Preparation method for improving peel strength of planar capacitor material and planar capacitor material
By controlling the particle size of the inorganic filler in the graphic capacitor material and the use of step -type mature treatment, the problem of low existing material peeling strength is solved, and higher peeling strength and capacitor density are achieved.
Patent Information
- Application Number
- CN202411504070.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-25
- Publication Date
- 2025-01-28
AI Technical Summary
The peel strength of existing planar capacitance materials is low, which leads to easy delamination between the dielectric material and the copper foil electrode during application and secondary processing, affecting product quality.
By providing dielectric materials, including epoxy resin, inorganic fillers, auxiliary, and solvents, the particle size of the inorganic filler is less than 0.1um, and the cooked processing method of step -by -step heating up is used to improve the peeling strength of the graphic capacitor material.
It significantly improves the peeling intensity of graphic capacitor materials, ensures the stability and reliability of the material in the application and processing process, while maintaining a high capacitance density.
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Figure CN119381176A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of capacitor technology, and in particular to a preparation method for improving the peeling strength of a planar capacitor material and a planar capacitor material. Background Art
[0002] Existing planar capacitor materials are made of polymer dielectric materials and copper foil with the aid of micro-nano technology. The peel strength of existing planar capacitor materials is as low as 0.5N / mm. During the application of planar capacitor materials or secondary processing and manufacturing, delamination and detachment occur between the dielectric material and the copper foil electrode, and even abnormalities such as blistering occur after reliability testing, which greatly affects product quality. Summary of the invention
[0003] In view of this, the present invention provides a preparation method for improving the peeling strength of a planar capacitor material, thereby improving the peeling strength of the planar capacitor material.
[0004] A preparation method for improving the peel strength of a planar capacitor material, the preparation method comprising:
[0005] A dielectric material is provided, which includes epoxy resin, inorganic filler, additives and solvent; wherein the volume of the inorganic filler of the polymer dielectric material accounts for 40% to 80%, the volume of the epoxy resin accounts for 10% to 60%, and the volume of the additive accounts for 5% to 30%.
[0006] Adding epoxy resin into a solvent, stirring and mixing to obtain a mixed solution;
[0007] The inorganic filler is stirred and dispersed in another solvent to obtain a suspension, wherein the particle size of the inorganic filler is less than 0.1 μm;
[0008] Dispersing the suspension in the mixed solution, then adding an additive and stirring to mix evenly to obtain a medium slurry mixture;
[0009] The dielectric slurry mixture is poured into a ball mill for grinding to obtain a liquid slurry of the dielectric material; before the liquid slurry of the dielectric material is coated on the first and second electrodes, it needs to be defoamed, including but not limited to defoaming by physical methods such as a mechanical defoamer, a centrifugal force defoaming device, and ultrasonic defoaming, so as to eliminate the effects of uneven slurry coating and reduced contact area between the slurry coating and the electrode layer caused by bubbles.
[0010] Providing a first electrode layer and a second electrode layer, placing a dielectric material liquid slurry on the surface of the first electrode layer and / or the second electrode layer, and then preheating the first electrode layer and the second electrode layer, wherein the preheating temperature is 80° C. to 130° C. and the preheating time is 30 seconds to 300 seconds; obtaining a planar capacitor material in which the solvent has volatilized but the dielectric material has not solidified;
[0011] The planar capacitor material is subjected to a curing treatment, and the curing temperature is controlled to increase step by step. Each time the temperature is increased, it is kept at the temperature for a preset time and then the temperature is increased again.
[0012] Optionally, the aging process includes preheating and heat preservation control, multiple temperature rise control and multiple heat preservation control;
[0013] During the preheating and heat preservation control, the planar capacitor material is controlled to mature at a first maturing temperature for a first preset time;
[0014] After the preheating and heat preservation control is performed on the planar capacitor material, the first temperature rise control is started to control the first aging temperature to rise to a second aging temperature, and the temperature rise process takes a second preset time;
[0015] After the second preset time has passed, the first heat preservation control is started to control the planar capacitor material to mature at the second maturing temperature for a third preset time;
[0016] After the third preset time has passed, the second temperature rise control and the subsequent second temperature keeping control are started, and the temperature rise control and the temperature keeping control are alternately performed in this way until the aging process is completed.
[0017] Optionally, the aging treatment includes temperature reduction control, and the temperature reduction control is started after the last time the heat preservation control is performed, so that the aging temperature of the planar capacitor material is reduced to the design temperature.
[0018] Optionally, the first aging temperature is 60°C, the first temperature rising control raises the aging temperature from 60°C to 80°C, the second temperature rising control raises the aging temperature from 80°C to 120°C, the third temperature rising control raises the aging temperature from 120°C to 170°C, and after the last heat preservation control is performed, the temperature reduction control is started to reduce the aging temperature from 170°C to 100°C.
[0019] Optionally, the first aging temperature is 60°C, the first temperature rising control raises the aging temperature from 60°C to 80°C, the second temperature rising control raises the aging temperature from 80°C to 120°C, the third temperature rising control raises the aging temperature from 120°C to 170°C, and the fourth temperature rising control raises the aging temperature from 170°C to 210°C. After the last heat preservation control, the temperature reduction control is started to reduce the aging temperature from 210°C to 100°C.
[0020] Optionally, before stirring and dispersing the inorganic filler in the solvent, the method further comprises:
[0021] After adding a set amount of the auxiliary agent to the inorganic filler, pour it into a grinding jar for grinding and refining. The rotation speed of the grinding jar is controlled to be 50 rpm to 150 rpm and the grinding time is 24 h to 240 h, so that the particle size of the inorganic filler is less than 0.1 um.
[0022] Optionally, the grinding jar contains a plurality of first grinding balls, a plurality of second grinding balls, a plurality of third grinding balls, a plurality of fourth grinding balls and a plurality of fifth grinding balls, the diameter of the first grinding balls is smaller than the diameter of the second grinding balls, the diameter of the second grinding balls is smaller than the diameter of the third grinding balls, the diameter of the third grinding balls is smaller than the diameter of the fourth grinding balls, and the diameter of the fourth grinding balls is smaller than the diameter of the fifth grinding balls.
[0023] Optionally, the diameter of the first grinding ball is 0.5 mm; the diameter of the second grinding ball is 1.0 mm; the diameter of the third grinding ball is 3.0 mm; the diameter of the fourth grinding ball is 5.0 mm; and the diameter of the fifth grinding ball is 8.0 mm.
[0024] Optionally, the number of the first grinding balls accounts for 10% to 50% of the total number of grinding balls; the number of the second grinding balls accounts for 20% to 60% of the total number of grinding balls; the number of the third grinding balls accounts for 10% to 50% of the total number of grinding balls; the number of the fourth grinding balls accounts for 20% to 60% of the total number of grinding balls; and the number of the fifth grinding balls accounts for 5% to 30% of the total number of grinding balls.
[0025] Optionally, the length of the planar capacitor material is greater than or equal to 2000 mm, and the width is 300 mm to 1300 mm.
[0026] Optionally, the peel strength of the planar capacitor material is greater than or equal to 0.7 N / mm.
[0027] Optionally, the capacitance density of the planar capacitor material is 0.1 to 9.3 nF / cm 2 .
[0028] Optionally, the particle size of the inorganic filler is greater than or equal to 0.025 um.
[0029] Optionally, the surface roughness of the first electrode layer and / or the second electrode layer is 0.3-0.4 um.
[0030] Optionally, the epoxy resin is added into the solvent, and stirred at a temperature of 20° C. to 40° C. for 5 min to 35 min to obtain a mixed solution.
[0031] Optionally, the medium slurry mixture is poured into a ball mill and ground at 50 rpm to 150 rpm for 168 h to 240 h.
[0032] Optionally, the temperature for laminating the first electrode layer and the second electrode layer is 100° C. to 130° C., and the laminating pressure is 1 to 5 kg / cm 2 .
[0033] Optionally, after the first electrode layer and the second electrode layer are laminated for the first time, a second lamination is performed, wherein the temperature is 130° C. to 200° C. and the lamination pressure is 5 to 10 kg / cm 2 ; Obtain the flexible planar capacitor material.
[0034] Optionally, the epoxy resin is at least one of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, alicyclic epoxy resin, epoxidized olefin compound, sugarcane polyol epoxy resin and mixed structure epoxy resin.
[0035] Optionally, the inorganic filler is at least one of sodium barium titanate, barium titanate, calcium copper titanate, strontium titanate, barium strontium titanate, calcium titanate, calcium barium titanate, lead zirconate titanate, sodium lead titanate, and lead titanate.
[0036] Optionally, the auxiliary agent is at least one of a curing agent, a dispersant, a coupling agent, a leveling agent, a defoaming agent, and a accelerator.
[0037] Optionally, the solvent is at least one of acetone, pentanone, alcohol, butanone and ketone.
[0038] The present invention also relates to a planar capacitor material, which is produced by the above-mentioned preparation method for improving the peeling strength of the planar capacitor material.
[0039] The particle size of the inorganic filler used in the preparation method for improving the peel strength of the planar capacitor material of the present invention is less than 0.1um, and the inorganic filler powder can be more fully dispersed in the solvent, which is more conducive to the dielectric material liquid slurry infiltration into the surface of the first electrode layer and / or the second electrode layer, achieving a good wetting effect, and microscopically making the contact area between the molecules of the dielectric material liquid slurry and the molecules of the first electrode layer and / or the second electrode layer larger, and macroscopically manifested as the adhesion between the dielectric material liquid slurry and the first electrode layer and the second electrode layer increased; at the same time, the preparation method adopts a step-by-step temperature increase method to ripen the planar capacitor material, so that the function of the polymer molecules of the medium and the metal molecules of the electrode is increased, and the momentum is also increased, thereby promoting the increase of the intermolecular interaction force, so that the step-by-step change of the ripening temperature can directly affect the improvement of the peel strength of the planar capacitor material; the present application combines the above two methods to greatly improve the peel strength of the planar capacitor material, and can also ensure that the planar capacitor material has a higher capacitance density. In addition, the use of this preparation method can continuously produce and prepare planar capacitor materials. BRIEF DESCRIPTION OF THE DRAWINGS
[0040] Figure 1 It is a schematic diagram of the temperature control coordinate structure of the aging treatment according to one embodiment of the present invention.
[0041] Figure 2 It is a schematic diagram of the cross-sectional structure of the planar capacitor material of this method. DETAILED DESCRIPTION
[0042] The following is a description of the implementation of the present invention by means of specific embodiments. Those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification.
[0043] In the following description, reference is made to the accompanying drawings, which describe several embodiments of the present invention. It should be understood that other embodiments may be used and that mechanical, structural, electrical, and operational changes may be made without departing from the spirit and scope of the present invention. The following detailed description should not be considered limiting, and the terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.
[0044] Although the terms first, second, etc. are used herein to describe various elements in some instances, these elements should not be limited by these terms. These terms are only used to distinguish one element from another element.
[0045] Furthermore, as used in this article, the singular forms "one", "an" and "the" are intended to include plural forms as well, unless there is an indication to the contrary in the context. It should be further understood that the terms "comprise", "include" indicate the presence of features, steps, operations, elements, components, projects, kinds, and / or groups, but do not exclude the presence, occurrence or addition of one or more other features, steps, operations, elements, components, projects, kinds, and / or groups. The terms "or" and "and / or" used herein are interpreted as inclusive, or mean any one or any combination. Therefore, "A, B or C" or "A, B and / or C" means "any of the following: A; B; C; A and B; A and C; B and C; A, B and C". Only when the combination of elements, functions, steps or operations is inherently mutually exclusive in some way, will there be an exception to this definition.
[0046] The present invention relates to a preparation method for improving the peel strength of a planar capacitor material, the preparation method comprising:
[0047] A dielectric material is provided, the dielectric material includes epoxy resin, inorganic filler, additive and solvent; wherein the volume of the inorganic filler of the polymer dielectric material accounts for 40% to 80%, for example, 50%, 60%, 70%; the volume of the epoxy resin accounts for 10% to 60%, for example, 20%, 30%, 40%, 50%; the volume of the additive accounts for 5% to 30%, for example, 10%, 15%, 20%, 25%. The dielectric constant of the polymer dielectric material is 8 to 40 (@1kHz, 1V), and the dielectric loss is less than or equal to 0.05.
[0048] Adding epoxy resin into a solvent, stirring and mixing to obtain a mixed solution;
[0049] The inorganic filler is stirred and dispersed in another solvent to obtain a suspension, wherein the particle size of the inorganic filler is less than 0.1 μm;
[0050] Dispersing the suspension in the mixed liquid, then adding an additive and stirring and mixing evenly to obtain a medium slurry mixture;
[0051] The dielectric slurry mixture is poured into a ball mill for grinding to obtain a liquid slurry of dielectric material; before the liquid slurry of dielectric material is coated on the first and second electrodes, it needs to be defoamed, including but not limited to defoaming by physical methods such as mechanical defoamers, centrifugal defoaming devices, and ultrasonic defoaming, so as to eliminate and reduce the effects of uneven slurry coating and reduced contact area between the slurry coating and the electrode layer caused by bubbles. After the liquid slurry of dielectric material is defoamed, the peel strength of the planar capacitor material can be relatively increased by 0.1N / mm or more, compared with the planar capacitor material made of slurry without defoaming treatment.
[0052] A first electrode layer and a second electrode layer are provided, and a liquid slurry of a dielectric material is disposed on the surface of the first electrode layer and / or the second electrode layer, and then the first electrode layer and the second electrode layer are preheated, wherein the preheating temperature is 80°C to 130°C and the preheating time is 30 seconds to 300 seconds; a planar capacitor material in which the solvent has evaporated but the dielectric material has not been solidified is obtained, and the slurry is still in a state of being slightly flowable, and sufficient time is required for it to automatically and fully infiltrate the surface of the first electrode layer and / or the second electrode layer. The dielectric layer thickness of the planar capacitor material in which the solvent has evaporated but the dielectric material has not been completely solidified is 3 to 40 um.
[0053] The planar capacitor material is subjected to a curing treatment, and the curing temperature is controlled to increase step by step. Each time the temperature is increased, it is kept at the temperature for a preset time and then the temperature is increased again.
[0054] The particle size of the inorganic filler used in the preparation method for improving the peel strength of the planar capacitor material of the present invention is less than 0.1um, and the inorganic filler powder can be more fully dispersed in the solvent, which is more conducive to the dielectric material liquid slurry infiltration into the surface of the first electrode layer and / or the second electrode layer, achieving a good wetting effect, and microscopically making the contact area between the molecules of the dielectric material liquid slurry and the molecules of the first electrode layer and / or the second electrode layer larger, and macroscopically manifested as the adhesion between the dielectric material liquid slurry and the first electrode layer and the second electrode layer increased; at the same time, the preparation method adopts a step-by-step temperature increase method to ripen the planar capacitor material, so that the function of the polymer molecules of the medium and the metal molecules of the electrode is increased, and the momentum is also increased, thereby promoting the increase of the intermolecular interaction force, so that the step-by-step change of the ripening temperature can directly affect the improvement of the peel strength of the planar capacitor material; the present application combines the above two methods to greatly improve the peel strength of the planar capacitor material, and can also ensure that the planar capacitor material has a higher capacitance density. In addition, the use of this preparation method can continuously produce and prepare planar capacitor materials.
[0055] Optionally, the aging process includes preheating and heat preservation control, multiple temperature rise control and multiple heat preservation control;
[0056] During preheating and heat preservation control, the planar capacitor material is controlled to mature at a first maturing temperature for a first preset time;
[0057] After the planar capacitor material is preheated and kept warm, the first temperature rise control is started to control the first aging temperature to rise to the second aging temperature, and the temperature rise process takes a second preset time;
[0058] After the second preset time, the first heat preservation control is started to control the planar capacitor material to mature at the second maturation temperature for a third preset time;
[0059] After the third preset time has passed, the second temperature rise control and the subsequent second temperature keeping control are started, and the temperature rise control and the temperature keeping control are alternately performed in this way until the aging process is completed.
[0060] Optionally, the aging treatment includes temperature reduction control, and the temperature reduction control is started after the last heat preservation control is performed to reduce the aging temperature of the planar capacitor material to the design temperature.
[0061] Optionally, Figure 1 FIG. 1 is a schematic diagram of a temperature control coordinate structure of a aging treatment according to an embodiment of the present invention. Figure 1As shown, the first aging temperature is 60°C, the first temperature rise control makes the aging temperature rise from 60°C to 80°C, the second temperature rise control makes the aging temperature rise from 80°C to 120°C, the third temperature rise control makes the aging temperature rise from 120°C to 170°C, and the temperature reduction control starts after the last temperature preservation control, so that the aging temperature drops from 170°C to 100°C. In this embodiment, the first preset time is 3h (hours); the first temperature rise time is 1h, and the first temperature preservation time is 6h; the second temperature rise time is 4h, and the second temperature preservation time is 15min (minutes); the third temperature rise time is 15min, and the third temperature preservation time is 15min; the temperature reduction time is 2h.
[0062] It is worth mentioning that the minimum peel strength of the flexible planar capacitor material produced using the above-mentioned aging treatment parameters is about 0.7N / mm (refer to IPC-TM-650 2.4.9 standard, using a tensile tester to test its 90° peel strength). The aging treatment parameters are not limited to the above and can be freely adjusted according to actual needs, but must meet the above-mentioned step-by-step temperature control and heat preservation control.
[0063] Optionally, see Figure 1 , the first aging temperature is 60°C, the first temperature rise control makes the aging temperature rise from 60°C to 80°C, the second temperature rise control makes the aging temperature rise from 80°C to 120°C, the third temperature rise control makes the aging temperature rise from 120°C to 170°C, the fourth temperature rise control makes the aging temperature rise from 170°C to 210°C, and the temperature reduction control starts after the last insulation control, so that the aging temperature drops from 210°C to 100°C. In this embodiment, the first preset time is 3h (hours); the first temperature rise time is 1h, and the first insulation time is 6h; the second temperature rise time is 4h, and the second insulation time is 15min (minutes); the third temperature rise time is 15min, and the third insulation time is 15min; the fourth temperature rise time is 30min, and the fourth insulation time is 1.5h; the temperature reduction time is 3h.
[0064] It is worth mentioning that the minimum peel strength of the flexible planar capacitor material produced using the above-mentioned aging treatment parameters is about 1.0N / mm (refer to IPC-TM-650 2.4.9 standard, using a tensile tester to test its 90° peel strength). The aging treatment parameters are not limited to the above and can be freely adjusted according to actual needs, but must meet the above-mentioned step-by-step temperature control and insulation control.
[0065] Optionally, before the inorganic filler is stirred and dispersed in the solvent, the method further comprises:
[0066] After adding a set amount of additives to the inorganic filler, pour it into the grinding jar for grinding and refining. Control the rotation speed of the grinding jar to 50rpm-150rpm and the grinding time to 24h-240h, so that the particle size of the inorganic filler is less than 0.1um.
[0067] Optionally, the grinding jar contains a plurality of first grinding balls, a plurality of second grinding balls, a plurality of third grinding balls, a plurality of fourth grinding balls and a plurality of fifth grinding balls, the diameter of the first grinding balls is smaller than the diameter of the second grinding balls, the diameter of the second grinding balls is smaller than the diameter of the third grinding balls, the diameter of the third grinding balls is smaller than the diameter of the fourth grinding balls, and the diameter of the fourth grinding balls is smaller than the diameter of the fifth grinding balls.
[0068] Optionally, the diameter of the first grinding ball is 0.5 mm; the diameter of the second grinding ball is 1.0 mm; the diameter of the third grinding ball is 3.0 mm; the diameter of the fourth grinding ball is 5.0 mm; and the diameter of the fifth grinding ball is 8.0 mm.
[0069] Optionally, the number of the first grinding balls accounts for 10% to 50% of the number of all grinding balls; the number of the second grinding balls accounts for 20% to 60% of the number of all grinding balls; the number of the third grinding balls accounts for 10% to 50% of the number of all grinding balls; the number of the fourth grinding balls accounts for 20% to 60% of the number of all grinding balls; and the number of the fifth grinding balls accounts for 5% to 30% of the number of all grinding balls.
[0070] Optionally, the length of the planar capacitor material is greater than or equal to 2000 mm, and the width is 300 mm to 1300 mm, for example, 400 mm, 500 mm, 600 mm, 800 mm, 900 mm, or 1200 mm.
[0071] Optionally, the peel strength of the planar capacitor material is greater than or equal to 0.7 N / mm.
[0072] Optionally, the capacitance density of the planar capacitor material is 0.1 to 9.3 nF / cm 2 , for example 0.2nF / cm 2 、0.6nF / cm 2 , 1nF / cm 2 , 2nF / cm 2 、3nF / cm 2 , 4nF / cm 2 , 5nF / cm 2 、6nF / cm 2 、7nF / cm 2 、8nF / cm 2 .
[0073] Optionally, the particle size of the inorganic filler is greater than or equal to 0.025 um.
[0074] Optionally, the surface roughness of the first electrode layer and / or the second electrode layer is 0.3-0.4 um.
[0075] Optionally, the epoxy resin is added to a solvent and stirred at a temperature of 20° C. to 40° C. for 5 min to 35 min to obtain a mixed solution.
[0076] Alternatively, the medium slurry mixture is poured into a ball mill and ground at 50 rpm to 150 rpm for 168 h to 240 h.
[0077] Optionally, the temperature for laminating the first electrode layer and the second electrode layer is 100° C. to 130° C., and the laminating pressure is 1 to 5 kg / cm 2 .
[0078] Optionally, after the first electrode layer and the second electrode layer are laminated for the first time, a second lamination is performed, and the temperature is controlled to be 130°C to 200°C and the lamination pressure is 5 to 10 kg / cm 2 ; Obtain flexible planar capacitor material.
[0079] Optionally, the epoxy resin is at least one of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, alicyclic epoxy resin, epoxidized olefin compound, sugarcane polyol epoxy resin and mixed structure epoxy resin.
[0080] Optionally, the inorganic filler is at least one of sodium barium titanate, barium titanate, calcium copper titanate, strontium titanate, barium strontium titanate, calcium titanate, calcium barium titanate, lead zirconate titanate, sodium lead titanate, and lead titanate.
[0081] Optionally, the auxiliary agent is at least one of a curing agent, a dispersant, a coupling agent, a leveling agent, a defoaming agent, and a accelerator.
[0082] Optionally, the solvent is at least one of acetone, pentanone, alcohol, butanone and ketone.
[0083] Figure 2 This is a schematic diagram of the cross-sectional structure of the planar capacitor material of this method, such as Figure 2 As shown, the present invention also relates to a planar capacitor material, which is obtained by the above-mentioned preparation method for improving the peeling strength of the planar capacitor material. In this embodiment, the planar capacitor material includes a first electrode layer 11, a second electrode layer 12, and a dielectric layer 15 arranged between the first electrode layer 11 and the second electrode layer 12.
[0084] The capacitance theoretical characteristic formula of the planar capacitor material of the present application is:
[0085]
[0086] Wherein, C is the capacitance value of the planar capacitor material, A is the area of the first electrode layer 11 and the second electrode layer 12 of the planar capacitor material, and D is k is the dielectric constant of the dielectric layer 15, K is a constant, and t is the distance between the first electrode layer 11 and the second electrode layer 12 of the planar capacitor material. From this calculation formula, it can be seen that the capacitance value C of the planar capacitor material is proportional to the facing area A of the planar capacitor material, inversely proportional to the distance t between the first electrode layer 11 and the second electrode layer 12, and proportional to the dielectric constant of the dielectric layer 15. At the same time, it is also obtained that the capacitance value per unit area (that is, the capacitance density C of the planar capacitor material) d ), the dielectric constant of the dielectric layer 15 is proportional to the distance t between the first electrode layer 11 and the second electrode layer 12, as shown in the following formula:
[0087]
[0088] The present invention can produce enough polymer dielectric material slurry (10kg-4000kg / 24h) by controlling the particle size of the inorganic filler to be less than 0.1um and using a step-by-step heating method to mature the planar capacitor material, thereby ensuring that the planar capacitor material coil can be continuously produced.
[0089] Example 1
[0090] For example, 4,4'-diaminodicyclohexylmethane glycidylamine epoxy resin hydrogenated AG-80, barium titanate, curing agent, dispersant, coupling agent and butanone solvent are used to prepare dielectric material slurry, wherein the particle size of inorganic material barium titanate is ball-milled to 50nm, and the mixed material is ground in the grinding tank for about 48h; the dielectric material slurry is made into a planar capacitor material semi-finished product on a copper foil electrode, and the semi-finished product is first subjected to 110℃ and 4kg / cm 2 The pressure was then pressed at 140°C and 6kg / cm 2 The pressed semi-finished product is pressed again with pressure, and then ripened at the following temperatures: 60℃ / 3h, (60℃-80℃) / 1h, 80℃ / 6h, (80℃-120℃) / 30min, 120℃ / 4h, (120℃-170℃) / 15min, 170℃ / 60min, (170℃-50℃) / 6h.
[0091] The peel strength of the finished planar capacitor material is tested to be 0.75N / mm and the capacitance density is 1.0nF / cm 2 (@1Khz), the loss is 0.016(@1Khz).
[0092] Example 2
[0093] For example, 4,4'-diaminodicyclohexylmethane glycidylamine epoxy resin hydrogenated AG-80, barium titanate, curing agent, dispersant, coupling agent and butanone solvent are used to prepare dielectric material slurry, wherein the particle size of inorganic material barium titanate is ball-milled to 50nm, and the mixed material is ground in the grinding tank for about 48h; the dielectric material slurry is made into a planar capacitor material semi-finished product on a copper foil electrode, and the semi-finished product is first subjected to 110℃ and 4kg / cm 2 The pressed semi-finished products are then aged at the following temperatures: 60°C / 3h, (60°C-80°C) / 1h, 80°C / 6h, (80°C-120°C) / 30min, 120°C / 4h, (120°C-170°C) / 15min, 170°C / 60min, (170°C-50°C) / 6h.
[0094] The peel strength of the finished flat capacitor material is 0.7N / mm and the capacitance density is 1.0nF / cm 2 (@1Khz), the loss is 0.017(@1Khz).
[0095] Example 3
[0096] For example, 4,4'-diaminodicyclohexylmethane glycidylamine epoxy resin hydrogenated AG-80, barium titanate, curing agent, dispersant, coupling agent and butanone solvent are used to prepare dielectric material slurry, wherein the particle size of inorganic material barium titanate is ball-milled to 50nm, and the mixed material is ground in the grinding tank for about 48h; the dielectric material slurry is made into a planar capacitor material semi-finished product on a copper foil electrode, and the semi-finished product is first subjected to 110℃ and 4kg / cm 2 The pressure was then pressed at 140°C and 6kg / cm 2 The pressed semi-finished product is pressed again with pressure, and then ripened at the following temperatures: 60℃ / 3h, (60℃-80℃) / 1h, 80℃ / 6h, (80℃-120℃) / 15min, 120℃ / 2h, (120℃-170℃) / 15min, 170℃ / 15min, (170℃-50℃) / 6h.
[0097] The peel strength of the finished flat capacitor material is 0.8N / mm and the capacitance density is 1.0nF / cm 2 (@1Khz), the loss is 0.019(@1Khz).
[0098] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by a person of ordinary skill in the art without departing from the spirit and technical concept disclosed by the present invention shall still be covered by the claims of the present invention.
Claims
1. A method for improving the peel strength of a planar capacitor material, characterized in that: The preparation method comprises: Providing a dielectric material, wherein the dielectric material comprises an epoxy resin, an inorganic filler, an additive and a solvent; Adding the epoxy resin into the solvent, stirring and mixing to obtain a mixed solution; Stirring and dispersing the inorganic filler in another solvent to obtain a suspension, wherein the particle size of the inorganic filler is less than 0.1 um; Dispersing the suspension in the mixed solution, then adding the additive and stirring to mix evenly to obtain a medium slurry mixture; Pour the dielectric slurry mixture into a ball mill for grinding to obtain a dielectric material liquid slurry; Providing a first electrode layer and a second electrode layer, placing the dielectric material liquid slurry on the surface of the first electrode layer and / or the second electrode layer, and then laminating and hot-pressing the first electrode layer and the second electrode layer to obtain a planar capacitor material in which the solvent has volatilized but the dielectric material has not solidified; The planar capacitor material is subjected to a curing treatment, and the curing temperature is controlled to increase step by step. Each time the temperature is increased, the temperature is kept at the temperature for a preset time and then the temperature is increased again.
2. The method for preparing a planar capacitor material for improving peel strength according to claim 1, characterized in that: The aging process includes preheating and heat preservation control, multiple temperature rise control and multiple heat preservation control; During the preheating and heat preservation control, the planar capacitor material is controlled to mature at a first maturing temperature for a first preset time; After the preheating and heat preservation control is performed on the planar capacitor material, the first temperature rise control is started to control the first aging temperature to rise to a second aging temperature, and the temperature rise process takes a second preset time; After the second preset time has passed, the first heat preservation control is started to control the planar capacitor material to mature at the second maturing temperature for a third preset time; After the third preset time has passed, the second temperature rise control and the subsequent second temperature keeping control are started, and the temperature rise control and the temperature keeping control are alternately performed in this way until the aging process is completed.
3. The method for preparing a planar capacitor material for improving peel strength according to claim 2, characterized in that: The aging process includes temperature reduction control, which is started after the last time the heat preservation control is performed, so that the aging temperature of the planar capacitor material is reduced to the design temperature.
4. The method for preparing a planar capacitor material for improving peel strength according to claim 3, characterized in that: Include any of the following: The first aging temperature is 60°C, the first temperature increase control causes the aging temperature to increase from 60°C to 80°C, the second temperature increase control causes the aging temperature to increase from 80°C to 120°C, the third temperature increase control causes the aging temperature to increase from 120°C to 170°C, and the temperature reduction control is started after the last temperature preservation control is performed, causing the aging temperature to decrease from 170°C to 100°C; The first aging temperature is 60°C, the first temperature rising control raises the aging temperature from 60°C to 80°C, the second temperature rising control raises the aging temperature from 80°C to 120°C, the third temperature rising control raises the aging temperature from 120°C to 170°C, the fourth temperature rising control raises the aging temperature from 170°C to 210°C, and the temperature dropping control is started after the last heat preservation control is performed, so that the aging temperature drops from 210°C to 100°C.
5. The method for improving the peel strength of a planar capacitor material according to any one of claims 1 to 4, characterized in that: Include any of the following: Before the inorganic filler is stirred and dispersed in the solvent, the method further comprises: Adding a set amount of the auxiliary agent to the inorganic filler and pouring it into a grinding jar for grinding and refining, controlling the rotation speed of the grinding jar to 50 rpm to 150 rpm and the grinding time to 24 h to 240 h, so that the particle size of the inorganic filler is less than 0.1 um; The grinding jar contains a plurality of first grinding balls, a plurality of second grinding balls, a plurality of third grinding balls, a plurality of fourth grinding balls and a plurality of fifth grinding balls, wherein the diameter of the first grinding balls is smaller than the diameter of the second grinding balls, the diameter of the second grinding balls is smaller than the diameter of the third grinding balls, the diameter of the third grinding balls is smaller than the diameter of the fourth grinding balls, and the diameter of the fourth grinding balls is smaller than the diameter of the fifth grinding balls; The diameter of the first grinding ball is 0.5 mm; the diameter of the second grinding ball is 1.0 mm; the diameter of the third grinding ball is 3.0 mm; the diameter of the fourth grinding ball is 5.0 mm; the diameter of the fifth grinding ball is 8.0 mm; The number of the first grinding balls accounts for 10% to 50% of the total number of grinding balls; the number of the second grinding balls accounts for 20% to 60% of the total number of grinding balls; the number of the third grinding balls accounts for 10% to 50% of the total number of grinding balls; the number of the fourth grinding balls accounts for 20% to 60% of the total number of grinding balls; the number of the fifth grinding balls accounts for 5% to 30% of the total number of grinding balls; The length of the planar capacitor material is greater than or equal to 2000 mm, and the width is 300 mm to 1300 mm; The peel strength of the planar capacitor material is greater than or equal to 0.7N / mm; The capacitance density of the planar capacitor material is 0.1 to 9.3 nF / cm 2 ; The particle size of the inorganic filler is greater than or equal to 0.025um; The surface roughness of the first electrode layer and / or the second electrode layer is 0.3-0.4 um.
6. The method for improving the peel strength of a planar capacitor material according to any one of claims 1 to 4, characterized in that: The epoxy resin is added into the solvent, and stirred at a temperature of 20° C. to 40° C. for 5 min to 35 min to obtain a mixed solution.
7. The method for improving the peel strength of a planar capacitor material according to any one of claims 1 to 4, characterized in that: The medium slurry mixture is poured into a ball mill and ground at 50 rpm to 150 rpm and a rotation speed of 168 h to 240 h.
8. The method for improving the peel strength of a planar capacitor material according to any one of claims 1 to 4, characterized in that: Include at least one of the following: The temperature for laminating the first electrode layer and the second electrode layer is 100° C. to 130° C., and the laminating pressure is 1 to 5 kg / cm 2 ; After the first electrode layer and the second electrode layer are laminated for the first time, a second lamination is performed, and the temperature is controlled to be 130°C to 200°C and the lamination pressure is 5 to 10 kg / cm 2 ; Obtain the flexible planar capacitor material.
9. The method for improving the peel strength of a planar capacitor material according to any one of claims 1 to 4, characterized in that: Include any of the following: The epoxy resin is at least one of a glycidyl ether epoxy resin, a glycidyl ester epoxy resin, a glycidyl amine epoxy resin, an alicyclic epoxy resin, an epoxidized olefin compound, a sugarcane polyol epoxy resin, and a mixed structure epoxy resin; The inorganic filler is at least one of sodium barium titanate, barium titanate, calcium copper titanate, strontium titanate, barium strontium titanate, calcium titanate, calcium barium titanate, lead zirconate titanate, sodium lead titanate, and lead titanate; The auxiliary agent is at least one of a curing agent, a dispersant, a coupling agent, a leveling agent, a defoaming agent, and a accelerator; The solvent is at least one of acetone, pentanone, alcohol, butanone and ketone.
10. A planar capacitor material, characterized in that: The planar capacitor material is obtained by the preparation method for improving the peeling strength of the planar capacitor material according to any one of claims 1 to 9.