CN112940654A - Packaging adhesive and preparation method and application thereof - Google Patents
Packaging adhesive and preparation method and application thereof Download PDFInfo
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- CN112940654A CN112940654A CN202110128507.5A CN202110128507A CN112940654A CN 112940654 A CN112940654 A CN 112940654A CN 202110128507 A CN202110128507 A CN 202110128507A CN 112940654 A CN112940654 A CN 112940654A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5026—Amines cycloaliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
- H05K3/284—Applying non-metallic protective coatings for encapsulating mounted components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to packaging glue and a preparation method and application thereof. The packaging adhesive comprises an agent A and an agent B, wherein the agent A comprises epoxy resin and a reactive diluent, and the agent B comprises an amine curing agent and a curing accelerator; wherein: the reactive diluent is at least one selected from the group consisting of cyclohexanediol ether, phenyl glycidyl ether, cyclohexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, cyclohexanediol diglycidyl ester, glycerol triglycidyl ether, trimethylolpropane triglycidyl ether and pentaerythritol tetraglycidyl ether. According to the packaging adhesive provided by the invention, the A agent is formed by selecting the proper type of reactive diluent and the epoxy resin, and the B agent is formed by matching the proper type of curing agent and the curing accelerator, so that the two-component packaging adhesive is obtained, and the substrate filled with the packaging adhesive can not be obviously warped after being cured. In addition, the potting adhesive has high hardness after being cured and good weather resistance.
Description
Technical Field
The invention relates to the technical field of epoxy resin packaging glue, in particular to packaging glue and a preparation method and application thereof.
Background
The packaging adhesive for the high-power light-emitting diode has high refractive index and high light transmittance, can increase the luminous flux of the LED, has low viscosity, is easy to bubble, is suitable for encapsulation and compression molding, and ensures that the LED has better durability and reliability. The LED packaging adhesive is mainly characterized by comprising the following components: the product is high-light-transmittance LED glue which is used for LED packaging and forming, and has the greatest characteristics of good water permeability, 500-hour high-temperature resistance and no discoloration, low viscosity after mixing, good fluidity, easy defoaming and long service life; the curing can be carried out at medium temperature or high temperature, and the curing speed is high; after curing, the paint has small yield, good moisture resistance, good luster and high hardness; the cured product has good mechanical strength, excellent electrical characteristics, humidity and heat resistance and atmospheric aging resistance.
The traditional packaging adhesive consists of a component A and a component B, wherein the component A comprises 60-80% of epoxy resin, 19-39% of low-viscosity modified epoxy resin, 0.1-0.5% of defoaming agent and 0.1-0.5% of flatting agent; the component B comprises 64 to 99 percent of amine curing agent, 0 to 20 percent of curing agent accelerator, 0 to 15 percent of modifier, 0.2 to 0.5 percent of antioxidant and 0.2 to 0.5 percent of ultraviolet absorbent; the preparation method of the component A comprises the following steps: adding the epoxy resin and the low-viscosity modified epoxy resin in the component A into a reaction kettle, stirring for 2-4 hours at 80-100 ℃, uniformly mixing the materials, cooling to 50 ℃, adding the defoaming agent and the flatting agent into the mixture of the epoxy resin and the diluent, continuously stirring for 30 minutes, then carrying out vacuum defoaming for 10-20 minutes, and subpackaging to obtain a finished product; the preparation method of the component B comprises the following steps: adding the amine curing agent, the curing agent accelerator, the modifier, the antioxidant and the ultraviolet absorbent required in the formula into a reaction kettle, stirring for 1 hour at the temperature of 50-60 ℃, uniformly mixing the materials, and subpackaging to obtain a finished product; (2) mixing in proportion: the component A and the component B are uniformly mixed according to the weight ratio of 100/(25-50); (3) vacuum defoaming: vacuum defoaming is carried out for 5-10 minutes at normal temperature; (4) and (3) curing: after being poured on a device by a machine, the material is cured for 2 to 24 hours at the temperature of between 20 and 60 ℃ to prepare the material. The epoxy resin in the component A comprises one or a mixture of more of flexible solid epoxy resin, liquid bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin and polyurethane modified epoxy resin, and the flexible solid epoxy resin is one of NPES-601, NPES-901 and NPES-903; the liquid bisphenol A epoxy resin is one of E-51 and E-44; the hydrogenated bisphenol A epoxy resin is an epoxy resin with an epoxy equivalent of 180-500; the preparation method of the polyurethane modified epoxy resin comprises the following steps: firstly, preparing an isocyanate-terminated prepolymer by using polyol and isocyanate as raw materials; secondly, reacting the isocyanate-terminated prepolymer with excessive secondary hydroxyl in the epoxy resin to obtain polyurethane modified epoxy resin; the low-viscosity modified epoxy resin in the component A is one of 1, 6-hexanediol diglycidyl ether, 1, 4-butanediol diglycidyl ether, polypropylene glycol diglycidyl ether and polyethylene glycol diglycidyl ether; the defoaming agent in the component A is one or a mixture of more of BYK-A530, BYK-141, BYK-065, BYK-066N, TEGO Airex 900, TEGO Airex 962, TEGO Airex 932, Dow Corning 100F and Dow Corning 163; the leveling agent in the component A is one of BYK-310, BYK-320, BYK-358N, TEGO Glide 450 and Perenol S43; the amine curing agent in the component B is one or a mixture of aliphatic amine curing agent, alicyclic amine curing agent and polyether amine curing agent; the curing agent accelerator in the component B is AEP; the modifier in the component B is one of nonyl phenol and DMP-30; the antioxidant in the component B is phosphite ester, and comprises the following components: bis (3, 5-di-tert-butylphenyl) pentaerythritol diphosphite (antioxidant 626), and one or a mixture of more of Ciba tris (2, 4-di-tert-butylphenyl) phosphite, CGA12, TP-10H, 317, 517, a polymeric phosphite antioxidant TP-20, and a polyfunctional phosphite antioxidant TP-80 containing a hindered phenol group and a macromolecular group; the ultraviolet absorbent in the component B is benzophenone or benzotriazole, and comprises: 2-hydroxy-4-methoxybenzophenone (UV-9), 2-hydroxy-4-octoxybenzophenone (UV-531), 2- (2 '-hydroxy-5' methylphenyl) benzotriazole (UV-P), 2- (2 'hydroxy-5' tert-octylphenyl) benzotriazole (UV-329), 2-phenylbenzimidazole-5-sulfonic acid (UV-T), 2- (2H-benzotriazol-2-yl) -4, 6-di-tert-amylphenol (UV-328), ethyl 2-cyano-3, 3-diphenylacrylate (UV-335), and N- (2-ethoxyphenyl) -N' - (4-ethylphenyl) ethanediamide (UV-1033).
However, the conventional encapsulation adhesive, as mentioned above, has a significant warpage after being cured after the substrate is poured.
Disclosure of Invention
Based on the above, the main purpose of the present invention is to provide a packaging adhesive, a preparation method and a use thereof. The sealant provided by the invention can not obviously warp after the pouring substrate is cured.
The specific technical scheme comprises the following steps:
the packaging adhesive comprises an agent A and an agent B, wherein the agent A comprises epoxy resin and a reactive diluent, and the agent B comprises an amine curing agent and a curing accelerator; wherein:
the reactive diluent is at least one selected from the group consisting of cyclohexanediol ether, phenyl glycidyl ether, cyclohexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, cyclohexanediol diglycidyl ester, glycerol triglycidyl ether, trimethylolpropane triglycidyl ether and pentaerythritol tetraglycidyl ether.
In one embodiment, the amine-based curing agent is at least one selected from the group consisting of diethylenetriamine, triethylenetetramine, polyetheramine, 4 ' -diaminodicyclohexylmethane, 3 ' -dimethyl-4, 4 ' -diaminodicyclohexylmethane, methylcyclohexanediamine, isofroxanediamine, and 1, 3-cyclohexyldimethylamine.
In one embodiment, the epoxy resin is selected from at least one of a bisphenol a type epoxy resin, a bisphenol F type epoxy resin, a bisphenol S type epoxy resin, and a hydrogenated bisphenol a epoxy resin.
In one embodiment, the curing accelerator is selected from at least one of salicylic acid, benzyldimethylamine, and aminoethylpiperazine.
In one embodiment, the agent A comprises 75-96 parts of epoxy resin and 4-25 parts of reactive diluent by mass per 100 parts of agent A, and the agent B comprises 60-98 parts of curing agent and 0.7-8 parts of curing accelerator by mass per 100 parts of agent B.
In one embodiment, the agent a further comprises other functional additives X, and the other functional additives X are selected from at least one of defoaming agents, dispersing agents, leveling agents and dyes.
In one embodiment, the defoaming agent is BYK-141, or/and the dispersing agent is BYK-9076, or/and the leveling agent is BYK-320, or/and the dye is a purple dye.
In one embodiment, the other functional additive X is added in an amount of 0.05 to 4 parts by mass per 100 parts by mass of the agent a.
In one embodiment, the agent B further comprises other functional additives Y, and the other functional additives Y are selected from at least one of an antioxidant, an ultraviolet absorber and a chain extender.
In one embodiment, the antioxidant is selected from at least one of pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, 8 tris (2, 4-di-tert-butylphenyl) phosphite and N, N' -1, 6-hexylene-bis- [3, 5-di-tert-butyl-4-hydroxy-hydrocinnamamide, or/and the ultraviolet absorbent is selected from at least one of hydroxyl triazine derivative and tetra-hydroxy-2, 2,6, 6-tetramethyl-1-piperidine ethanol bismethylsuccinic acid polymer, and/or the chain extender is selected from at least one of cyclohexanediol, hexanediol, benzyl alcohol and diethylene glycol ether alcohol.
In one embodiment, the other functional assistant Y is added in an amount of 0.26 to 14 parts by mass per 100 parts by mass of the agent B.
In one embodiment, the mass ratio of the agent A to the agent B is 100: (20-100).
The preparation method of the packaging adhesive comprises the steps of preparing the agent A and preparing the agent B;
the step of preparing the agent A comprises the following steps: mixing the components contained in the agent A;
the step of preparing the agent B comprises the following steps: mixing the components contained in the agent B.
A circuit board comprises a substrate and packaging adhesive, wherein the packaging adhesive is the packaging adhesive.
A method for preparing a circuit board, comprising the steps of:
and taking the substrate, pouring the packaging adhesive, and curing.
In one embodiment, the curing temperature is 110-120 ℃, and the curing time is 4-8 min.
Compared with the prior art, the invention has the following beneficial effects:
according to the packaging adhesive provided by the invention, the A agent is formed by selecting the proper type of reactive diluent and the epoxy resin, and the B agent is formed by matching the proper type of curing agent and the curing accelerator, so that the two-component packaging adhesive is obtained, and the substrate filled with the packaging adhesive can not be obviously warped after being cured. In addition, the potting adhesive has high hardness after being cured and good weather resistance.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth 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 packaging adhesive comprises an agent A and an agent B, wherein the agent A comprises epoxy resin and a reactive diluent, and the agent B comprises an amine curing agent and a curing accelerator; wherein:
the reactive diluent is at least one selected from the group consisting of cyclohexanediol ether, phenyl glycidyl ether, cyclohexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, cyclohexanediol diglycidyl ester, glycerol triglycidyl ether, trimethylolpropane triglycidyl ether and pentaerythritol tetraglycidyl ether.
According to the packaging adhesive provided by the embodiment of the invention, the agent A is formed by selecting the proper type of reactive diluent and the epoxy resin, and the agent B is formed by matching the proper type of curing agent and the curing accelerator, so that the two-component packaging adhesive is obtained, and the substrate filled with the packaging adhesive can not be obviously warped after being cured. In addition, the potting adhesive has high hardness after being cured and good weather resistance.
The performance of the packaging adhesive provided by the embodiment of the invention is specifically embodied as follows: curing at 110-120 deg.C within 4-8 min, wherein the cured substrate (such as COB plate) has no obvious warpage, Tg >75 deg.C, hardness > shore D75, thermal shock resistance-40 deg.C- +80 deg.C/100 cycle, high temperature steaming test (PCT), 0.2MPa, 121 deg.C, and 72H steaming without abnormity.
In one embodiment, the amine-based curing agent is at least one selected from the group consisting of diethylenetriamine, triethylenetetramine, polyetheramine, 4 ' -diaminodicyclohexylmethane, 3 ' -dimethyl-4, 4 ' -diaminodicyclohexylmethane, methylcyclohexanediamine, isofroxanediamine, and 1, 3-cyclohexyldimethylamine.
In one example, the epoxy resin is selected from at least one of a bisphenol a type epoxy resin, a bisphenol F type epoxy resin, a bisphenol S type epoxy resin, and a hydrogenated bisphenol a epoxy resin.
In one example, the curing accelerator is selected from at least one of salicylic acid, benzyldimethylamine, and aminoethylpiperazine.
In one example, the agent A comprises 75-96 parts of epoxy resin and 4-25 parts of reactive diluent by mass per 100 parts of agent A, and the agent B comprises 60-98 parts of curing agent and 0.7-8 parts of curing accelerator by mass per 100 parts of agent B.
In one example, the agent A further comprises other functional auxiliary agents X, and the other functional auxiliary agents X are selected from at least one of defoaming agents, dispersing agents, leveling agents and dyes.
In one example, the defoaming agent is BYK-141, or/and the dispersing agent is BYK-9076, or/and the leveling agent is BYK-320, or/and the dye is a purple dye. Violet dyes of embodiments of the present invention include, but are not limited to, the Violet powder CLARIANT PV Fast Violet RL Pigment Violet 23.
In one embodiment, the other functional additive X is added in an amount of 0.05 to 4 parts by mass per 100 parts by mass of the agent a.
In one example, the agent B further comprises other functional auxiliary agents Y, and the other functional auxiliary agents Y are selected from at least one of an antioxidant, an ultraviolet absorber and a chain extender.
In one example, the antioxidant is at least one selected from the group consisting of pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, 8 tris (2, 4-di-tert-butylphenyl) phosphite and N, N' -1, 6-hexylene-bis- [3, 5-di-tert-butyl-4-hydroxy hydrocinnamamide, or/and the ultraviolet absorbent is selected from at least one of hydroxyl triazine derivative and tetra-hydroxy-2, 2,6, 6-tetramethyl-1-piperidine ethanol bismethylsuccinic acid polymer, and/or the chain extender is selected from at least one of cyclohexanediol, hexanediol, benzyl alcohol and diethylene glycol ether alcohol.
In one example, the other functional additive Y is added in an amount of 0.26 to 14 parts by mass per 100 parts by mass of the agent B.
The viscosity of the agent A provided by the embodiment of the invention is 7000cps to 13000cps at 25 ℃, and the viscosity of the agent B is 50cps to 300cps at 25 ℃.
In one example, the mass ratio of the agent a to the agent B is 100: (20-100).
The preparation method of the packaging adhesive comprises the steps of preparing the agent A and preparing the agent B;
the step of preparing the agent A comprises the following steps: mixing the components contained in the agent A;
the step of preparing the agent B comprises the following steps: mixing the components contained in the agent B.
In one example, the step of preparing the agent a comprises: preheating epoxy resin to 70-100 ℃, adding an active diluent into the epoxy resin, and stirring uniformly at a high-speed dispersion stirrer speed of 400-1000 rmp for 60-120 min.
In one example, the step of preparing the agent B comprises: adding a curing accelerator into the amine curing agent, stirring and dissolving uniformly at the rotation speed of 200-400 rpm, stirring and dissolving at the rotation speed of 200-400 rpm, mixing, and filtering with a 320-mesh sieve.
A circuit board comprises a substrate and packaging adhesive, wherein the packaging adhesive is the packaging adhesive.
A method for preparing a circuit board, comprising the steps of:
and taking the substrate, pouring the packaging adhesive, and curing.
In one example, the curing temperature is 110-120 ℃, and the curing time is 4-8 min.
Example 1
The embodiment provides a packaging adhesive and a preparation method thereof. Wherein:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive comprises the following steps:
the preparation method comprises the following steps: preheating epoxy resin to 70 ℃, adding an active diluent and other functional additives into the epoxy resin, and stirring uniformly for 60min at a high-speed dispersion stirrer speed of 400rmp/min to obtain an agent A;
the preparation of the agent B comprises the following steps: adding a curing accelerator into an amine curing agent, rotating at the speed of 200rpm, adding an antioxidant, an ultraviolet absorbent and a chain extender, stirring and dissolving uniformly at the speed of 200rpm, and filtering the mixed product through a 320-mesh filter.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 50.
Example 2
The embodiment provides a packaging adhesive and a preparation method thereof. Wherein:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive comprises the following steps:
the preparation method comprises the following steps: preheating epoxy resin to 80 ℃, adding an active diluent and other functional additives into the epoxy resin, and stirring uniformly for 100min at the high-speed dispersion stirrer speed of 700rmp/min to obtain an agent A;
the preparation of the agent B comprises the following steps: adding a curing accelerator into an amine curing agent, rotating at 300rpm, adding an antioxidant, an ultraviolet absorbent and a chain extender, stirring and dissolving uniformly at 300rpm, and filtering the mixed product through a 320-mesh filter.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 45.
Example 3
The embodiment provides a packaging adhesive and a preparation method thereof. Wherein:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive comprises the following steps:
the preparation method comprises the following steps: preheating epoxy resin to 100 ℃, adding an active diluent and other functional auxiliaries into the epoxy resin, and stirring uniformly at the rotating speed of 1000rmp/min by using a high-speed dispersion stirrer for 120min to obtain an agent A;
the preparation of the agent B comprises the following steps: adding a curing accelerator into an amine curing agent, rotating at the speed of 400rpm, adding an antioxidant, an ultraviolet absorbent and a chain extender, stirring and dissolving uniformly at the speed of 400rpm, and filtering the mixed product through a 320-mesh filter.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 22.
Table 1, example 1 to example 3 encapsulant formulations
Example 4
The embodiment provides a packaging adhesive and a preparation method thereof. Wherein:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive comprises the following steps:
the preparation method comprises the following steps: preheating epoxy resin to 70 ℃, adding an active diluent and other functional additives into the epoxy resin, and stirring uniformly for 60min at a high-speed dispersion stirrer speed of 400rmp/min to obtain an agent A;
the preparation of the agent B comprises the following steps: adding a curing accelerator into an amine curing agent, rotating at the speed of 200rpm, adding an antioxidant, an ultraviolet absorbent and a chain extender, stirring and dissolving uniformly at the speed of 200rpm, and filtering the mixed product through a 320-mesh filter.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 42.
Example 5
The embodiment provides a packaging adhesive and a preparation method thereof. Wherein:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive comprises the following steps:
the preparation method comprises the following steps: preheating epoxy resin to 70 ℃, adding an active diluent and other functional additives into the epoxy resin, and stirring uniformly for 60min at a high-speed dispersion stirrer speed of 400rmp/min to obtain an agent A;
the preparation of the agent B comprises the following steps: adding a curing accelerator into an amine curing agent, rotating at the speed of 200rpm, adding an antioxidant, an ultraviolet absorbent and a chain extender, stirring and dissolving uniformly at the speed of 200rpm, and filtering the mixed product through a 320-mesh filter.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 40.
Table 2, example 4 to example 5 encapsulant formulations
Comparative example 1
The comparative example is a comparative example of example 1, the difference relative to example 1 mainly comprises the difference of the type of the reactive diluent, and specifically, propylene oxide butyl ether is adopted to replace phenyl glycidyl ether, and the encapsulation glue of the comparative example is specifically as follows:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive refers to example 1.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 50.
Comparative example 2
This comparative example is that of example 1, and the difference with respect to example 1 mainly includes the difference in the kind of the curing agent, specifically, the acid anhydride curing agent is used instead of the amine curing agent. The encapsulation adhesive of the comparative example is specifically as follows:
the packaging adhesive comprises an agent A and an agent B,
the agent A comprises:
the agent B comprises:
the preparation method of the packaging adhesive refers to example 1.
When the packaging adhesive is used, the agent A and the agent B are mixed according to the mass ratio of 100: 50.
Performance testing
The performance test method of the packaging adhesive with the formula comprises the following steps:
uniformly mixing the agent A and the agent B according to a proportion, and pouring 100mm multiplied by 170mm multiplied by 2mm FR4 PCB, wherein the thickness of a glue layer is 0.2 mm-0.4 mm, and the total glue amount is 4.2-4.8 g; curing at 110-125 ℃ for 5 min-10 min, curing at 80-100 ℃ for 1 h-2 h, baking and curing to obtain a 100mm x 170mm x 2mm FR4 PCB with a cured adhesive layer, and carrying out the following performance tests:
(1) and (3) testing the warping rate, wherein the testing method comprises the following steps: packaging a 0.4mm adhesive layer on a 100mm, 170mm and 2mm FR4 board, curing, and performing cold and heat shock to-40-105 to obtain a warpage rate of less than 0.3%; warping rate: the sheet material bends causing a gap H1 between the sheet material and the planar substrate as a percentage of the length H of the sheet material.
(2) Test PCT experiment, cooking at 121 deg.C under 0.2Mpa for 72H.
(3) Test Tg, test method: taking 2 g-4 g of mixed glue, curing at 80 ℃/2H, cooling, measuring Tg by DSC, and increasing the temperature rate to 20 ℃/min.
(4) The test method comprises the following steps: minus 40 ℃ to plus 80 ℃.
(5) Hardness, test method: according to relevant reasonable curing conditions, 5g of cylindrical curing block is subjected to hardness measurement by a Shore hardness meter
The test results are given in the following table:
TABLE 3
| Tg/℃ | hardness/D | PCT | Number of cycles of thermal and cold shock resistance | Warping rate | |
| Example 1 | 75～86 | 77～82 | No abnormality of colloid | >100 | <0.15％ |
| Example 2 | 77～88 | 77～85 | No abnormality of colloid | >100 | <0.19％ |
| Example 3 | 77～88 | 76～82 | No abnormality of colloid | >100 | <0.17％ |
| Example 4 | 75～83 | 75～83 | No abnormality of colloid | >100 | <0.16％ |
| Example 5 | 70～85 | 70～80 | No abnormality of colloid | <100 | <0.17％ |
| Comparative example 1 | 65～75 | 68～78 | No abnormality of colloid | <100 | >0.62％ |
| Comparative example 2 | 70～82 | 68～75 | Melting of colloids | <100 | >0.58％ |
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 present patent shall be subject to the appended claims.
Claims (16)
1. The packaging adhesive is characterized by comprising an agent A and an agent B, wherein the agent A comprises epoxy resin and a reactive diluent, and the agent B comprises an amine curing agent and a curing accelerator; wherein:
the reactive diluent is at least one selected from the group consisting of cyclohexanediol ether, phenyl glycidyl ether, cyclohexanediol diglycidyl ether, polypropylene glycol diglycidyl ether, cyclohexanediol diglycidyl ester, glycerol triglycidyl ether, trimethylolpropane triglycidyl ether and pentaerythritol tetraglycidyl ether.
2. The encapsulant of claim 1, wherein the amine curing agent is at least one selected from diethylenetriamine, triethylenetetramine, polyetheramine, 4 ' -diaminodicyclohexylmethane, 3 ' -dimethyl-4, 4 ' -diaminodicyclohexylmethane, methylcyclohexanediamine, isophoronediamine, and 1, 3-cyclohexyldimethylamine.
3. The encapsulant of claim 1, wherein the epoxy resin is at least one selected from the group consisting of bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, and hydrogenated bisphenol A epoxy resin.
4. The encapsulant of claim 1, wherein the curing promoter is at least one member selected from salicylic acid, benzyldimethylamine, and aminoethylpiperazine.
5. The packaging adhesive according to any one of claims 1 to 4, wherein the agent A comprises 75 to 96 parts by mass of epoxy resin and 4 to 25 parts by mass of reactive diluent per 100 parts by mass of the agent A, and the agent B comprises 60 to 98 parts by mass of curing agent and 0.7 to 8 parts by mass of curing accelerator per 100 parts by mass of the agent B.
6. The packaging adhesive according to any one of claims 1 to 4, wherein the agent A further comprises other functional additives X, and the other functional additives X are selected from at least one of defoaming agents, dispersing agents, leveling agents and dyes.
7. The packaging adhesive as claimed in claim 6, wherein the defoamer is BYK-141, or/and the dispersant is BYK-9076, or/and the leveling agent is BYK-320, or/and the dye is a violet dye.
8. The packaging adhesive according to claim 6, wherein the other functional auxiliary X is added in an amount of 0.05 to 4 parts by mass per 100 parts by mass of the agent A.
9. The packaging adhesive as claimed in any one of claims 1 to 4, wherein the agent B further comprises other functional auxiliary agents Y, and the other functional auxiliary agents Y are selected from at least one of an antioxidant, an ultraviolet absorber and a chain extender.
10. The packaging adhesive according to claim 9, wherein the antioxidant is at least one selected from the group consisting of pentaerythritol tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, 8 tris (2, 4-di-tert-butylphenyl) phosphite, and N, N' -1, 6-hexylene-bis- [3, 5-di-tert-butyl-4-hydroxy-phenylacrylamide, or/and the ultraviolet absorbent is selected from at least one of hydroxyl triazine derivative and tetra-hydroxy-2, 2,6, 6-tetramethyl-1-piperidine ethanol bismethylsuccinic acid polymer, and/or the chain extender is selected from at least one of cyclohexanediol, hexanediol, benzyl alcohol and diethylene glycol ether alcohol.
11. The encapsulating adhesive according to claim 9, wherein the other functional auxiliary Y is added in an amount of 0.26 to 14 parts by mass per 100 parts by mass of the agent B.
12. The packaging adhesive according to any one of claims 1 to 4, 7 to 8 and 10 to 11, wherein the mass ratio of the agent A to the agent B is 100: (20-100).
13. A method for producing an encapsulating adhesive as claimed in any one of claims 1 to 12, characterized in that the production method comprises a step of producing the agent a and a step of producing the agent B;
the step of preparing the agent A comprises the following steps: mixing the components contained in the agent A;
the step of preparing the agent B comprises the following steps: mixing the components contained in the agent B.
14. A circuit board, characterized in that, the circuit board comprises a substrate and packaging glue, and the packaging glue of any claim 1 to 12 is adopted as the packaging glue.
15. A preparation method of a circuit board is characterized by comprising the following steps:
and taking the substrate, pouring the packaging adhesive, and curing.
16. The method for manufacturing a wiring board according to claim 15, wherein the curing temperature is 110 ℃ to 120 ℃, and the curing time is 4min to 8 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113835170A (en) * | 2021-11-26 | 2021-12-24 | 长芯盛（武汉）科技有限公司 | Injection molding packaging method of photoelectric module and photoelectric module thereof |
| CN116355566A (en) * | 2023-03-06 | 2023-06-30 | 山东凯恩新材料科技有限公司 | Packaging adhesive and preparation method and application thereof |
| CN116731286A (en) * | 2023-08-08 | 2023-09-12 | 宁德时代新能源科技股份有限公司 | Modified hydrogenated bisphenol type epoxy resin and preparation method and application thereof |
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| CN110845980A (en) * | 2019-10-09 | 2020-02-28 | 深圳大学 | COB packaging adhesive and preparation method thereof |
| CN111454679A (en) * | 2019-01-18 | 2020-07-28 | 杨超 | L ED molding packaging adhesive and using method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113835170A (en) * | 2021-11-26 | 2021-12-24 | 长芯盛（武汉）科技有限公司 | Injection molding packaging method of photoelectric module and photoelectric module thereof |
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| CN116355566B (en) * | 2023-03-06 | 2024-03-15 | 山东凯恩新材料科技有限公司 | Packaging adhesive and preparation method and application thereof |
| CN116731286A (en) * | 2023-08-08 | 2023-09-12 | 宁德时代新能源科技股份有限公司 | Modified hydrogenated bisphenol type epoxy resin and preparation method and application thereof |
| CN116731286B (en) * | 2023-08-08 | 2024-01-19 | 宁德时代新能源科技股份有限公司 | Modified hydrogenated bisphenol type epoxy resin and preparation method and application thereof |
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| CN112940654B (en) | 2023-01-31 |
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