METHOD FOR HANDLING A LIQUID FOR ELECTROLYTIC SEPARATION, AND DEVICE FOR ELECTROLYTIC SEPARATION

Abstract

A method for handling a dispersion for electrolytic deposition is used in the case where an electrolytic deposition film is formed on a support with conductive properties by anionic electrolytic deposition, and the method includes: adjusting the concentration of an organic acid contained in the dispersion for electrolytic deposition by subjecting the dispersion for electrolytic deposition to an anion exchange treatment.An electrolytic deposition device (10) is used in the case where an electrolytic deposition film is formed on a support with conductive properties by anionic electrolytic deposition, and the electrolytic deposition device includes: an electrolytic deposition container (20) in which an electrolytic deposition dispersion is stored and into which a support and a counter electrode are immersed; an anion exchange device (30) to subject the electrolytic deposition dispersion to an anion exchange treatment; and a circulation device for the electrolytic deposition dispersion (40) to circulate the electrolytic deposition dispersion between the electrolytic deposition container (20) and the anion exchange device (30).

Description

TECHNICAL AREA

[0001] The present invention relates to a method for handling a dispersion for electrolytic deposition, which is used in the electrolytic deposition of an electrolytic deposition film onto a substrate with conductive properties by anionic electrolytic deposition, and to a device for electrolytic deposition.

[0002] The present application claims priority over Japanese patent application No. 2023-070848, filed on April 24, 2023, and Japanese patent application No. 2024-017168, filed on February 7, 2024, the contents of which are hereby incorporated by reference. STATE OF THE ART

[0003] An insulated conductor, in which a support with conductive properties is coated with an insulating film consisting of an insulating resin, is widely used as a conductive material or as a heat dissipation plate material for various types of electrical equipment requiring insulation.

[0004] Various resins are used as components of the insulating film, and for example, patent document 1 discloses the use of a polyimide resin, such as a polyamide-imide resin, and patent document 2 proposes the use of a mixed resin consisting of a polyimide resin and a fluoropolymer resin.

[0005] A method for forming the insulating film, which consists of such an insulating resin, on a surface of the support with conductive properties is known as an electrolytic deposition method.

[0006] In the electrolytic deposition process, the substrate on which the insulating film is to be formed and a counter electrode are immersed in the electrolytic deposition dispersion in which the insulating film materials are dispersed. A voltage is applied between the substrate and the counter electrode to deposit the insulating film materials onto the substrate surface, thereby forming the electrolytic deposition film. The electrolytic deposition film is then heated to fuse the insulating film to the substrate, thus forming the insulating film.

[0007] Other examples of the electrolytic deposition process include an anionic electrolytic deposition process, in which a voltage is applied to the support as the anode to form the insulating film on the surface of the support, and a cationic electrolytic deposition process, in which a voltage is applied to the support as the cathode to form the insulating film on the surface of the support. Citation list of patent documents Patent document 1: Unexamined Japanese patent application, first publication no. 2017-115120 Patent document 2: Japanese unexamined patent application, first publication no. 2018-070663 SUMMARY OF THE INVENTION Technical Task

[0008] A dispersion for anionic electrolytic deposition, used in the anionic electrolytic deposition process, contains a solid component containing the resin described above, water, an organic solvent, and a neutralizing agent. The pH is lowered near the surface of the anode (support) by applying a voltage, the solid component is deposited on the surface of the anode (support), and the electrolytic deposition film is formed.

[0009] If the electrolytic deposition is carried out continuously using the anionic electrolytic deposition method, there is a risk that blistering will occur if the electrolytic deposition film is baked onto the surface of the anode to form the insulating film.

[0010] The present invention was made in view of the circumstances described above, and an objective of the present invention is to provide a method for handling a dispersion for electrolytic deposition and an apparatus for electrolytic deposition, with which the occurrence of bubble formation can be suppressed when an electrolytic deposition film is baked on, and an insulating film can be formed stably. Solution to the task

[0011] As a result of intensive investigations carried out by the present inventors to achieve the above-described objective, it was found that in a case where electrolytic deposition is carried out continuously using the anionic electrolytic deposition method, the concentration of the organic acid contained in the dispersion for electrolytic deposition increases, and blistering occurs when the electrolytic deposition film is baked on.

[0012] Therefore, it was found that the occurrence of blistering during baking can be suppressed by appropriately controlling the concentration of the organic acid contained in the dispersion for electrolytic deposition.

[0013] The present invention was made on the basis of the findings described above, and one aspect 1 of the present invention is a method for handling a dispersion for electrolytic deposition, which is used in the case in which an electrolytic deposition film is formed on a support with conductive properties by anionic electrolytic deposition, wherein the method comprises: adjusting a concentration of an organic acid contained in the dispersion for electrolytic deposition by subjecting the dispersion for electrolytic deposition to an anion exchange treatment.

[0014] In the method for handling a dispersion for electrolytic deposition according to aspect 1 of the present invention, since the concentration of the organic acid contained in the dispersion for electrolytic deposition is controlled, even in a case where the electrolytic deposition is carried out continuously, the concentration of the organic acid is not excessively increased, and it is possible to suppress the occurrence of bubble formation during baking, and it is possible to form the insulating film stably.

[0015] An aspect 2 of the present invention is the method for handling a dispersion for electrolytic deposition according to aspect 1 of the present invention, wherein the dispersion for electrolytic deposition comprises water, an organic solvent, a solid component and a neutralizing agent, and the solid component includes at least one polyimide resin.

[0016] In the method for handling a dispersion for electrolytic deposition according to aspect 2 of the present invention, since the dispersion for electrolytic deposition contains at least the polyimide resin as a solid component, it is possible to form the insulating film with excellent insulating properties in a stable manner.

[0017] An aspect 3 of the present invention is the method for handling a dispersion for electrolytic deposition according to aspect 1 or 2 of the present invention, wherein the dispersion for electrolytic deposition contains at least one carboxylic acid as an organic acid.

[0018] In the method for handling a dispersion for electrolytic deposition according to aspect 3 of the present invention, since the dispersion for electrolytic deposition contains at least the carboxylic acid as an organic acid, a rapid drop in pH at the surface of the anode (the support) can be suppressed by the pH buffering effect of the carboxylic acid, which is the organic acid, and it is possible to form the electrolytic deposition film stably.

[0019] An aspect 4 of the present invention is the method for handling a dispersion for electrolytic deposition according to aspect 1 or 2 of the present invention, wherein the dispersion for electrolytic deposition contains at least one hydroxy acid as an organic acid.

[0020] In the method for handling a dispersion for electrolytic deposition according to aspect 4 of the present invention, since the dispersion for electrolytic deposition contains at least the hydroxy acid as an organic acid, a rapid drop in pH at the surface of the anode (the support) can be suppressed by the pH buffering effect of the hydroxy acid, which is the organic acid, and it is possible to form the electrolytic deposition film stably.

[0021] An aspect 5 of the present invention is the method for handling a dispersion for electrolytic deposition according to one of aspects 1 to 4 of the present invention, wherein the concentration of the organic acid contained in the electrolytic deposition is adjusted to be in the range of 5 mg / L or more and 500 mg / L or less.

[0022] In the dispersion for electrolytic deposition according to aspect 5 of the present invention, since the concentration of the organic acid is adjusted to be in the range of 5 mg / L or more and 500 mg / L or less, it is possible to exert a suitable pH buffering effect, to form the electrolytic deposition film stably, and to selectively suppress the occurrence of bubble formation during curing.

[0023] An aspect 6 of the present invention is the method for handling a dispersion for electrolytic deposition according to one of aspects 1 to 5 of the present invention, wherein the dispersion for electrolytic deposition contains a fluorinated resin together with a polyimide resin as a solid component.

[0024] In the method for handling a dispersion for electrolytic deposition according to aspect 6 of the present invention, in which the fluorinated resin is included together with the polyimide resin as a solid component, the insulating film with particularly good insulating properties and dielectric properties can be formed.

[0025] An aspect 7 of the present invention is an electrolytic deposition apparatus used in a case where an electrolytic deposition film is formed on a support having conductive properties by anionic electrolytic deposition, the electrolytic deposition apparatus comprising: an electrolytic deposition container in which an electrolytic deposition dispersion is stored and into which a support and a counter electrode are immersed; an anion exchange device for subjecting the electrolytic deposition dispersion to an anion exchange treatment; and a circulation device for circulating the electrolytic deposition dispersion between the container and the anion exchange device.

[0026] Since the apparatus for electrolytic deposition according to aspect 7 of the present invention includes the vessel for electrolytic deposition, the anion exchange device for subjecting the dispersion for electrolytic deposition to anion exchange treatment, and the circulation device for the dispersion for electrolytic deposition for circulating the dispersion for electrolytic deposition between the vessel for electrolytic deposition and the anion exchange device, the concentration of the organic acid contained in the dispersion for electrolytic deposition can be appropriately controlled, and even in the case where the electrolytic deposition is carried out continuously, the concentration of the organic acid is not excessively increased, and the occurrence of bubble formation during baking can be suppressed.and the insulating film can be formed stably. Advantageous effects of the invention

[0027] According to the present invention, it is possible to provide a method for handling a dispersion for electrolytic deposition and a device for electrolytic deposition, with which the occurrence of bubble formation can be suppressed in the case in which the electrolytic deposition film is baked on, and the insulating film can be formed stably. BRIEF DESCRIPTION OF THE DRAWINGS [ Fig. 1] A flowchart showing a manufacturing process for insulating films using an electrolytic deposition apparatus according to an embodiment of the present invention. [ Fig. 2] A schematic explanatory diagram of the apparatus for electrolytic deposition according to an embodiment of the present invention. [ Fig. 3] A schematic explanatory diagram of a device for electrolytic deposition according to another embodiment of the present invention. DESCRIPTION OF THE EXECUTION FORMS

[0028] The following describes a method for handling a dispersion for electrolytic deposition and a device for electrolytic deposition according to an embodiment of the present invention.

[0029] The method for handling a dispersion for electrolytic deposition according to the present embodiment is a method for handling a dispersion for electrolytic deposition in the case that an electrolytic deposition film, serving as a precursor to an insulating film, is formed on a surface of a support with conductive properties.

[0030] In the present embodiment, the method serves to handle a dispersion for electrolytic deposition, which is used in an anionic electrolytic deposition process in which a voltage is applied to the support as the anode and an insulating film is formed on the surface of the support, which is the anode.

[0031] In the present embodiment, the dispersion to be handled for electrolytic deposition contains water, an organic solvent, a solid component and a neutralizing agent.

[0032] In the dispersion for electrolytic deposition according to the present embodiment, as described above, the dispersion for electrolytic deposition contains an amine as a neutralizing agent, since the dispersion is used in anionic electrolytic deposition.

[0033] Furthermore, the dispersion for electrolytic deposition according to the present embodiment can contain an organic acid in a suitable quantity from the outset.

[0034] By containing a suitable amount of organic acid in the electrolytic deposition film, it is possible to suppress the occurrence of fine cracks in a later described firing step S03.

[0035] An organic acid may contain at least one carboxylic acid. Examples of carboxylic acids include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, oxalic acid, malonic acid, benzoic acid, phthalic acid, trimellitic acid, hydroxy acids, and the like.

[0036] In particular, at least one carboxylic acid is preferably present as the organic acid. Examples of hydroxy acids include glycolic acid, hydroxypropionic acid, hydroxybutyric acid, tartronic acid, glyceric acid, and similar compounds. Furthermore, hydroxypropionic acid, hydroxybutyric acid, and the like exhibit effects independent of the functional group position, meaning that positional isomers also display the effect.

[0037] In the present embodiment, the solid component comprises at least one polyimide resin, and it is preferred that the solid component comprises two types of resins, namely a polyimide resin and a fluoropolymer resin.

[0038] In the present embodiment, examples of the polyimide resin include polyamideimide, polyetherimide, polyimide, and the like. Examples of fluoropolymer resins include polytetrafluoroethylene, perfluoroalkoxyalkane, and the like.

[0039] Furthermore, the average particle diameter of the solid component need only be 50 nm or more and 300 nm or less, preferably 50 nm or more and 250 nm or less, and even more preferably 50 nm or more and 200 nm or less. In addition, the standard deviation of the particle diameter of the solid component needs only be 250 nm or less, preferably 150 nm or less, and even more preferably 100 nm or less.

[0040] The polyimide resin and the fluoropolymer, which represent the solid components, are dispersed in the water and the organic solvent.

[0041] Examples of the organic solvent are N,N-dimethylacetamide, propylene carbonate, dimethyl sulfoxide, N,N-dimethylformamide, γ-butyrolactone, N-methyl-2-pyrrolidone, N-methyl-2-pyrrolidone and the like.

[0042] Furthermore, the water content in the dispersion for electrolytic deposition is preferably 15 wt.% or more, and particularly preferably 50 wt.% or more. In addition, the water content in the dispersion for electrolytic deposition is preferably 85 wt.% or less, and more preferably 75 wt.% or less.

[0043] Furthermore, the proportion of organic solvent in the dispersion for electrolytic deposition is preferably 15 wt.% or more and more preferably 50 wt.% or more. In addition, the proportion of organic solvent in the dispersion for electrolytic deposition is preferably 85 wt.% or less and more preferably 75 wt.% or less.

[0044] Next, the process for producing an insulating film using the dispersion for electrolytic deposition will be described with reference to Fig. 1 described.

[0045] As in Fig. As shown in Figure 1, the method for producing insulating films in the present embodiment includes a step for pretreating the surface S01, a step for forming an electrolytic deposition film S02 and a step for baking S03. (Step for surface pretreatment S01)

[0046] First, the substrate on which the electrolytic deposition film (insulation film) is to be formed is prepared.

[0047] This carrier has conductive properties and consists, for example, of a metallic material such as copper, a copper alloy, aluminum, or an aluminum alloy.

[0048] Then the surface of the carrier described above is treated with a surface treatment fluid such as an organic solvent or a surfactant to remove the adhering oil and grease or an oxidized film. (Step towards the formation of an electrolytic deposition film SO2)

[0049] Next, the support and a counter electrode are immersed in the electrolytic deposition dispersion according to the present embodiment, and a voltage is applied between the anode (support) and the cathode (counter electrode), with the support acting as the anode and the counter electrode as the cathode. As a result, the pH of the electrolytic deposition dispersion near the support decreases, and the solid component (in the present embodiment, a mixture of the polyimide resin and the fluorinated resin) is deposited on the surface of the support. Consequently, the electrolytic deposition film forms on the surface of the support. Since, in this case, the organic acid is added to the electrolytic deposition dispersion in the present embodiment, the organic solvent is adequately contained in the electrolytic deposition film due to the pH-buffering effect of the organic acid.

[0050] The temperature (liquid temperature) of the dispersion for electrolytic deposition in step S02 for the formation of the electrolytic deposition film is preferably set to be in a range of 5°C or higher and 35°C or lower.

[0051] Setting the liquid temperature to 5°C or higher prevents water from mixing into the electrolytic deposition dispersion due to condensation. Conversely, setting the liquid temperature to 35°C or lower improves the storage stability of the electrolytic deposition dispersion and allows for stable electrolytic film formation.

[0052] The applied voltage between the carrier (anode) and the counter electrode (cathode) in the step to form the electrolytic deposition film S02 is preferably in the range of 10 V or more and 600 V or less.

[0053] Setting the applied voltage to 10 V or more ensures electrolytic deposition and improves productivity. Conversely, setting the applied voltage to 600 V or less suppresses the formation of numerous bubbles on the substrate surface, and in the subsequent curing step S03, it suppresses the occurrence of a large number of irregular structures in the insulating film due to bubble bursting. (Burning step S03)

[0054] In the curing step S03, the support on which the electrolytic deposition film containing the solid component is formed in step S02 to form the insulating film is dried, for example, in a temperature range of 200°C or higher and equal to or lower than the melting point of the solid component, the remaining dispersion for the electrolytic deposition is removed, and then the insulating film is cured onto the support to form the insulating film.

[0055] The curing temperature in curing step S03 can be any temperature range in which the electrolytic deposition film of the solid component is formed and the insulating film is formed on the substrate, and only needs to be within a range of, for example, 200°C or higher and 400°C or lower. Furthermore, the curing time only needs to be within a range of, for example, 0.5 minutes or more and 60 minutes or less.

[0056] The steps described above form the insulating film containing the solid component on the substrate with conductive properties.

[0057] In a case where electrolytic deposition is carried out continuously, the organic acid, such as the carboxylic acid, is generated, and the concentration of the organic acid contained in the electrolytic deposition dispersion increases. In this case, there is a concern that blistering may occur during the curing of the electrolytic deposition film.

[0058] Therefore, in the present embodiment, the dispersion for electrolytic deposition is handled in such a way that the concentration of the organic acid contained in the dispersion for electrolytic deposition is controlled.

[0059] The following describes the device for electrolytic deposition 10 according to the present embodiment and the method for handling a dispersion for electrolytic deposition using the device for electrolytic deposition 30 with reference to Fig. 2 described.

[0060] The in Fig.2 The device for electrolytic deposition 10 shown comprises a container for electrolytic deposition (20) in which the dispersion for electrolytic deposition is stored and into which a support and a counter electrode are immersed, an anion exchange device (30) to subject the dispersion for electrolytic deposition to an anion exchange treatment, and a circulation device for the dispersion for electrolytic deposition (40) (supply line (41) and return line (42)) to circulate the dispersion for electrolytic deposition between the container for electrolytic deposition (20) and the anion exchange device (30).

[0061] The dispersion for electrolytic deposition is stored in the electrolytic deposition container (20), and the support serving as the anode and the counter electrode serving as the cathode are immersed in the dispersion for electrolytic deposition. Then a voltage is applied between the support and the counter electrode to form the electrolytic deposition film on the surface of the support.

[0062] As in Fig. As shown in Figure 2, the anion exchange device 30 comprises an anion exchange container 31 in which an anion exchange resin 32 is arranged.

[0063] The dispersion for electrolytic deposition is fed from the electrolytic deposition container 20 through the extraction line 41 into the anion exchange container 31. During storage of the dispersion for electrolytic deposition in the anion exchange container 31, the organic acid contained in the dispersion is removed by the anion exchange resin 32.

[0064] This makes it possible to control the concentration of the organic acid contained in the dispersion for electrolytic deposition. Examples of organic acids contained in the dispersion for electrolytic deposition include carboxylic acids.

[0065] The dispersion for electrolytic deposition, in which the concentration of the organic acid in the anion exchange container 31 is controlled, is then directed via the return line 42 into the container for electrolytic deposition 20.

[0066] In the dispersion for electrolytic deposition, which is stored in the electrolytic deposition vessel 20, the concentration of the organic acid is preferably adjusted to a range of 5 mg / L or more and 500 mg / L or less.

[0067] In the method for handling a dispersion for electrolytic deposition according to the present embodiment with the configuration described above, since the concentration of the organic acid contained in the dispersion for electrolytic deposition is controlled, even in a case where the electrolytic deposition is carried out continuously, the concentration of the organic acid is not excessively increased, and it is possible to suppress the occurrence of bubble formation during baking, and it is possible to form the insulating film stably.

[0068] In the present embodiment, in the case where the dispersion for electrolytic deposition contains the water, the organic solvent, the solid component and the neutralizing agent, and the solid component includes at least the polyimide resin, the electrolytic deposition film containing at least the polyimide resin can be formed, and the insulating film with excellent insulating properties can be formed stably.

[0069] In the present embodiment, if the dispersion for electrolytic deposition contains at least the carboxylic acid as an organic acid, a rapid drop in pH on the surface of the anode (the support) can be suppressed by the pH buffering effect of the organic acid, and the electrolytic deposition film can be formed stably.

[0070] In the present embodiment, in a case where the dispersion for electrolytic deposition contains at least the hydroxy acid as an organic acid, a rapid drop in pH on the surface of the anode (the support) can be suppressed by the pH buffering effect of the organic acid, and the electrolytic deposition film can be formed stably.

[0071] In the present embodiment, if the concentration of the organic acid contained in the dispersion for electrolytic deposition is adjusted to be in the range of 5 mg / L or more and 500 mg / L or less, it is possible to exert a suitable pH buffering effect, to form the electrolytic deposition film stably, and to selectively prevent the occurrence of bubble formation during curing.

[0072] In the present embodiment, if the dispersion for electrolytic deposition contains the fluorinated resin together with the polyimide resin as a solid component, the electrolytic deposition film containing the mixed resin from the polyimide resin and the fluorinated resin can be formed, and the insulating film with particularly excellent insulating properties can be formed stably.

[0073] Since the electrolytic deposition apparatus 10, according to the present embodiment, comprises the electrolytic deposition container in which the electrolytic deposition dispersion is stored and into which the support and the counter electrode are immersed, the anion exchange device for subjecting the electrolytic deposition dispersion to anion exchange treatment, and the electrolytic deposition circulation device for circulating the electrolytic deposition dispersion between the electrolytic deposition container and the anion exchange device, the concentration of the organic acid contained in the electrolytic deposition dispersion can be adjusted appropriately, and even in a case where the electrolytic deposition is carried out continuously,The concentration of organic acid is not excessively increased, the occurrence of blistering during curing can be suppressed, and the insulating film can be formed stably.

[0074] The embodiment of the present invention has been described above, but the present invention is not limited to such an embodiment and can be modified in a suitable manner without departing from the technical features of the present invention.

[0075] In the present embodiment, the device for electrolytic deposition, which is in Fig. Figure 2 is shown as an example, but the present invention is not limited to such an electrolytic deposition device, and an electrolytic deposition device with a different configuration may be used.

[0076] For example, a device for electrolytic deposition 110, as in Fig. 3 shown, are used. In the Fig. The electrolytic deposition device 110 shown in Figure 3 can include the anion exchange device 130, with which the dispersion is subjected to the anion exchange treatment for electrolytic deposition, an ultrafiltration device 131, and an exchange layer vessel 132 in which an anion exchange layer 133 and a cation exchange layer 134 are arranged alternately. As a further method for controlling the organic acidity, a process using electrodialysis or similar methods can be employed. Examples

[0077] The following describes the results of confirmation tests carried out to confirm the effectiveness of the present invention.

[0078] As shown in Tables 1 and 2, the water, the organic solvent, the solid component, the neutralizing agent and the organic acid were prepared and mixed in the mass ratios given in Tables 1 and 2, thereby obtaining the dispersion for electrolytic deposition.

[0079] In Invention Examples 1 to 24, the dispersion for electrolytic deposition of the anion exchange treatment was described using the Fig. The device shown in Figure 2 was subjected to electrolytic deposition. The change in the concentration of the organic acid is shown in Tables 1 and 2.

[0080] The concentration of the organic acid contained in the electrolytic deposition film was determined in the following way.

[0081] The dispersion for electrolytic deposition was diluted with ultrapure water, and the filtrate obtained by removing impurities and passing through a membrane filter was used as a solution for ion chromatographic measurement.

[0082] The measurement was then performed using a Thermo Fisher Scientific ICS-5000+ ion chromatograph. The stationary phases of the ion chromatograph were the anion exchange columns Dionex IonPac AG15 and Dionex IonPac AS15, the eluent was an aqueous potassium hydroxide solution, the suppressor was a Dionex ADRS 600, and the detector was an electrical conductivity detector.

[0083] Furthermore, the stability of the dispersions for electrolytic deposition of Invention Examples 1 to 24, in which the anion exchange treatment was carried out, and the stability of the dispersions for electrolytic deposition of Comparative Examples 1 to 3, in which the anion exchange treatment was not carried out, were evaluated.

[0084] If the dispersion for electrolytic deposition was kept at 40°C for 5 days, the case in which precipitation or separation occurred in the dispersion for electrolytic deposition was rated as "B", and the case in which no precipitation or separation occurred in the dispersion for electrolytic deposition was rated as "A". The evaluation results are shown in Tables 1 and 2.

[0085] Then a flat square rod (1.47 mm × 2.94 mm × 25 cm length) made of oxygen-free copper was produced as a support with conductive properties and a cylindrical copper sheet as a counter electrode.

[0086] The support and counter electrode were immersed in the dispersion described above for electrolytic deposition, and the liquid temperature of the dispersion for electrolytic deposition was set to 20°C, the applied voltage to 300 V, and the holding time to 0.5 minutes; and thereby the electrolytic deposition film was formed.

[0087] The electrolytic deposition film was then baked in a three-stage temperature increase profile at a workpiece temperature of 140°C to 170°C for 10 minutes, at a workpiece temperature of 240°C to 260°C for 5 minutes, and at a workpiece temperature of 340°C to 350°C for 90 seconds, and then rapidly cooled; and this formed the insulating film.

[0088] Then the appearance of the formed insulating film was examined, and the blistering was assessed.

[0089] The case in which bubble formation in the insulation film was observed by visual observation was assessed as "present", and the case in which bubble formation was not observed was assessed as "not present".

[0090] Furthermore, the relative permittivity of the insulating film was measured as follows. The evaluation results are listed in Tables 1 and 2. Silver paste was applied to two 10 mm wide sections at the ends and to a 100 mm wide central section on the surface of the insulating film; this prepared a test specimen. The capacitance between the conductor and the silver paste in the central area was measured using a HIOKI EE CORPORATION IM3536 LCR meter, and the relative permittivity was calculated from the measured capacitance and the film thickness. [Table 1] Organic solvent Solid component Organic acid Anion exchange Stability of the dispersion for electrolytic deposition Evaluation Art Art Art Concentration of organic acid before exchange (mg / L) Concentration of organic acid after exchange (mg / L) Blistering Relative dielectric constant Example of the invention 1 N,N-Dimethylacetamide PAI Methanesulfonic acid 25 4 A Unavailable 4,0 2 N,N-Dimethylformamide PEI Methanesulfonic acid 25 3 A Unavailable 3,6 3 Propylene carbonate PI Trimellitic acid 30 3 A Unavailable 3,4 4 Dimethyl sulfoxide PAI Phthalic acid 15 2 A Unavailable 4,0 5 N,N-Dimethylformamide PAI Butyric acid 20 3 A Unavailable 4,0 6 Propylene carbonate PAI Benzoic acid 1000 300 A Unavailable 4,0 7 γ-Butyrolactone PAI Formic acid 1500 150 A Unavailable 4,0 8 N,N-Dimethylacetamide PAI Malonic acid 1200 200 A Unavailable 4,0 9 Propylene carbonate PI Benzoic acid 1500 400 A Unavailable 3,4 10 N-Methyl-2-pyrrolidone PI Formic acid + Trimellitic acid 50 5 A Unavailable 3,4 11 N,N-Dimethylformamide PI Trimellitic acid 100 50 A Unavailable 3,4 12 N,N-Dimethylformamide PAI Formic acid + Acetic acid 500 150 A Unavailable 4,0 13 N-Methyl-2-pyrrolidone PAI Formic acid + Phthalic acid + Butyric acid 1000 500 A Unavailable 4,0 14 N,N-Dimethylacetamide PAI Formic acid + Valeric acid 600 200 A Unavailable 4,0 Polyimide resin: Polyamideimide (PAI), Polyimide (PI), and Polyetherimide (PEI) Fluoropolymer resin: Polytetrafluoroethylene (PTFE) and polytetrafluoroethylene perfluoroalkyl vinyl ether (PFA) [Table 2] Organic solvent Solid component Organic acid Anion exchange Stability of the dispersion for electrolytic deposition Evaluation Art Art Art Concentration of organic acid before exchange (mg / L) Concentration of organic acid after exchange (mg / L) Blistering Relative dielectric constant 15 Dimethyl sulfoxide PAI Formic acid + Benzoic acid 800 330 A Unavailable 4,0 16 N-Methyl-2-pyrrolidone PAI Formic acid + Malonic acid 50 25 A Unavailable 4,0 17 Dimethyl sulfoxide PAI Formic acid + Acetic acid + Butyric acid 100 10 A Unavailable 4,0 18 N-Methyl-2-pyrrolidone PAI+PFA Formic acid 80 40 A Unavailable 2,6 19 N-Methyl-2-pyrrolidone PAI+PTFE Formic acid 100 60 A Unavailable 2,7 20 N-Methyl-2-pyrrolidone PAI Glycolic acid 800 15 A Unavailable 4,0 21 N-Methyl-2-pyrrolidone PAI Hydroxypropionic acid 600 30 A Unavailable 4,0 22 N-Methyl-2-pyrrolidone PAI Hydroxybutyric acid 700 10 A Unavailable 4,0 23 N-Methyl-2-pyrrolidone PAI Tartronic acid 650 200 A Unavailable 4,0 24 N-Methyl-2-pyrrolidone PAI Glyceric acid 1200 250 A Unavailable 4,0 Comparative example 1 N,N-Dimethylacetamide PAI Methanesulfonic acid 600 - B Available 3,4 2 γ-Butyrolactone PAI Formic acid 1500 - B Available 4,0 3 Propylene carbonate PI Benzoic acid 1500 - B Available 2,7 Polyimide resin: Polyamideimide (PAI), Polyimide (PI), and Polyetherimide (PEI) Fluoropolymer resin: Polytetrafluoroethylene (PTFE) and polytetrafluoroethylene perfluoroalkyl vinyl ether (PFA)

[0091] In comparative examples 1 to 3, the stability of the dispersion for electrolytic deposition was rated "B" because the concentration of the organic acid contained in the dispersion was not adjusted. Furthermore, blistering occurred in the insulating film after curing.

[0092] On the other hand, in Invention Examples 1 to 24, the stability of the dispersion for electrolytic deposition was rated "A" because the concentration of the organic acid contained in the dispersion was adjusted. Furthermore, no blistering occurred in the insulating film after curing.

[0093] Furthermore, the solid component in Invention Examples 18 and 19 contained the polyimide resin and the fluorinated resin, and the relative dielectric constant was sufficiently low, and the insulation properties were particularly good.

[0094] From the results of the confirmation experiments described above, it was found that, according to the inventive examples, it was possible to provide a method for handling a dispersion for electrolytic deposition and a device for electrolytic deposition with which the occurrence of bubble formation could be suppressed in the case in which the electrolytic deposition film was baked on, and the insulating film could be formed stably. INDUSTRIAL APPLICABILITY

[0095] It is possible to provide a method for handling a dispersion for electrolytic deposition and the device for electrolytic deposition, with which the occurrence of bubble formation can be suppressed in the case in which the electrolytic deposition film is baked on, and the insulating film can be formed stably. QUOTES INCLUDED IN THE DESCRIPTION

[0000] This list of documents cited by the applicant was automatically generated and is included solely for the reader's convenience. The list is not part of the German patent or utility model application. The DPMA accepts no liability for any errors or omissions. Cited patent literature

[0000] JP 2023-070848

[0002] JP 2024-017168

[0002] JP 2017-115120

[0007] JP 2018-070663

[0007]

Claims

[1] A method for handling a dispersion for electrolytic deposition, which is used in the case where an electrolytic deposition film is formed on a support with conductive properties by anionic electrolytic deposition, the method comprising: Adjusting the concentration of an organic acid contained in the dispersion for electrolytic deposition by subjecting the dispersion for electrolytic deposition to an anion exchange treatment. [2] The method for handling a dispersion for electrolytic deposition according to claim 1, wherein the dispersion for electrolytic deposition comprises water, an organic solvent, a solid component and a neutralizing agent, and the solid component includes at least one polyimide resin. [3] The method for handling a dispersion for electrolytic deposition according to claim 1, wherein the dispersion for electrolytic deposition contains at least one carboxylic acid as an organic acid. [4] The method for handling a dispersion for electrolytic deposition according to claim 1, wherein the dispersion for electrolytic deposition contains at least one hydroxy acid as an organic acid. [5] The method for handling a dispersion for electrolytic deposition according to claim 1, wherein the concentration of the organic acid contained in the dispersion for electrolytic deposition is adjusted to be in the range of 5 mg / L or more and 500 mg / L or less. [6] The method for handling a dispersion for electrolytic deposition according to claim 1, wherein the dispersion for electrolytic deposition comprises a fluorinated resin together with a polyimide resin as the solid component. [7] An electrolytic deposition device used in a case where an electrolytic deposition film is formed on a support having conductive properties by anionic electrolytic deposition, the electrolytic deposition device comprising: a container for electrolytic deposition in which a dispersion for electrolytic deposition is stored and into which a support and a counter electrode are immersed; an anion exchange device to subject the dispersion to anion exchange treatment for electrolytic deposition; and a circulation device for circulating the dispersion for electrolytic deposition between the container for electrolytic deposition and the anion exchange device.

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