] In addition, if the viscosity of the mixed metal oxide coating solution used in the present invention is high, the coating power is good, but the bonding strength of the surface area of ​​the pretreated electrode substrate (10) is lowered, and if the viscosity of the coating solution is low, the problem of spreading occurs in the coating phenomenon, so the optimal viscosity of the coating solution can be manufactured to have 5,000 to 8,000 cps (centipoise).

[0143] Next, in the step (S23) where a coating solution is prepared by irradiating the dissolved elements with ultrasound, each dissolved element may be irradiated with ultrasound of 20 kHz to 50 kHz through ultrasonic dispersion to undergo the steps of particle dispersion, cell crushing, particle grinding, and homogenization by repeatedly applying intense pressure and depressurization.

[0144] At this time, the usage period and usage conditions are determined by the irradiation time, interval, and frequency according to the components of the solution, and can be arranged to make the particle size ultrafine, such as nano-size and smaller.

[0145] And, in the step (S23) where the coating solution is prepared by irradiating the dissolved element with ultrasound, the coating solution may be prepared by irradiating the dissolved element with ultrasound 2 to 5 times repeatedly at a frequency of 20 to 50 kHz for 20 to 60 minutes.

[0146] FIG. 9 is a flowchart of the steps for manufacturing an insoluble electrode by coating an electrode substrate with a coating solution prepared according to an embodiment of the present invention.

[0147] Referring to FIG. 9, the step (S30) of manufacturing an insoluble electrode by coating an electrode substrate with a manufactured coating solution may include: a step (S31) of applying a coating solution to a pretreated electrode substrate; a step (S32) of drying the electrode substrate coated with the coating solution; a step (S33) of performing heat treatment on the dried electrode substrate; a step (S34) of sequentially repeating the steps of applying the coating solution, drying the electrode substrate, and performing heat treatment until a coating layer of a preset thickness is formed; and a step (S35) of manufacturing an insoluble electrode by performing a heat sintering process when a coating layer of a preset thickness is formed.

[0148] First, in the step (S31) where a coating solution is applied to a pretreated electrode substrate, a coating solution prepared by the method described above may be applied to the pretreated electrode substrate (10).

[0149] At this time, application methods can be achieved using techniques such as spraying, brushing, rolling, and dipping.

[0150] Spray coating is an economical method that allows for uniform and stable coating on the surface by spraying the coating solution onto the electrode substrate (10) with a spray nozzle in nano-sized particles, and is suitable for mass production with minimal loss of solution.

[0151] Brushing coating is a method of applying a coating solution to an electrode substrate (10) with a brush. Although the coating method is simple and cost-effective, the material of the brush and the skill level of the operator are required to obtain a certain quality and depending on the product.

[0152] Rolling coating is a method of applying a solution to an electrode substrate (10) with a roller. Although the coating method is simple and cost-effective, the material of the roller and the skill of the operator are required to ensure consistent quality and the desired product.

[0153] Dipping coating is a method of obtaining a coating film by immersing an electrode substrate in a coating solution to form a precursor layer on the surface of the material and then firing it at a suitable temperature. It is used for relatively small products and is one of the economical methods because, compared to spray coating, the surface is relatively uniform and the loss of coating solution can be reduced.

[0154] In the step (S31) where a coating solution is applied to the pretreated electrode substrate, the coating solution prepared may be applied or sprayed onto the surface of the pretreated electrode substrate (10) using any one of these methods.

[0155] At this time, 2g / m² of the coating solution is applied once. 2 Thickness greater than or equal to this can be applied.

[0156] Next, in the step (S32) where the electrode substrate coated with the coating solution is dried, the electrode substrate (10) coated or sprayed with the coating solution may be dried. At this time, the drying temperature may be set to a temperature of 60 to 90°C and may be set to be dried for 10 to 20 minutes.

[0157] Next, in the step (S33) where heat treatment is performed on the dried electrode substrate, the dried electrode substrate (10) may be heat-treated within a temperature range of 400 to 650 degrees.

[0158] Next, in the step (S34) in which the steps of applying a coating solution, drying an electrode substrate, and performing heat treatment are repeated sequentially until a coating layer of a preset thickness is formed, the steps of applying a coating solution to a pretreated electrode substrate (S31), drying an electrode substrate with the applied coating solution (S32), and performing heat treatment on a dried electrode substrate (S33) may be arranged to be repeated sequentially 5 to 10 times until a coating layer of a preset thickness is formed.

[0159] At this time, the preset final coating thickness can be set to a range of 3 to 6 μm.

[0160] Next, in the step (S35) where a coating layer of a predetermined thickness is formed and a heat sintering process is performed to manufacture an insoluble electrode, if the predetermined final coating thickness is satisfied, the coating liquid application, drying, and heat treatment processes for the electrode substrate (10) may be stopped and the final heat sintering may be performed to manufacture the insoluble electrode (20).

[0161] At this time, the heat sintering process may be arranged to be carried out for 30 to 90 minutes within a temperature range of 550°C to 850°C.

[0162] The lifespan of the insoluble electrode (20) prepared in this way can be measured in the following way.

[0163] First, a specimen with a width of 25 mm x a height of 25 mm is prepared, and the electrolytic solution is an electrolytic cell with a sulfuric acid concentration of 22% or less. The specimen spacing is set to 20 mm, the current density is 700 ASD or less, the operating temperature is 90°C or less, and the voltage is 10 V or less, so that the lifespan of the insoluble electrode (20) can be checked. The lifespan test is conducted until a rapid reaction occurs in the voltage graph, and when a rapid reaction occurs, it can be determined that the lifespan has ended.

[0164] FIG. 10 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 200x magnification to confirm the microstructure and elemental composition of an insoluble substrate according to the present invention.

[0165] Figure 11 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 500x magnification to confirm the microstructure and elemental composition of an insoluble substrate according to the present invention.

[0166] FIG. 12 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 2,000x magnification to confirm the microstructure and elemental composition of an insoluble substrate according to the present invention.

[0167] FIG. 13 is an image of SE (Secondary Electrons) and BSE (Backscattered Electrons) taken with a scanning electron microscope at 10,000x magnification to confirm the microstructure and elemental composition of the insoluble substrate according to the present invention.

[0168] Referring to Figures 10 to 13, the microstructure and composition of the specimen surface were confirmed using a scanning electron microscope. The analysis conditions were Acc. Voltage: 3kV, Current: 1.6nA, and Magnification 200x / 500x / 2000x / 5000x / 10000x. At this time, it can be seen that different morphologies were observed in each region at 2,000x and 10,000x magnifications.

[0169] FIG. 14 is a graph showing the qualitative or quantitative analysis of elements on the surface of a material using an Energy Dospersive Spectroscope for an insoluble substrate according to the present invention.

[0170] Referring to Fig. 14, elements on the surface of the material were qualitatively or quantitatively analyzed using an Energy Dospersive Spectroscope. The analysis conditions were surface analysis and depth profile, with an etching time of 5 sec / 5 times.

[0171] FIG. 15 is an image taken at 5,000x magnification with a scanning electron microscope to confirm the elemental composition of the insoluble substrate according to the present invention, and FIG. 16 is an image taken to confirm the molecular structure and crystal structure of the mixture of the insoluble substrate according to the present invention.

[0172] Figures 17 and 18 are images taken to confirm the molecular structure and crystal structure of iridium and tantalum when mixed together.

[0173] Referring to Figures 15 to 18, to confirm the molecular structure and crystal structure when iridium and tantalum are mixed, 2400g of paper and 2400g of slide glass were measured, and the analysis conditions were Laser: 532nm, Exposure time: 0.3s, Number of accumulation: 10, Accumulation cycle: 1s, ND Filter: 10%.

[0174] Figures 19 to 21 are images of an insoluble substrate taken by an X-ray photoelectron spectrometer.

[0175] Referring to FIGS. 19 to 21, an X-ray Photoelectron Spectroscope (XPS) is used to determine the composition and chemical bonding state of a sample surface and to measure the depth profile of each element by measuring the energy of photoelectrons emitted after X-rays are incident on the surface of a sample.

[0176] The analysis conditions were surface analysis and depth profile, and etching time: 5 sec / 5 times.

[0177] Figure 22 is a table showing the effect of pretreatment on the electrode substrate, Figure 23 is a table showing the effect of coating solution on the electrode substrate, and Figure 24 is a table showing the effect of drying and heat treatment on the electrode substrate.

[0178] The effect of the present invention according to the above configuration is that the speed and efficiency of the electrochemical reaction can be increased by using an insoluble titanium substrate coated with a platinum compound. This can improve productivity by increasing the electrodeposition rate of copper during the production of electrolytic copper foil.

[0179] In addition, according to the present invention, corrosion or performance degradation of the electrode can be minimized by coating the anode with iridium oxide, which has resistance to oxygen generation. This ensures the stability of the electrode during the electrolytic copper foil manufacturing process, enabling long-term use.

[0180] In addition, according to the present invention, the quality of the electrolytic copper foil produced is improved due to the high reactivity and stability of the insoluble electrode (20). High-quality copper foil increases applicability in the electronic device and battery industries and contributes to maximizing the performance of the final product.

[0181] Furthermore, according to the present invention, in addition to the production of electrolytic copper foil, it can be applied to various fields such as brine electrolysis, wastewater treatment, and electrochemical cleaning. This versatility increases the potential for commercialization of the technology and can promote its utilization in various industrial sectors.

[0182] Although the foregoing description of the present invention has been illustrated with reference to the drawings, it is for illustrative purposes only, and those skilled in the art will understand that other specific forms can be easily modified without altering the technical spirit or essential features of the invention. Therefore, the embodiments described above should be understood as illustrative in all respects and not restrictive. For example, each component described as a single unit may be implemented in a distributed manner, and components described as distributed may likewise be implemented in a combined form. Furthermore, the described techniques may be performed in a different order than the described method.

[0183] The embodiments described in this specification and the accompanying drawings are merely illustrative of some of the technical ideas included in the present invention. Accordingly, the scope of the present invention is defined by the claims set forth below, and all modifications or variations derived from the meaning and scope of the claims and equivalent concepts thereof should be interpreted as being included within the scope of the present invention.

[0184]

[0185] <Explanation of Symbols>

[0186] 1: Electrolyte

[0187] 2: Copper foil

[0188] 10: Electrode substrate

[0189] 11: Uneven parts

[0190] 20: Insoluble electrode

[0191] 100: Electrolytic copper foil production device with temperature control and copper foil width adjustment functions

[0192] 110: Water tank

[0193] 120: Drum section

[0194] 121: Drum body

[0195] 122: Rotation axis

[0196] 123: Cathode material

[0197] 130: Anode

[0198] 140: Temperature control unit

[0199] 141: Bass

[0200] 142: Tube

[0201] 143: Heat transfer fluid inlet

[0202] 144: Heat transfer fluid outlet

[0203] 145: Sensor module

[0204] 146: Control Module

[0205] 150: Electrolyte supply unit

[0206] 160: Electrolyte discharge section

[0207] 161: Exhaust

[0208] 162: Electrolyte outlet

[0209] 170: Winding section

Claims

1. A tank section containing an electrolyte inside; A drum section provided inside the above-mentioned tank section and configured to electrodeposit copper foil using the above-mentioned electrolyte; An anode portion provided inside the above-mentioned tank portion and connected to the drum portion through the electrolyte at the bottom of the above-mentioned drum portion; and Electrolytic copper foil production device having temperature control and copper foil width adjustment functions, characterized by including a temperature control unit provided at the lower part of the anode portion.

2. In Paragraph 1, The above temperature control unit is, A base provided with a curved surface so that the above positive electrode is coupled to the upper surface; A tube provided inside the above base; A heat transfer medium inlet provided on one side of the above tube; and It includes a heat medium discharge port provided on the other side of the above tube, Electrolytic copper foil production device having temperature control and copper foil width control functions, characterized by being configured to allow a heat medium to circulate inside the above-mentioned tube.

3. In Paragraph 2, The above temperature control unit is, A sensor module for measuring the temperature of the above electrolyte; and An electrolytic copper foil production apparatus having temperature control and copper foil width control functions, characterized by including a control module provided to control the temperature of a heat medium circulating through the tube so that the temperature of the electrolyte measured by the sensor module above maintains a preset temperature.

4. In Paragraph 2, The above temperature control unit is, Electrolytic copper foil production device having temperature control and copper foil width control functions, characterized by being arranged as a pair spaced apart from each other, and arranged so that the electrolyte is supplied between the drum part and the anode part through a hollow portion formed spaced apart from each other.

5. In Paragraph 1, Electrolytic copper foil production device having temperature control and copper foil width control functions, characterized in that the drum portion and the anode portion are formed spaced apart from each other by a predetermined distance to allow the electrolyte to flow in.

6. In Paragraph 1, Electrolyte supply unit provided to supply electrolyte into the interior of the above-mentioned tank unit; and Electrolytic copper foil production device having temperature control and copper foil width control functions, characterized by including an electrolyte discharge section provided on the side of the above-mentioned tank section and configured to discharge the electrolyte overflowing from the above-mentioned tank section to the outside.

7. In Paragraph 6, The above electrolyte discharge unit is, A discharge body provided on the outer perimeter of the above-mentioned tank portion and receiving the electrolyte overflowing from the above-mentioned tank portion; and Electrolytic copper foil production device having temperature control and copper foil width control functions, characterized by including an electrolyte discharge port provided at the bottom of the discharge body.

8. In Paragraph 1, Electrolytic copper foil production apparatus having temperature control and copper foil width control functions, characterized by further including a winding unit configured to transfer and wind the copper foil generated in the above drum unit to a core.

9. In Paragraph 1, The above drum section is, A cylindrical drum body arranged to rotate in one direction; A rotating shaft formed by penetrating the center of the drum body; and Electrolytic copper foil production apparatus having temperature control and copper foil width control functions, characterized by including a cathode material formed along the outer surface of the drum body.

10. In Paragraph 1, The above anode is, Electrolytic copper foil production apparatus having temperature control and copper foil width control functions, characterized by being provided with an insoluble electrode formed by coating a coating solution of an anode material onto an electrode substrate made of titanium material.

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