CN113488305A - Adhesive, integrally-formed inductor and preparation method - Google Patents
Adhesive, integrally-formed inductor and preparation method Download PDFInfo
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- CN113488305A CN113488305A CN202110638492.7A CN202110638492A CN113488305A CN 113488305 A CN113488305 A CN 113488305A CN 202110638492 A CN202110638492 A CN 202110638492A CN 113488305 A CN113488305 A CN 113488305A
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 77
- 239000006247 magnetic powder Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000004804 winding Methods 0.000 claims abstract description 30
- 239000012745 toughening agent Substances 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims description 35
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- 239000002131 composite material Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000003822 epoxy resin Substances 0.000 claims description 14
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- 229920001971 elastomer Polymers 0.000 claims description 11
- 230000009969 flowable effect Effects 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 11
- 229920001021 polysulfide Polymers 0.000 claims description 11
- 239000005077 polysulfide Substances 0.000 claims description 11
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- 238000003756 stirring Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- ORTUYCUWCKNIND-UHFFFAOYSA-N 3-[2-(2-aminoethylamino)ethylamino]propanenitrile Chemical compound NCCNCCNCCC#N ORTUYCUWCKNIND-UHFFFAOYSA-N 0.000 claims description 9
- 229920000459 Nitrile rubber Polymers 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 8
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- 239000004643 cyanate ester Substances 0.000 claims description 7
- 239000004944 Liquid Silicone Rubber Substances 0.000 claims description 6
- 239000004642 Polyimide Substances 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 6
- 229920002492 poly(sulfone) Polymers 0.000 claims description 6
- 229920000768 polyamine Polymers 0.000 claims description 6
- 229920000570 polyether Polymers 0.000 claims description 6
- 229920001721 polyimide Polymers 0.000 claims description 6
- 229920002379 silicone rubber Polymers 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 150000008065 acid anhydrides Chemical class 0.000 claims description 4
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- 238000005336 cracking Methods 0.000 abstract description 12
- 238000011084 recovery Methods 0.000 abstract description 6
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- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- AHZMUXQJTGRNHT-UHFFFAOYSA-N [4-[2-(4-cyanatophenyl)propan-2-yl]phenyl] cyanate Chemical compound C=1C=C(OC#N)C=CC=1C(C)(C)C1=CC=C(OC#N)C=C1 AHZMUXQJTGRNHT-UHFFFAOYSA-N 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
- H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F17/00—Fixed inductances of the signal type
- H01F17/04—Fixed inductances of the signal type with magnetic core
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F17/00—Fixed inductances of the signal type
- H01F17/04—Fixed inductances of the signal type with magnetic core
- H01F2017/048—Fixed inductances of the signal type with magnetic core with encapsulating core, e.g. made of resin and magnetic powder
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to an adhesive, an integrally formed inductor and a preparation method. The raw materials for preparing the adhesive mainly comprise resin, a high-temperature curing agent, a medium-temperature curing agent and a toughening agent, under the auxiliary action of the medium-temperature curing agent, the adhesive can enable the integrally formed inductor to generate a crosslinking curing reaction at a medium-temperature stage when the temperature range is 60-100 ℃ in the baking process to realize partial curing, and contributes to the bonding strength of soft magnetic powder, so that the elastic recovery of a coil winding in a compression state in the integrally formed inductor is effectively inhibited, the adhesive is applied to the preparation process of the integrally formed inductor, the cracking phenomenon of the integrally formed inductor in the baking process after room-temperature pressing can be effectively improved, and meanwhile, the adhesive adopts the high-temperature curing agent as a main curing agent to generate a second curing reaction at a high-temperature stage, so that the integrally formed inductor also has good high-temperature resistance.
Description
Technical Field
The invention relates to the field of bonding materials, in particular to an adhesive, an integrally formed inductor and a preparation method.
Background
The inductor is an element capable of converting electric energy into magnetic energy to be stored, and mainly plays roles in filtering, oscillating, delaying, trapping, screening signals, filtering noise, stabilizing current, inhibiting electromagnetic wave interference and the like in a circuit, and equipment cannot be easily damaged due to current problems only when an electronic product is used after the inductor is installed in the circuit. With the continuous development of the inductor industry, the manufacturing technology of inductor products is continuously upgraded and updated, and the integrally formed inductor is a relatively novel inductor product, and because the integrally formed inductor has the advantages of miniaturization, strong anti-electromagnetic interference performance, low noise, high frequency and the like, the integrally formed inductor is more and more widely applied to electronic products.
The integrally formed inductor comprises a base body and a coil winding, wherein the coil winding can be embedded into soft magnetic powder in a powder metallurgy mode, and then the adhesive is solidified and prepared in a baking mode. In the preparation process of the integrally formed inductor, the soft magnetic powder and the adhesive are two raw materials which are important, wherein the soft magnetic powder has electromagnetic characteristics, eddy current loss and hysteresis loss are required to be small when the soft magnetic powder is used for alternating current occasions, the adhesive can achieve the purpose of reducing the loss by blocking eddy current transmission among the powder, and the adhesive can provide binding force for the combination of the soft magnetic powder after being solidified.
In the powder metallurgy pressing process, a coil winding is in a compressed state due to pressure and is embedded into soft magnetic powder, the coil is heated and can recover deformation in the subsequent baking and curing process, an integrally formed inductor is required to have good heat resistance, so high-temperature curing is usually adopted, the curing temperature of a general adhesive is 120-250 ℃, the adhesive is not cured before reaching the high-temperature curing temperature, sufficient bonding strength cannot be provided for the coil winding and the soft magnetic powder, the coil winding cannot be prevented from recovering deformation in the baking and curing process, and the phenomenon that a product is cracked in the baking process of the integrally formed inductor is easily caused, so the curing performance of the adhesive has direct influence on the appearance of the integrally formed inductor after being baked.
Because the conventional adhesive in the current market cannot provide enough adhesive strength for the coil winding and the soft magnetic powder at the medium-low temperature stage, the coil winding cannot be prevented from being deformed, the cracking problem of the integrally formed inductor in the baking process is serious, and the large-scale production and application of the integrally formed inductor are greatly limited. In order to improve the cracking phenomenon generated in the baking process, although the number of copper coils of the coil winding can be reduced to reduce the coil recovery deformation force of the winding in the baking process, or a hot pressing process is adopted to improve the cracking condition, the product performance is reduced or the cost is increased.
Disclosure of Invention
Accordingly, there is a need for an adhesive and a method for preparing the same that can effectively improve the cracking phenomenon of an integrally formed inductor, and does not cause product performance degradation and increase production cost.
In addition, it is necessary to provide an integrally molded inductor prepared by using the adhesive and a preparation method thereof.
The invention provides an adhesive which comprises the following raw material components in parts by mass:
the curing temperature of the high-temperature curing agent is 120-250 ℃, and the curing temperature of the medium-temperature curing agent is 60-100 ℃.
In one embodiment, the curing temperature of the high-temperature curing agent is between 150 ℃ and 240 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 85 ℃.
In one embodiment, the resin is a mixture of one or more of epoxy, phenolic, and silicone.
In one embodiment, the high temperature curing agent is a mixture of one or more of aromatic polyamine, anhydride, dicyandiamide, cyanate ester, and hydrazide.
In one embodiment, the medium-temperature curing agent is one or more of N-cyanoethyldiethylenetriamine, isophoronediamine and ethylenediamine.
In one embodiment, the toughening agent is a mixture of one or more of carboxyl liquid nitrile rubber, polysulfide rubber, liquid silicone rubber, polyether, polysulfone, polyimide, nano calcium carbonate and nano titanium dioxide.
The invention also provides a preparation method of the adhesive, which comprises the following steps:
preparing the following raw material components in parts by mass:
wherein the curing temperature of the high-temperature curing agent is between 120 and 250 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 100 ℃;
and mixing the raw materials, and uniformly stirring to prepare the adhesive.
In one embodiment, the resin is a mixture of one or more of epoxy resin, phenolic resin and silicone resin; and/or
The high-temperature curing agent is one or a mixture of more of aromatic polyamine, acid anhydride, dicyandiamide, cyanate ester and hydrazide; and/or
The medium-temperature curing agent is one or a mixture of N-cyanoethyl diethylenetriamine, isophorone diamine and ethylene diamine; and/or
The toughening agent is one or a mixture of more of carboxyl liquid nitrile rubber, polysulfide rubber, liquid silicone rubber, polyether, polysulfone, polyimide, nano calcium carbonate and nano titanium dioxide.
The invention also provides a preparation method of the integrally formed inductor, which comprises the following steps:
dissolving the adhesive with a solvent;
uniformly mixing the dissolved adhesive with the soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor.
In one embodiment, the binder is 2% to 5% by mass of the soft magnetic powder.
In one embodiment, the solvent is acetone, and the mass of the solvent is 5% to 20% of the mass of the soft magnetic powder.
In one embodiment, the baking is a staged type baking.
In one embodiment, the specific operations of the staged baking are as follows: heating the mixture from room temperature to 60 ℃, and keeping the mixture for 1 to 2 hours; heating from 60 ℃ to 80 ℃, and keeping for 1-2 hours; raising the temperature from 80 ℃ to 100 ℃, and keeping for 1-2 hours; heating from 100 ℃ to 120 ℃, and keeping for 1-2 hours; heating the mixture from 120 ℃ to the curing temperature required by the high-temperature curing agent, and keeping the mixture for 1 to 2 hours.
The invention also provides an integrally formed inductor which comprises the adhesive, the soft magnetic powder and the coil winding, wherein the coil winding is embedded in the soft magnetic composite material formed by mixing the adhesive and the soft magnetic powder.
In one embodiment, the integrally formed inductor is prepared by the above method for preparing the integrally formed inductor.
In the preparation formula of the adhesive, besides resin, high-temperature curing agent and toughening agent, medium-temperature curing agent is added, under the auxiliary action of the medium-temperature curing agent, the adhesive can ensure that the integrally formed inductor generates crosslinking curing reaction at the medium-temperature stage when the temperature range is 60-100 ℃ in the baking process to realize partial curing, contributes adhesive strength to soft magnetic powder, thereby effectively inhibiting the coil winding in a compressed state in the integrated inductor from generating elastic recovery, applying the adhesive in the preparation process of the integrated inductor, can effectively improve the cracking phenomenon of the integrally formed inductor in the baking process after being pressed at room temperature, meanwhile, the adhesive adopts a high-temperature curing agent as a main curing agent and can generate a secondary curing reaction at a high-temperature stage, so that the integrally formed inductor also has good high-temperature resistance. The integrally formed inductor prepared by the invention does not reduce the number of coils of the coil winding, so that the electromagnetic property of the inductor is not reduced, a hot pressing process is not needed, and the generation cost can be effectively reduced.
Drawings
FIG. 1 is a DSC test chart of example 2 and comparative example 2.
Detailed Description
In order to facilitate understanding of the present invention, the adhesive, the integrally formed inductor and the manufacturing method of the present invention will be described more fully with reference to the following specific embodiments. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The adhesive comprises the following raw material components in parts by mass:
the curing temperature of the high-temperature curing agent is 120-250 ℃, and the curing temperature of the medium-temperature curing agent is 60-100 ℃. The adhesive is added with the medium-temperature curing agent as an auxiliary agent, and can perform a first cross-linking curing reaction at a medium-temperature stage of 60-100 ℃ to realize partial curing, so that the adhesive can provide certain bonding strength for the soft magnetic powder at the medium-temperature stage, thereby effectively inhibiting the coil winding in a compressed state in the integrally formed inductor from elastic recovery, and meanwhile, the high-temperature curing agent is still the main curing agent of the adhesive, so that the adhesive can perform a second curing at a high-temperature stage of 120-250 ℃, thereby enabling the integrally formed inductor to have good high-temperature resistance.
In one embodiment, the curing temperature of the high-temperature curing agent is between 150 ℃ and 240 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 85 ℃. The adhesive prepared within the curing temperature range has better anti-cracking effect when being applied to preparing integrally formed electric appliances.
In one embodiment, the resin is a mixture of one or more of epoxy, phenolic, and silicone. The above resins are all thermosetting resins and have good heat resistance.
In one embodiment, the high temperature curing agent is a mixture of one or more of aromatic polyamine, anhydride, dicyandiamide, cyanate ester, and hydrazide. The high-temperature curing agent has low activity, and can be used for crosslinking and curing the resin only by needing high temperature. Specifically, the curing temperature is between 120 ℃ and 250 ℃. Further, the curing temperature is between 150 ℃ and 240 ℃.
In one embodiment, the medium-temperature curing agent is one or more of N-cyanoethyldiethylenetriamine, isophoronediamine and ethylenediamine. The medium-temperature curing agent has high activity due to containing active hydrogen atoms, and can crosslink and cure resin at a lower temperature. Specifically, the curing temperature is between 60 ℃ and 100 ℃. Further, the curing temperature is between 60 ℃ and 85 ℃.
In one embodiment, the toughening agent is a mixture of one or more of carboxyl liquid nitrile rubber, polysulfide rubber, liquid silicone rubber, polyether, polysulfone, polyimide, nano calcium carbonate and nano titanium dioxide. Wherein the grain size of the nano calcium carbonate is between 10nm and 100nm, and the grain size of the nano titanium dioxide is between 10nm and 100 nm.
A preparation method of the adhesive comprises the following steps:
preparing the following raw material components in parts by mass:
wherein the curing temperature of the high-temperature curing agent is between 120 and 250 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 100 ℃;
and mixing the raw materials, and uniformly stirring to prepare the adhesive.
In one embodiment, the resin is a mixture of one or more of epoxy resin, phenolic resin and silicone resin; and/or
The high-temperature curing agent is one or a mixture of more of aromatic polyamine, acid anhydride, dicyandiamide, cyanate ester and hydrazide; and/or
The medium-temperature curing agent is one or a mixture of N-cyanoethyl diethylenetriamine, isophorone diamine and ethylene diamine; and/or
The toughening agent is one or a mixture of more of carboxyl liquid nitrile rubber, polysulfide rubber, liquid silicone rubber, polyether, polysulfone, polyimide, nano calcium carbonate and nano titanium dioxide. Wherein the grain size of the nano calcium carbonate is between 10nm and 100nm, and the grain size of the nano titanium dioxide is between 10nm and 100 nm.
A preparation method of an integrally formed inductor comprises the following steps:
dissolving the adhesive with a solvent;
uniformly mixing the dissolved adhesive with the soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor.
In one embodiment, the binder is 2% to 5% by mass of the soft magnetic powder.
In one embodiment, the solvent is acetone, and the mass of the solvent is 5% to 20% of the mass of the soft magnetic powder.
In one embodiment, the baking is a staged type baking. Specifically, the temperature is raised from room temperature to 60 ℃, and the temperature is kept for 1 to 2 hours; heating from 60 ℃ to 80 ℃, and keeping for 1-2 hours; raising the temperature from 80 ℃ to 100 ℃, and keeping for 1-2 hours; heating from 100 ℃ to 120 ℃, and keeping for 1-2 hours; heating the mixture from 120 ℃ to the curing temperature required by the high-temperature curing agent, and keeping the mixture for 1 to 2 hours.
An integrally formed inductor comprising the adhesive of any of the above embodiments, soft magnetic powder, and a coil winding embedded in a soft magnetic composite material formed by mixing the adhesive and the soft magnetic powder.
In one embodiment, the integrally formed inductor is prepared by the above method for preparing the integrally formed inductor. The integrated inductor can be applied to the 0650-330 machines, but is not limited thereto.
The adhesive, the integrally molded inductor and the production method of the present invention will be described in detail with reference to the following specific examples, in which all the raw materials are commercially available unless otherwise specified.
Among them, epoxy resin E44 and epoxy resin E51 were purchased from south asian resin factories, bisphenol a type cyanate ester was purchased from shanghai international trade limited, carboxyl-terminated liquid nitrile rubber was purchased from shanghai international trade limited, and liquid epoxy-terminated polysulfide rubber was purchased from Nanjing novelties chemical limited.
Example 1:
(1) preparing an adhesive: weighing, mixing and uniformly stirring 100 parts of epoxy resin E44100, 56 parts of high-temperature curing agent bisphenol A cyanate ester, 10 parts of intermediate-temperature curing agent isophorone diamine and 5 parts of toughening agent carboxyl-terminated liquid nitrile rubber according to parts by mass. Wherein the high-temperature curing temperature is 240 ℃, and the medium-temperature curing temperature is 80 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Example 2:
(1) preparing an adhesive: weighing 44100 parts of epoxy resin E, 15 parts of high-temperature curing agent m-phenylenediamine, 10 parts of medium-temperature curing agent N-cyanoethyl diethylenetriamine and 10 parts of toughening agent liquid-state epoxy-terminated polysulfide rubber according to parts by mass, mixing and stirring uniformly. Wherein the high-temperature curing temperature is 150 ℃, and the medium-temperature curing temperature is 80 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Example 3:
(1) preparing an adhesive: weighing 44100 parts of epoxy resin E, 15 parts of high-temperature curing agent m-phenylenediamine, 15 parts of medium-temperature curing agent N-cyanoethyl diethylenetriamine and 10 parts of toughening agent liquid-state epoxy-terminated polysulfide rubber according to parts by mass, mixing and stirring uniformly. Wherein the high-temperature curing temperature is 150 ℃, and the medium-temperature curing temperature is 80 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Example 4:
(1) preparing an adhesive: weighing 44100 parts of epoxy resin E, 15 parts of high-temperature curing agent m-phenylenediamine, 25 parts of medium-temperature curing agent N-cyanoethyl diethylenetriamine and 10 parts of toughening agent liquid-state epoxy-terminated polysulfide rubber according to parts by mass, mixing and stirring uniformly. Wherein the high-temperature curing temperature is 150 ℃, and the medium-temperature curing temperature is 80 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Example 5:
(1) preparing an adhesive: weighing 100 parts of epoxy resin E51100 parts, 80 parts of high-temperature curing agent methyltetrahydrophthalic anhydride, 15 parts of medium-temperature curing agent ethylenediamine and 5 parts of titanium dioxide with the grain size of 50nm serving as a toughening agent according to the mass parts, mixing and uniformly stirring. Wherein the high-temperature curing temperature is 150 ℃, and the medium-temperature curing temperature is 85 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Comparative example 1:
(1) preparing an adhesive: weighing, mixing and uniformly stirring 100 parts of epoxy resin E44100 parts, 56 parts of high-temperature curing agent bisphenol A cyanate ester and 5 parts of toughening agent carboxyl-terminated liquid nitrile rubber according to parts by mass. Wherein the high-temperature curing temperature is 240 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Comparative example 2:
(1) preparing an adhesive: weighing 44100 parts of epoxy resin E, 15 parts of high-temperature curing agent m-phenylenediamine and 10 parts of toughening agent liquid-state epoxy-terminated polysulfide rubber according to parts by mass, mixing and stirring uniformly. Wherein the high-temperature curing temperature is 150 DEG C
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
Comparative example 3:
(1) preparing an adhesive: weighing and mixing 51100 parts of epoxy resin E, 80 parts of high-temperature curing agent methyltetrahydrophthalic anhydride and 5 parts of titanium dioxide with the grain diameter of 50nm serving as a toughening agent in parts by mass, and uniformly stirring. Wherein the high-temperature curing temperature is 150 ℃.
(2) Preparing an integrally formed inductor:
dissolving 3.5 parts by mass of the adhesive obtained in (1) with 15 parts by mass of acetone;
uniformly mixing the dissolved adhesive with 100 parts by mass of soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing, molding and baking to prepare the integrally molded inductor with the model number of 0650 and 330. The baking method comprises the following steps: heating from room temperature to 60 ℃, and keeping for 1 hour; heating from 60 deg.C to 80 deg.C, and holding for 1 hr; raising the temperature from 80 ℃ to 100 ℃ and keeping the temperature for 1 hour; heating from 100 deg.C to 120 deg.C, and holding for 1 hr; the temperature is raised from 120 ℃ to the curing temperature required by the high-temperature curing agent, and the curing temperature is kept for 1 hour.
As shown in fig. 1, as can be seen from the DSC test graphs of example 2 and comparative example 2, after the medium-temperature curing agent was added, the integrally formed inductor has 2 exothermic peaks at the middle temperature stage and the high temperature stage respectively, which shows that the integrally formed inductor undergoes twice curing in the baking process, the curing strength at the middle temperature stage is weaker, and the integrally formed inductor contributes certain bonding strength to the soft magnetic powder through partial curing, thereby effectively inhibiting the coil winding in a compressed state in the integrated inductor from elastic recovery to achieve the effect of crack resistance, ensuring that the integrally formed inductor prepared has good high temperature resistance, the integrally formed inductor without the medium-temperature curing agent only has 1 exothermic peak at the high-temperature stage, which indicates that the integrally formed inductor is cured only at the high-temperature stage, and cannot effectively inhibit the coil winding from elastic recovery and realize the anti-cracking effect.
The cracking condition of the integrally formed inductors with the model number of 0650-330 prepared in the examples 1-5 and the comparative examples 1-3 is tested, and the test and calculation method comprises the following steps: each of 132 integrally molded inductor products prepared by the above examples and comparative examples was optionally observed by microscopic observation, and whether the integrally molded inductor cracked was judged from 1/2, whether the crack length of each face of the integrally molded inductor product exceeded the face length, and if the crack length of either face of the integrally molded inductor exceeded 1/2 of the face length, the product was judged to be cracked, otherwise the product was judged not to be cracked. The crack ratios of the integrally formed inductor products obtained according to the test and calculation methods are shown in table 1 below, for example:
TABLE 1 integrally molded inductor cracking ratios obtained in examples and comparative examples
As can be seen from table 1, after the medium-temperature curing agent is added to the adhesive formula, the adhesive is applied to the preparation process of the integrally formed inductor, compared with the process without the medium-temperature curing agent, the crack rate of the integrally formed inductor prepared by using the medium-temperature curing agent as the auxiliary curing agent is obviously reduced, and the cracking condition is obviously improved, which indicates that the addition of the medium-temperature curing agent to the adhesive has a good effect of being conductive to cracking resistance of the integrally formed inductor. From the test results of examples 2 to 4, it can be seen that the higher the addition amount of the medium-temperature curing agent, the more remarkable the crack resistance effect of the integrally molded inductor.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims, and the description and the drawings can be used for explaining the contents of the claims.
Claims (15)
1. The adhesive is characterized by comprising the following raw material components in parts by mass:
wherein the curing temperature of the high-temperature curing agent is between 120 and 250 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 100 ℃.
2. The adhesive according to claim 1, wherein the curing temperature of the high-temperature curing agent is between 150 ℃ and 240 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 85 ℃.
3. An adhesive according to any one of claims 1 to 2, wherein the resin is a mixture of one or more of epoxy resin, phenolic resin and silicone resin.
4. The adhesive according to any one of claims 1 to 2, wherein the high-temperature curing agent is a mixture of one or more of aromatic polyamine, acid anhydride, dicyandiamide, cyanate ester, and hydrazide.
5. The adhesive according to any one of claims 1 to 2, wherein the medium temperature curing agent is one or a mixture of N-cyanoethyldiethylenetriamine, isophoronediamine and ethylenediamine.
6. The adhesive according to any one of claims 1 to 2, wherein the toughening agent is a mixture of one or more of carboxyl liquid nitrile rubber, polysulfide rubber, liquid silicone rubber, polyether, polysulfone, polyimide, nano calcium carbonate and nano titanium dioxide.
7. The preparation method of the adhesive is characterized by comprising the following steps:
preparing the following raw material components in parts by mass:
wherein the curing temperature of the high-temperature curing agent is between 120 and 250 ℃; the curing temperature of the medium-temperature curing agent is between 60 and 100 ℃;
and mixing the raw materials, and uniformly stirring to prepare the adhesive.
8. The method for preparing the adhesive according to claim 7, wherein the resin is a mixture of one or more of epoxy resin, phenolic resin and silicone resin; and/or
The high-temperature curing agent is one or a mixture of more of aromatic polyamine, acid anhydride, dicyandiamide, cyanate ester and hydrazide; and/or
The medium-temperature curing agent is one or a mixture of N-cyanoethyl diethylenetriamine, isophorone diamine and ethylene diamine; and/or
The toughening agent is one or a mixture of more of carboxyl liquid nitrile rubber, polysulfide rubber, liquid silicone rubber, polyether, polysulfone, polyimide, nano calcium carbonate and nano titanium dioxide.
9. A preparation method of an integrally formed inductor is characterized by comprising the following steps:
dissolving the adhesive according to any one of claims 1 to 6 in a solvent;
uniformly mixing the dissolved adhesive with the soft magnetic powder to form a flowable soft magnetic composite material;
and embedding the coil winding into the soft magnetic composite material, pressing and molding, and baking to prepare the integrally molded inductor.
10. The method of manufacturing an integrally formed inductor according to claim 9, wherein the mass of the binder is 2% to 5% of the mass of the soft magnetic powder.
11. The method for manufacturing an integrally formed inductor according to claim 9, wherein the solvent is acetone, and the mass of the solvent is 5% to 20% of the mass of the soft magnetic powder.
12. The method for manufacturing an integrally formed inductor according to any one of claims 9 to 11, wherein the baking is a step-type baking.
13. The method for manufacturing an integrally formed inductor according to claim 12, wherein the step-type baking comprises the following specific operations: heating the mixture from room temperature to 60 ℃, and keeping the mixture for 1 to 2 hours; heating from 60 ℃ to 80 ℃, and keeping for 1-2 hours; raising the temperature from 80 ℃ to 100 ℃, and keeping for 1-2 hours; heating from 100 ℃ to 120 ℃, and keeping for 1-2 hours; heating the mixture from 120 ℃ to the curing temperature required by the high-temperature curing agent, and keeping the mixture for 1 to 2 hours.
14. An integrally molded inductor comprising the binder according to any one of claims 1 to 6, soft magnetic powder, and a coil winding embedded in a soft magnetic composite material formed by mixing the binder and the soft magnetic powder.
15. The integrally formed inductor according to claim 14, which is produced by the method for producing an integrally formed inductor according to any one of claims 9 to 13.
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