CN117264367A - Epoxy resin material and preparation method and application thereof - Google Patents
Epoxy resin material and preparation method and application thereof Download PDFInfo
- Publication number
- CN117264367A CN117264367A CN202311137423.3A CN202311137423A CN117264367A CN 117264367 A CN117264367 A CN 117264367A CN 202311137423 A CN202311137423 A CN 202311137423A CN 117264367 A CN117264367 A CN 117264367A
- Authority
- CN
- China
- Prior art keywords
- epoxy resin
- resin material
- weight
- contained
- amount
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 153
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 153
- 239000000463 material Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 48
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 36
- 239000005011 phenolic resin Substances 0.000 claims abstract description 36
- 239000000945 filler Substances 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 19
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 21
- 239000007822 coupling agent Substances 0.000 claims description 18
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 claims description 18
- 239000003086 colorant Substances 0.000 claims description 17
- 150000002500 ions Chemical class 0.000 claims description 17
- 239000003607 modifier Substances 0.000 claims description 17
- 235000010290 biphenyl Nutrition 0.000 claims description 16
- 239000004305 biphenyl Substances 0.000 claims description 16
- 229920003986 novolac Polymers 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002516 radical scavenger Substances 0.000 claims description 10
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- -1 aralkyl phenol Chemical compound 0.000 claims description 8
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 6
- 239000006082 mold release agent Substances 0.000 claims description 6
- 239000005350 fused silica glass Substances 0.000 claims description 5
- RGBIPJJZHWFFGE-UHFFFAOYSA-N cyclohexa-2,5-diene-1,4-dione;triphenylphosphane Chemical group O=C1C=CC(=O)C=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RGBIPJJZHWFFGE-UHFFFAOYSA-N 0.000 claims description 4
- 125000001624 naphthyl group Chemical group 0.000 claims description 4
- 239000004065 semiconductor Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 3
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 3
- 229910002026 crystalline silica Inorganic materials 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 125000000623 heterocyclic group Chemical group 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- JUAHKSBERRLSHD-UHFFFAOYSA-N tetraphenyl-$l^{5}-phosphane Chemical class C1=CC=CC=C1P(C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 JUAHKSBERRLSHD-UHFFFAOYSA-N 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims description 2
- 125000004185 ester group Chemical group 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 9
- 238000003756 stirring Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000013022 formulation composition Substances 0.000 description 6
- 239000004593 Epoxy Substances 0.000 description 5
- 239000005022 packaging material Substances 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 230000009477 glass transition Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical group [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 229960001545 hydrotalcite Drugs 0.000 description 2
- 229910001701 hydrotalcite Inorganic materials 0.000 description 2
- 235000013873 oxidized polyethylene wax Nutrition 0.000 description 2
- 239000004209 oxidized polyethylene wax Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical group CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920006336 epoxy molding compound Polymers 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- 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
- C08G59/62—Alcohols or phenols
- C08G59/621—Phenols
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of epoxy resin compositions, in particular to an epoxy resin material and a preparation method and application thereof, and especially relates to a high-pressure-resistant epoxy resin material and a preparation method and application thereof. The raw materials of the epoxy resin material comprise epoxy resin, a curing agent, a solid filler and an accelerator, wherein the curing agent contains phenolic resin with a structure shown in a formula (1), m is more than or equal to 1, n is more than or equal to 1, and m and n are independent integers. The epoxy resin material prepared by the invention has good high-pressure resistance, particularly under the high-temperature condition, the high-pressure resistance can reach more than 1200V, in addition, the epoxy resin material has better reliability,
Description
Technical Field
The invention relates to the technical field of epoxy resin compositions, in particular to an epoxy resin material and a preparation method and application thereof, and especially relates to a high-pressure-resistant epoxy resin material and a preparation method and application thereof.
Background
The epoxy resin is used as a main resin and a curing agent to be cured at high temperature under the action of a curing accelerator, wherein the combination of the epoxy resin and the phenolic resin is the main stream of the current electronic plastic packaging material, and the plastic packaging material meeting the electronic packaging requirement can be prepared by adding inorganic fillers such as silicon dioxide, calcium carbonate and the like, flame retardants and various auxiliary agents into the materials. Epoxy molding compounds have many beneficial properties and are commonly used in the field of electronic packaging.
With the development of the semiconductor industry, the requirements for packaging materials are also increasing, and particularly, devices with special applications pose greater challenges for high voltage resistance, particularly at high temperatures. Patent CN109651762a discloses a high pressure resistant epoxy resin composition, which uses an epoxy resin with a special structure and a coupling agent with a special functional structure, so that the epoxy resin composition can resist high pressure impact after plastic packaging is completed, and the high pressure resistance reaches 5000V or higher, but the high pressure resistance of the product at high temperature is not mentioned.
Disclosure of Invention
The invention aims at providing higher requirements for the high-pressure resistance of an epoxy plastic package material, particularly the high-pressure resistance at high temperature in the prior art, but the current epoxy plastic package material only has better high-pressure resistance at normal temperature, so that an epoxy resin material and a preparation method and application thereof are provided. The epoxy resin material is prepared by adopting the curing agent with a specific structure as a raw material, so that the epoxy resin material has better high-pressure resistance, and meanwhile, under the high-temperature condition, the high-pressure resistance of the epoxy resin material reaches more than 1200V, and in addition, the epoxy resin material also has better reliability.
In order to achieve the above object, the first aspect of the present invention provides an epoxy resin material, which is prepared from raw materials comprising an epoxy resin, a curing agent, a solid filler and an accelerator, wherein the curing agent comprises a phenolic resin of a structure represented by formula (1),
wherein m is greater than or equal to 1, n is greater than or equal to 1, and m and n are each independently integers.
Preferably, the mass ratio of the epoxy resin, the curing agent, the solid filler and the accelerator is 10-70:5-50:150-500:1.
preferably, the phenolic resin of the structure shown in formula (1) is present in an amount of 50% by weight or more, based on 100% by weight of the total weight of the curing agent.
Preferably, the curing agent further contains one or more of a novolac resin, a biphenyl novolac resin, a naphthalene novolac resin, an aralkyl phenol novolac resin, and a polyfunctional novolac resin.
Preferably, the epoxy resin is selected from one or more of o-cresol epoxy resin, biphenyl type epoxy resin, aralkyl type epoxy resin, ester ring type epoxy resin, heterocyclic type epoxy resin, bisphenol a type epoxy resin, bisphenol F type epoxy resin, dicyclopentadiene type epoxy resin, naphthalene ring type epoxy resin, and multifunctional type epoxy resin.
Preferably, the solid filler is crystalline silica and/or fused silica.
Preferably, the accelerator is triphenylphosphine-1, 4-benzoquinone adduct and/or tetraphenylphosphine salt.
Preferably, the raw materials for preparing the epoxy resin material further comprise one or more than two of a release agent, a colorant, a coupling agent, a low-stress modifier and an ion trapping agent.
Preferably, the epoxy resin material comprises 1 to 20 wt%, the curing agent comprises 1 to 15 wt%, the solid filler comprises 60 to 90 wt%, the accelerator comprises 0.01 to 1 wt%, the release agent comprises 0.1 to 1 wt%, the colorant comprises 0.1 to 1 wt%, the coupling agent comprises 0.1 to 1 wt%, the low stress modifier comprises 0.1 to 1 wt%, and the ion scavenger comprises 0.1 to 1 wt%, based on 100 wt% of the total weight of the raw materials of the epoxy resin material.
The second aspect of the present invention provides a method for preparing the epoxy resin material, which comprises the following steps:
(1) Heating and melting the curing agent, and then cooling and crushing to obtain an intermediate;
(2) Mixing the intermediate obtained in the step (1), epoxy resin, solid filler and accelerator;
(3) Extruding the material obtained in the step (2), and molding to obtain the epoxy resin material.
Preferably, in step (1), the temperature of the heating to melt is 100-150 ℃.
Preferably, in step (3), the temperature of the extrusion is 85-105 ℃.
The third aspect of the invention provides an application of the epoxy resin material in a semiconductor packaging material.
Through the technical scheme, the epoxy resin material provided by the invention has the following beneficial effects:
according to the invention, phenolic resin with a specific structure is used as a curing agent, so that the finally prepared epoxy resin material has good high-pressure resistance; after the product is molded, the high-pressure resistance of the product reaches over 1200V, especially under the high-temperature condition, and the epoxy resin material has better reliability.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The first aspect of the invention provides an epoxy resin material, which is prepared from raw materials including epoxy resin, a curing agent, a solid filler and an accelerator, wherein the curing agent contains phenolic resin with a structure shown as a formula (1),
wherein m is greater than or equal to 1, n is greater than or equal to 1, and m and n are each independently integers.
In order to make the epoxy resin material prepared have better high-pressure resistance at high temperature, in a preferred embodiment, the phenolic resin with the structure shown in the formula (1) is obtained commercially, and the manufacturer is Xin-dao Dai gold chemical Co., ltd, and the product mark is HE-510-05.
In the epoxy resin material, the content of the phenolic resin with the structure shown in the formula (1) is more than or equal to 50 weight percent based on 100 weight percent of the total weight of the curing agent.
In a specific embodiment of the epoxy resin material of the present invention, the curing agent further contains one or more of a novolac resin, a biphenyl type novolac resin, a naphthalene type novolac resin, an aralkyl phenol type novolac resin, and a polyfunctional group type novolac resin.
In the epoxy resin material of the present invention, in specific embodiments, the epoxy resin may be a conventional choice in the art. In a preferred embodiment, the epoxy resin is selected from one or two or more of o-cresol epoxy resin, biphenyl type epoxy resin, aralkyl type epoxy resin, ester ring type epoxy resin, heterocyclic type epoxy resin, bisphenol a type epoxy resin, bisphenol F type epoxy resin, dicyclopentadiene type epoxy resin, naphthalene ring type epoxy resin, and multifunctional type epoxy resin. In a more preferred embodiment, the epoxy resin is selected from one or more of o-cresol epoxy resin, biphenyl epoxy resin and multifunctional epoxy resin.
In the epoxy resin material of the present invention, the solid filler is crystalline silica and/or fused silica. In a preferred embodiment, the solid filler is fused silica. In a more preferred embodiment, the solid filler has a maximum particle size of 75 μm and a median particle size of 15-25 μm.
In the epoxy resin material, the accelerator is triphenylphosphine-1, 4-benzoquinone adduct and/or tetraphenylphosphine salt.
In order to make the prepared epoxy resin material have better high-pressure resistance performance at high temperature and better reliability, the dosages of the epoxy resin, the curing agent, the solid filler and the accelerator need to be reasonably controlled, and in a preferred embodiment, the mass ratio of the dosages of the epoxy resin, the curing agent, the solid filler and the accelerator is 10-70:5-50:150-500:1, for example 10:5:150: 1. 20:15:200: 1. 22:17:450: 1. 23.3:17.3:283: 1. 33:23.5:187.5: 1. 36.5:24:266.7: 1. 37.5:39:415: 1. 45:33:410:1 or 70:50:500:1.
in the epoxy resin material of the present invention, in a specific embodiment, the raw material for preparing the epoxy resin material further contains one or more of a mold release agent, a colorant, a coupling agent, a low stress modifier, and an ion scavenger.
In the epoxy resin material of the present invention, in a specific embodiment, the mold release agent may be a conventional choice in the art. In a preferred embodiment, the release agent is an oxidized polyethylene wax.
In the epoxy materials of the present invention, in particular embodiments, the colorant may be a conventional choice in the art. In a preferred embodiment, the colorant is carbon black.
In the epoxy resin material of the present invention, in a specific embodiment, the coupling agent may be a conventional choice in the art. In a preferred embodiment, the coupling agent is gamma-glycidoxypropyl trimethoxysilane (KH 560).
In the epoxy materials of the present invention, in particular embodiments, the low stress modifier may be a conventional choice in the art. In a preferred embodiment, the low stress modifier is a silicone modified epoxy resin.
In the epoxy materials of the present invention, in particular embodiments, the ion scavenger may be a conventional choice in the art. In a preferred embodiment, the ion scavenger is hydrotalcite.
In the epoxy resin material of the present invention, in a specific embodiment, the epoxy resin is 1 to 20 wt%, the curing agent is 1 to 15 wt%, the solid filler is 60 to 90 wt%, the accelerator is 0.01 to 1 wt%, the releasing agent is 0.1 to 1 wt%, the colorant is 0.1 to 1 wt%, the coupling agent is 0.1 to 1 wt%, the low stress modifier is 0.1 to 1 wt%, and the ion scavenger is 0.1 to 1 wt%, based on 100 wt% of the total weight of the raw materials of the epoxy resin material.
In the epoxy resin material according to the present invention, in a preferred embodiment, the epoxy resin is contained in an amount of 4 to 15 wt%, the curing agent is contained in an amount of 3 to 10 wt%, the solid filler is contained in an amount of 75 to 90 wt%, the accelerator is contained in an amount of 0.2 to 0.4 wt%, the releasing agent is contained in an amount of 0.3 to 0.8 wt%, the colorant is contained in an amount of 0.3 to 0.5 wt%, the coupling agent is contained in an amount of 0.2 to 0.8 wt%, the low-stress modifier is contained in an amount of 0.2 to 0.5 wt%, and the ion scavenger is contained in an amount of 0.1 to 0.5 wt%, based on 100 wt% of the total weight of the raw materials of the epoxy resin material.
The second aspect of the present invention provides a method for preparing the epoxy resin material, which comprises the following steps:
(1) Heating and melting the curing agent, and then cooling and crushing to obtain an intermediate;
(2) Mixing the intermediate obtained in the step (1), epoxy resin, solid filler and accelerator;
(3) Extruding the material obtained in the step (2), and molding to obtain the epoxy resin material.
In the process of the present invention, in step (1), the curing agent, the low stress modifier and the mold release agent are melted by heating in a preferred embodiment.
In the method of the present invention, in step (1), in a specific embodiment, the temperature of the heat melting is 100 to 150 ℃.
In the process according to the invention, in step (2), in a preferred embodiment, the intermediate obtained in step (1), the epoxy resin, the solid filler, the accelerator, the colorant, the coupling agent and the ion scavenger are mixed.
In the process of the invention, in step (3), in a specific embodiment, the extrusion temperature is from 85 to 105 ℃.
The third aspect of the invention provides an application of the epoxy resin material in a semiconductor packaging material.
The present invention will be described in detail by way of examples, but the scope of the present invention is not limited thereto.
In the following examples and comparative examples:
a1: the structural phenolic resin shown in the formula (1) is purchased from Nippon iron and gold chemistry Co., ltd, and the brand is HE-510-05;
a2: phenolic novolac resin, available from Jinan Shengquan group Co., ltd, brand PF 8010;
a3: multifunctional phenolic resin, available from Ming He Chemicals, under the trade designation MEH 7500;
a4: biphenyl type phenolic resin, available from Ming He Chemicals, trade name MEH 7851SS;
a5: XYLOK phenolic resin, available from Jinan Shengquan group Co., ltd, brand SH 4064;
a6: naphthalene type phenolic resin, which is purchased from Xin-Ri iron and Zhu Jing chemical Co., ltd, and has the trade name SN 485;
b1: biphenyl type epoxy resin, which is purchased from Mitsubishi chemical corporation and has the brand YX4000;
b2: multifunctional epoxy resin available from DIC corporation under the trade designation HP 7241;
b3: o-cresol epoxy resin, available from Jinan Shengquan group Co., ltd, brand SQCN 700-3;
c: solid filler: fused silica (maximum particle size 75 μm, median particle size 15-25 μm), available from Jiangsu-associated New Material Co., ltd;
d: coupling agent: gamma-glycidoxypropyl trimethoxysilane, available from Jiangsu morning photo-coupling agent Co., ltd, brand KH 560;
e: and (3) an accelerator: triphenylphosphine-1, 4-benzoquinone adduct, available from Nanjing blue Bian biochemical technology Co., ltd, under the trademark TPP-BQ;
f: low stress modifier: the organosilicon modified epoxy resin is purchased from Dow Corning company and has the brand of SF-8241EG;
g: and (3) a release agent: oxidized polyethylene wax, available from clariant under the trade designation PED 522;
h: ion scavenger: hydrotalcite, available from Japan Kogyo chemical Co., ltd., trade name DHT-4C;
i: coloring agent: carbon black, available from Mitsubishi chemical corporation under the trademark MA100.
Example 1
Example 1 the raw material formulation composition for preparing the epoxy resin material is shown in table 1.
The method for preparing the epoxy resin material in this example is as follows:
(1) Heating and melting phenolic resin with a structure shown in a formula (1), a release agent and a low-stress modifier in proportion at 100 ℃, and then cooling and crushing to prepare an intermediate;
(2) Stirring and mixing the intermediate obtained in the step (1), biphenyl epoxy resin, o-cresol epoxy resin, solid filler, colorant, accelerator, coupling agent and ion capturing agent in proportion;
(3) Extruding the material obtained in the step (2) through double screws, wherein the temperature of the material extruded through the double screws is controlled at 100 ℃, and after tabletting and cooling, the material is crushed and pre-pressed and molded by a cake making machine, so that the epoxy resin material is prepared.
Example 2
Example 2 the raw material formulation composition for preparing the epoxy resin material is shown in table 1.
The method for preparing the epoxy resin material in this example is as follows:
(1) Heating and melting phenolic resin, biphenyl type phenolic resin, release agent and low-stress modifier with the structure shown in formula (1) at the temperature of 120 ℃ in proportion, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate obtained in the step (1), biphenyl epoxy resin, solid filler, colorant, accelerator, coupling agent and ion capturing agent in proportion;
(3) Extruding the material obtained in the step (2) through double screws, wherein the temperature of the material extruded through the double screws is controlled to be 105 ℃, and after tabletting and cooling, the material is crushed and pre-pressed and molded by a cake making machine, so that the epoxy resin material is prepared.
Example 3
Example 3 the raw material formulation composition for preparing the epoxy resin material is shown in table 1.
The method for preparing the epoxy resin material in this example is as follows:
the method comprises the steps of heating and melting phenolic resin, linear phenolic resin, multifunctional phenolic resin, release agent and low-stress modifier with the structure shown in the formula (1) at 130 ℃ in proportion, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate obtained in the step (1), biphenyl epoxy resin, multifunctional epoxy resin, o-cresol epoxy resin, solid filler, colorant, accelerator, coupling agent and ion capturing agent in proportion;
(3) Extruding the material obtained in the step (2) through double screws, wherein the temperature of the material extruded through the double screws is controlled at 100 ℃, and after tabletting and cooling, the material is crushed and pre-pressed and molded by a cake making machine, so that the epoxy resin material is prepared.
Example 4
Example 4 the raw material formulation composition for preparing the epoxy resin material is shown in table 1.
The method for preparing the epoxy resin material in this example is as follows:
(1) Heating and melting phenolic resin, linear phenolic resin, a mold release agent and a low-stress modifier with the structure shown in the formula (1) at 140 ℃ in proportion, cooling and crushing to prepare an intermediate;
(2) Stirring and mixing the intermediate obtained in the step (1), the multifunctional epoxy resin, the solid filler, the colorant, the accelerator, the coupling agent and the ion capturing agent in proportion;
(3) Extruding the material obtained in the step (2) through double screws, wherein the temperature of the material extruded through the double screws is controlled at 85 ℃, and after tabletting and cooling, the material is crushed and pre-pressed and molded by a cake making machine, so that the epoxy resin material is prepared.
Example 5
Example 5 the raw material formulation composition for preparing the epoxy resin material is shown in table 1.
The method for preparing the epoxy resin material in this example is as follows:
(1) Heating and melting phenolic resin, biphenyl type phenolic resin, release agent and low-stress modifier with the structure shown in formula (1) at 150 ℃ in proportion, cooling and crushing to prepare an intermediate;
(2) Stirring and mixing the intermediate obtained in the step (1), biphenyl epoxy resin, o-cresol epoxy resin, solid filler, colorant, accelerator, coupling agent and ion capturing agent in proportion;
(3) Extruding the material obtained in the step (2) through double screws, wherein the temperature of the material extruded through the double screws is controlled at 100 ℃, and after tabletting and cooling, the material is crushed and pre-pressed and molded by a cake making machine, so that the epoxy resin material is prepared.
Example 6
Example 6 the raw material formulation composition for preparing the epoxy resin material is shown in table 1.
The method for preparing the epoxy resin material in this example is as follows:
(1) The method comprises the steps of heating and melting phenolic resin with a structure shown in a formula (1), multifunctional phenolic resin, a mold release agent and a low-stress modifier in proportion at 130 ℃, cooling and crushing to prepare an intermediate;
(2) Stirring and mixing the intermediate obtained in the step (1), o-cresol epoxy resin, solid filler, colorant, accelerator, coupling agent and ion capturing agent in proportion;
(3) Extruding the material obtained in the step (2) through double screws, wherein the temperature of the material extruded through the double screws is controlled at 100 ℃, and after tabletting and cooling, the material is crushed and pre-pressed and molded by a cake making machine, so that the epoxy resin material is prepared.
Comparative example 1
The procedure of example 1 was followed, except that the phenolic resin having the structure represented by formula (1) was replaced with a multifunctional phenolic resin.
Comparative example 2
The procedure of example 2 was followed except that the phenolic resin of the structure shown in formula (1) was replaced with the XYLOK phenolic resin in its entirety.
Comparative example 3
The procedure of example 3 was followed, except that the phenolic resin having the structure represented by formula (1) was replaced with a biphenyl type phenolic resin.
Comparative example 4
The procedure of example 4 was followed except that the phenolic resin having the structure represented by formula (1) was replaced with a naphthalene type phenolic resin.
Table 1: examples 1 to 6 and comparative examples 1 to 4 raw material ratios
The products prepared in examples 1 to 6 and comparative examples 1 to 4 were respectively subjected to gel time, flowability, glass transition temperature, electrical properties (high voltage resistance) and reliability tests.
Test case
(1) Gel time: heating an electric hot plate to 175+/-1 ℃, placing 2-3g of a sample on an iron plate, continuously stirring with a small needle, and testing the time for the sample to change from fluid to colloid.
(2) Fluidity: a30 g sample was taken and measured by a resin transfer injection molding machine with the aid of a spiral flow metal mold at an injection pressure of 70kgf/cm2 and a mold temperature of 175.+ -. 1 ℃.
(3) Glass transition temperature: the test was performed using a thermo-mechanical analyzer (TMA).
(4) Electrical properties (high voltage resistance): taking SOP8 as an example, after the completion of the encapsulation at 175 ℃, the post-curing was performed at 175 ℃ for 8 hours, and then the high pressure resistance was tested at 150 ℃ under 1200V high pressure.
(5) Reliability: and (3) baking the qualified product at 125 ℃ for 24 hours, then placing the product in a moisture absorption box with the temperature of 30 ℃/humidity of 60% RH for moisture absorption for 168 hours, directly performing infrared reflow soldering for 3 times (the highest temperature of 260 ℃), and testing the layering condition of the product by using an ultrasonic scanner.
The results of the gel time, flowability, glass transition temperature, electrical properties (high voltage resistance) and reliability test of the epoxy resin materials prepared in examples 1 to 6 and comparative examples 1 to 4 are shown in Table 2.
TABLE 2
From the test results of examples 1 to 6 and comparative examples 1 to 4, it can be seen that: the phenolic resin with the structure shown in the formula (1) is used as a curing agent, so that the finally prepared epoxy resin material has good high-pressure resistance; after the product is molded, the high-pressure resistance of the product reaches over 1200V, and in addition, the epoxy resin material has better reliability, and meanwhile, the flow property, the glass transition temperature and the electrical property of the product are better.
The foregoing is merely exemplary embodiments of the present invention and are not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. An epoxy resin material is characterized in that the raw materials for preparing the epoxy resin material comprise epoxy resin, a curing agent, solid filler and an accelerator, wherein the curing agent comprises phenolic resin with a structure shown in a formula (1),
wherein m is greater than or equal to 1, n is greater than or equal to 1, and m and n are each independently integers.
2. The epoxy resin material according to claim 1, wherein the mass ratio of the amounts of the epoxy resin, the curing agent, the solid filler and the accelerator is 10 to 70:5-50:150-500:1.
3. the epoxy resin material according to claim 1 or 2, wherein the phenolic resin of the structure represented by formula (1) is contained in an amount of 50% by weight or more based on 100% by weight of the total weight of the curing agent.
4. The epoxy resin material according to claim 1, wherein the curing agent further contains one or more of a novolac resin, a biphenyl novolac resin, a naphthalene novolac resin, an aralkyl phenol novolac resin, and a polyfunctional novolac resin.
5. The epoxy resin material according to claim 1, wherein the epoxy resin is one or two or more selected from the group consisting of o-cresol epoxy resin, biphenyl epoxy resin, aralkyl epoxy resin, ester ring type epoxy resin, heterocyclic type epoxy resin, bisphenol a type epoxy resin, bisphenol F type epoxy resin, dicyclopentadiene type epoxy resin, naphthalene ring type epoxy resin, and polyfunctional type epoxy resin;
preferably, the solid filler is crystalline silica and/or fused silica;
preferably, the accelerator is triphenylphosphine-1, 4-benzoquinone adduct and/or tetraphenylphosphine salt.
6. The epoxy resin material according to claim 1, wherein the raw material for producing the epoxy resin material further contains one or more of a mold release agent, a colorant, a coupling agent, a low-stress modifier and an ion scavenger.
7. The epoxy resin material according to claim 6, wherein the epoxy resin is contained in an amount of 1 to 20% by weight, the curing agent is contained in an amount of 1 to 15% by weight, the solid filler is contained in an amount of 60 to 90% by weight, the accelerator is contained in an amount of 0.01 to 1% by weight, the releasing agent is contained in an amount of 0.1 to 1% by weight, the colorant is contained in an amount of 0.1 to 1% by weight, the coupling agent is contained in an amount of 0.1 to 1% by weight, the low-stress modifier is contained in an amount of 0.1 to 1% by weight, and the ion scavenger is contained in an amount of 0.1 to 1% by weight, based on 100% by weight of the total weight of the raw materials of the epoxy resin material.
8. A method for producing an epoxy resin material according to any one of claims 1 to 7, characterized in that the method comprises the steps of:
(1) Heating and melting the curing agent, and then cooling and crushing to obtain an intermediate;
(2) Mixing the intermediate obtained in the step (1), epoxy resin, solid filler and accelerator;
(3) Extruding the material obtained in the step (2), and molding to obtain the epoxy resin material.
9. The method of claim 8, wherein in step (1), the temperature of the heat melting is 100-150 ℃;
preferably, in step (3), the temperature of the extrusion is 85-105 ℃.
10. Use of an epoxy resin material according to any one of claims 1 to 7 and an epoxy resin material prepared by the method according to claim 8 or 9 in a semiconductor encapsulation material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311137423.3A CN117264367A (en) | 2023-09-05 | 2023-09-05 | Epoxy resin material and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311137423.3A CN117264367A (en) | 2023-09-05 | 2023-09-05 | Epoxy resin material and preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117264367A true CN117264367A (en) | 2023-12-22 |
Family
ID=89205390
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311137423.3A Pending CN117264367A (en) | 2023-09-05 | 2023-09-05 | Epoxy resin material and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117264367A (en) |
-
2023
- 2023-09-05 CN CN202311137423.3A patent/CN117264367A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113201204B (en) | High Tg and low warp MUF epoxy resin composition and preparation method thereof | |
| US20020128354A1 (en) | Novel hardener for epoxy molding compounds | |
| CN114456543A (en) | Epoxy resin composition, epoxy resin plastic packaging material, and preparation method and application thereof | |
| CN112980139A (en) | Epoxy resin composition for tantalum capacitor packaging and preparation method thereof | |
| CN109651762B (en) | High-pressure-resistant epoxy resin composition and preparation method thereof | |
| CN117264367A (en) | Epoxy resin material and preparation method and application thereof | |
| CN112679141A (en) | Epoxy resin composition for improving appearance of semiconductor package and preparation method thereof | |
| CN114276651B (en) | Epoxy resin composition suitable for low-pressure encapsulation and preparation method thereof | |
| KR102228914B1 (en) | Epoxy resin composition | |
| CN114276650A (en) | Epoxy resin composition and preparation method thereof | |
| CN115572459B (en) | Epoxy resin material and preparation method thereof | |
| JP3916783B2 (en) | Epoxy resin composition for semiconductor encapsulation and semiconductor device using the same | |
| TWI343925B (en) | Epoxy resin composition for packaging semiconductor device, method of making the same, and semiconductor device using the same | |
| JP3551281B2 (en) | Epoxy resin composition | |
| JPH01152151A (en) | Epoxy resin composition | |
| CN111117158A (en) | Low-cost low-stress epoxy composition and preparation method thereof | |
| JPS62112622A (en) | Sealing resin composition | |
| JP3573565B2 (en) | Epoxy resin composition tablet | |
| JPH06239976A (en) | Epoxy resin composition and sealed semiconductor device | |
| JPH0621152B2 (en) | Sealing resin composition | |
| KR960000217B1 (en) | Semiconductor device mold epoxy resin | |
| JPS60161423A (en) | Resin composition for sealing | |
| JPH0562612B2 (en) | ||
| JPH0275619A (en) | Epoxy resin composition for sealing semiconductor | |
| JP3468900B2 (en) | Semiconductor device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |