CN116515242A - High-dielectric-constant powdery epoxy molding compound and preparation method thereof - Google Patents
High-dielectric-constant powdery epoxy molding compound and preparation method thereof Download PDFInfo
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- CN116515242A CN116515242A CN202310455702.8A CN202310455702A CN116515242A CN 116515242 A CN116515242 A CN 116515242A CN 202310455702 A CN202310455702 A CN 202310455702A CN 116515242 A CN116515242 A CN 116515242A
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- epoxy
- epoxy resin
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- 229920006336 epoxy molding compound Polymers 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003822 epoxy resin Substances 0.000 claims abstract description 84
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 84
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 45
- 239000004593 Epoxy Substances 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 34
- 229920003023 plastic Polymers 0.000 claims abstract description 30
- 239000004033 plastic Substances 0.000 claims abstract description 30
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 26
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 23
- 239000000654 additive Substances 0.000 claims abstract description 20
- 230000000996 additive effect Effects 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 20
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 38
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 36
- 229920001568 phenolic resin Polymers 0.000 claims description 36
- 239000005011 phenolic resin Substances 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 23
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 238000004806 packaging method and process Methods 0.000 claims description 9
- 239000007822 coupling agent Substances 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 5
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002113 barium titanate Inorganic materials 0.000 claims description 3
- JRQJLSWAMYZFGP-UHFFFAOYSA-N 1,1'-biphenyl;phenol Chemical group OC1=CC=CC=C1.C1=CC=CC=C1C1=CC=CC=C1 JRQJLSWAMYZFGP-UHFFFAOYSA-N 0.000 claims description 2
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003086 colorant Substances 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 229920003986 novolac Polymers 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 2
- 239000007767 bonding agent Substances 0.000 claims 1
- 239000006082 mold release agent Substances 0.000 claims 1
- 239000002516 radical scavenger Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 8
- 238000000748 compression moulding Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 15
- 229920001903 high density polyethylene Polymers 0.000 description 11
- 239000004700 high-density polyethylene Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 10
- 238000001125 extrusion Methods 0.000 description 5
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001721 transfer moulding 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the field of C08L63/00, in particular to a powdery epoxy molding compound with high dielectric constant and a preparation method thereof. The preparation raw materials at least comprise the following components in parts by weight: 3-8 parts of epoxy resin, 2-5 parts of curing agent, 0.2-0.5 part of silane coupling agent, 0.1-1 part of additive, 0-30 parts of silicon dioxide and 50-92 parts of high dielectric constant filler. The high-content addition of the low-grain-size aluminum oxide is realized by optimizing the formula and the preparation process, the epoxy plastic package material in the form of solid powder with high dielectric constant is prepared, and the plastic package is carried out by adopting a compression molding method in combination with a package testing factory, so that the chip performance can be comprehensively improved from the aspects of performance (high dielectric constant) and product structure (thin plastic package thickness).
Description
Technical Field
The invention relates to the field of C08L63/00, in particular to a powdery epoxy molding compound with high dielectric constant and a preparation method thereof.
Background
In recent years, in mobile phones, a touch chip is gradually formed on a flat plate, and an epoxy molding compound packaged by the touch chip needs a high dielectric constant to effectively and rapidly conduct bioelectricity of a human body to the inside of the chip during working so as to trigger a chip function. On the other hand, the thinner the epoxy molding compound above the package, the smaller the loss thereof, and the more sensitive the chip function. The traditional transfer molding can not meet the requirements, and injection molding is needed to be carried out by adopting a compression molding method; for example, chinese patent application (publication No. CN 107141721B) discloses a high dielectric constant epoxy resin composition and a preparation method thereof, wherein a high dielectric filler, a stress absorber and fumed silica are introduced into a system of epoxy resin, a curing agent and a curing agent accelerator, wherein the high dielectric filler is barium titanate or alumina, which can achieve a high dielectric constant of 7 or more, but the fluidity of the prepared product needs to be further improved. Therefore, it is important to provide an epoxy molding compound in the form of solid powder with high dielectric constant to use the use requirement of compression molding method and the requirement of thin package.
Disclosure of Invention
The invention provides a high-dielectric-constant powdery epoxy molding compound, which is prepared from the following raw materials in parts by weight: 3-8 parts of epoxy resin, 2-5 parts of curing agent, 0.2-0.5 part of silane coupling agent, 0.1-1 part of additive, 0-30 parts of silicon dioxide and 50-92 parts of high dielectric constant filler.
As a preferable technical scheme, the additive is at least one of a release agent, an ion capturing agent, a colorant, a binding agent and a low-stress agent; preferably, the additive is a release agent; preferably, the release agent is a high density polyethylene oxidized wax (Honeywell AC 316A);
based on the system, the high-density polyethylene oxidized wax is introduced as a release agent, so that the plastic package material product has excellent metal stripping property, and the processing difficulty is reduced. In addition, the inventor unexpectedly discovers that the added high-density polyethylene oxidized wax and the coupling agent in the system jointly act to realize good dispersion of silicon dioxide and high-dielectric constant filler in the system, and ensure that the spiral flow length of the prepared product is at a proper level.
As a preferable technical scheme, the silane coupling agent is an epoxy silane coupling agent; preferably, the epoxy silane coupling agent is 3- (2, 3-glycidoxy) propyl trimethoxysilane (KH-560).
Based on the system, the epoxy silane coupling agent, especially KH-560 is introduced, so that the combination of silicon dioxide, aluminum oxide and resin in the system is realized, and meanwhile, the high-density polyethylene oxidized wax in the system is matched, so that the fluidity of a plastic package product is effectively improved, and the use requirement of thin package is met.
As a preferable technical scheme, the epoxy resin is at least one of polyaromatic epoxy resin, polyfunctional epoxy resin, bisphenol A type epoxy resin and phenol biphenyl type epoxy resin.
Preferably, the epoxy resin is a combination of bisphenol a type epoxy resin and multifunctional epoxy resin; the mass ratio of the bisphenol A type epoxy resin to the multifunctional epoxy resin is (1-4): (4-1).
Preferably, the bisphenol A type epoxy resin has an epoxy equivalent of 176-184g/eq.
Preferably, the epoxy equivalent of the multifunctional epoxy resin is 165-174g/eq.
The types of the bisphenol A type epoxy resin and the multifunctional epoxy resin are NPEL-127 (Nanya) and 1032H60 (Mitsubishi chemical).
As a preferable technical scheme, the curing agent is a combination of a linear phenolic resin and a multifunctional phenolic resin; the mass ratio of the linear phenolic resin to the multifunctional phenolic resin is (1-3): (1-2).
Preferably, the type of the phenolic novolac resin is PF-8011 (holy spring in Shandong); the model of the multifunctional phenolic resin is MEH-7500 (Ming He Chemicals).
Based on the system, the problem of spiral flow length reduction of the plastic package material due to excessive high molecular weight of the resin and excessive increase of molecular chain length is avoided on the premise of ensuring that the basic performance of the plastic package material meets the requirement by adopting the combined action of bisphenol A type epoxy resin, multifunctional epoxy resin, linear phenolic resin and multifunctional phenolic resin combined curing agent.
As a preferred embodiment, the silica has a maximum particle size of 20 to 30. Mu.m, preferably 20. Mu.m.
As a preferable technical scheme, the high dielectric constant filler is at least one selected from aluminum oxide, barium titanate, calcium titanate and strontium titanate;
preferably, the high dielectric constant filler is aluminum oxide; the maximum particle size of the aluminum oxide is 25-35 μm, preferably 25 μm.
As a preferable technical scheme, the mass ratio of the silicon dioxide to the high dielectric constant filler is (5-10): (82-87).
The inventor finds that the dispersibility of the aluminum oxide is poor along with the reduction of the particle size in the exploration process, and the fluidity of a system is poor, in order to realize that the plastic package material meets the requirement of thin plastic package, the maximum particle size of the aluminum oxide is controlled to be 25 microns, and the inventor ensures that the spiral flow length of the plastic package material is more than 55 inches while ensuring that the provided product has a dielectric constant higher than 7 and low dielectric loss under the combined action of various raw materials in the system by matching and introducing silicon dioxide with the maximum particle size of 20 microns, so that the internal structure of the product is prevented from being damaged due to the excessively high viscosity of the powdery epoxy plastic package material product during compression molding.
The invention also provides a preparation method of the powdery epoxy molding compound with high dielectric constant, which at least comprises the following steps:
(1) Respectively pulverizing epoxy resin and curing agent with a resin pulverizer to obtain powder, packaging, and sealing at low temperature for use;
(2) Adding silicon dioxide, aluminum oxide, a coupling agent and an additive into a high-speed stirrer in batches for mixing, and then adding the epoxy resin and the curing agent which are crushed in the step (1) for mixing again to obtain a mixed material;
(3) And (3) mixing the mixed material in the step (2) by adopting a double-screw extruder, and cooling, crushing and screening to obtain a powdery epoxy plastic package material product.
Preferably, the fineness of the pulverization in the step (1) is less than 0.5mm;
preferably, the mixing and remixing time in the step (2) is 10-20 min;
preferably, the extrusion temperature of the twin-screw extruder in the step (3) is 90-120 DEG C
Preferably, the powder epoxy molding compound product in the step (4) is obtained with the particle size of 0.5-2.0 mm.
According to the invention, the powder epoxy molding compound product with the particle size of 0.5-2.0 mm is prepared by optimizing the preparation process, and the requirement of the compression molding process can be met.
Advantageous effects
1. The invention provides a high-dielectric-constant powdery epoxy plastic packaging material, which is combined with a packaging and testing factory to carry out plastic packaging by adopting a compression molding method, and can comprehensively improve the chip performance from the aspects of performance (high dielectric constant) and product structure (thin plastic packaging thickness).
2. Based on the system, the high-density polyethylene oxidized wax is introduced as a release agent, so that the plastic package material product provided by the invention has excellent metal stripping property, the processing difficulty is reduced, and meanwhile, the high-density polyethylene oxidized wax and the coupling agent in the system act together to realize good dispersion of silicon dioxide and high-dielectric constant filler in the system, and the spiral flow length of the product prepared is ensured to be at a proper level.
3. Based on the system, the epoxy silane coupling agent, especially KH-560 is introduced, so that the combination of silicon dioxide, aluminum oxide and resin in the system is realized, and meanwhile, the high-density polyethylene oxidized wax in the system is matched, so that the fluidity of a plastic package product is effectively improved, and the use requirement of thin package is met.
4. Based on the system, the problem of spiral flow length reduction of the plastic package material due to excessive high molecular weight of the resin and excessive increase of molecular chain length is avoided on the premise of ensuring that the basic performance of the plastic package material meets the requirement by adopting the combined action of bisphenol A type epoxy resin, multifunctional epoxy resin, linear phenolic resin and multifunctional phenolic resin combined curing agent.
5. The inventor ensures that the spiral flow length of the plastic package material is more than 55 inches while the provided product has a dielectric constant higher than 7 and low dielectric loss under the combined action of various raw materials in a system by matching and introducing part of silicon dioxide with the maximum particle diameter of 20 mu m, and avoids the damage to the internal structure of the product caused by the overhigh viscosity of the powdered epoxy plastic package material during compression molding.
Detailed Description
Example 1
In one aspect, embodiment 1 of the invention provides a high-dielectric-constant powdery epoxy molding compound, which is prepared from, by weight, 5 parts of epoxy resin, 3 parts of a curing agent, 0.3 part of a silane coupling agent, 0.5 part of an additive and 92 parts of a high-dielectric-constant filler.
The additive is a release agent; the release agent is high-density polyethylene oxidized wax (Honeywell AC 316A);
the silane coupling agent is an epoxy silane coupling agent; the epoxy silane coupling agent is 3- (2, 3-glycidoxy) propyl trimethoxy silane (KH-560).
The epoxy resin is a combination of bisphenol A epoxy resin and multifunctional epoxy resin; the mass ratio of the bisphenol A type epoxy resin to the multifunctional epoxy resin is 1:4.
the epoxy equivalent of the bisphenol A type epoxy resin is 176-184g/eq.
The epoxy equivalent of the multifunctional epoxy resin is 165-174g/eq.
The types of the bisphenol A type epoxy resin and the multifunctional epoxy resin are NPEL-127 (Nanya) and 1032H60 (Mitsubishi chemical).
The curing agent is a combination of linear phenolic resin and multifunctional phenolic resin; the mass ratio of the linear phenolic resin to the multifunctional phenolic resin is 2:1.
the model of the linear phenolic resin is PF-8011 (Shandong holy spring); the model of the multifunctional phenolic resin is MEH-7500 (Ming He Chemicals).
The high dielectric constant filler is aluminum oxide; the maximum particle size of the aluminum oxide is 25 μm (NA 1045W of Jiangsu-associated rayl).
The embodiment 1 of the invention provides a preparation method of a high-dielectric-constant powdery epoxy molding compound, which comprises the following steps:
(1) Respectively pulverizing epoxy resin and curing agent with a resin pulverizer to obtain powder, packaging, and sealing at low temperature for use;
(2) Adding aluminum oxide, a coupling agent and an additive into a high-speed stirrer in batches for mixing, and then adding the epoxy resin and the curing agent which are crushed in the step (1) for mixing again to obtain a mixed material;
(3) And (3) mixing the mixed material in the step (2) by adopting a double-screw extruder, and cooling, crushing and screening to obtain a powdery epoxy plastic package material product.
The fineness of the crushing in the step (1) is 0.3mm;
the mixing and remixing time in the step (2) is 20min;
the extrusion temperature of the twin-screw extruder in the step (3) is 100 DEG C
The powder epoxy plastic package material product in the step (4) is obtained with the grain diameter of 0.5-2.0 mm.
Example 2
In one aspect, the embodiment 2 of the invention provides a high-dielectric-constant powdery epoxy molding compound, which is prepared from 5 parts by weight of epoxy resin, 3 parts by weight of curing agent, 0.3 part by weight of silane coupling agent, 0.5 part by weight of additive, 7 parts by weight of silicon dioxide and 85 parts by weight of high-dielectric-constant filler.
The additive is a release agent; the release agent is high-density polyethylene oxidized wax (Honeywell AC 316A);
the silane coupling agent is an epoxy silane coupling agent; the epoxy silane coupling agent is 3- (2, 3-glycidoxy) propyl trimethoxy silane (KH-560).
The epoxy resin is a combination of bisphenol A epoxy resin and multifunctional epoxy resin; the mass ratio of the bisphenol A type epoxy resin to the multifunctional epoxy resin is 1:4.
the epoxy equivalent of the bisphenol A type epoxy resin is 176-184g/eq.
The epoxy equivalent of the multifunctional epoxy resin is 165-174g/eq.
The types of the bisphenol A type epoxy resin and the multifunctional epoxy resin are NPEL-127 (Nanya) and 1032H60 (Mitsubishi chemical).
The curing agent is a combination of linear phenolic resin and multifunctional phenolic resin; the mass ratio of the linear phenolic resin to the multifunctional phenolic resin is 2:1.
the model of the linear phenolic resin is PF-8011 (Shandong holy spring); the model of the multifunctional phenolic resin is MEH-7500 (Ming He Chemicals).
The maximum particle size of the silica was 20. Mu.m (SO-C4 of Admatechs, japan).
The high dielectric constant filler is aluminum oxide; the maximum particle size of the aluminum oxide is 25 μm (NA 1045W of Jiangsu-associated rayl).
The embodiment 2 of the invention provides a preparation method of a high-dielectric-constant powdery epoxy molding compound, which comprises the following steps:
(1) Respectively pulverizing epoxy resin and curing agent with a resin pulverizer to obtain powder, packaging, and sealing at low temperature for use;
(2) Adding silicon dioxide, aluminum oxide, a coupling agent and an additive into a high-speed stirrer in batches for mixing, and then adding the epoxy resin and the curing agent which are crushed in the step (1) for mixing again to obtain a mixed material;
(3) And (3) mixing the mixed material in the step (2) by adopting a double-screw extruder, and cooling, crushing and screening to obtain a powdery epoxy plastic package material product.
The fineness of the crushing in the step (1) is 0.3mm;
the mixing and remixing time in the step (2) is 20min;
the extrusion temperature of the twin-screw extruder in the step (3) is 100 DEG C
The powder epoxy plastic package material product in the step (4) is obtained with the grain diameter of 0.5-2.0 mm.
Example 3
The embodiment 3 of the invention provides a high-dielectric-constant powdery epoxy molding compound, which is prepared from 5 parts by weight of epoxy resin, 3 parts by weight of curing agent, 0.3 part by weight of silane coupling agent, 0.5 part by weight of additive, 47 parts by weight of silicon dioxide and 45 parts by weight of high-dielectric-constant filler.
The additive is a release agent; the release agent is high-density polyethylene oxidized wax (Honeywell AC 316A);
the silane coupling agent is an epoxy silane coupling agent; the epoxy silane coupling agent is 3- (2, 3-glycidoxy) propyl trimethoxy silane (KH-560).
The epoxy resin is a combination of bisphenol A epoxy resin and multifunctional epoxy resin; the mass ratio of the bisphenol A type epoxy resin to the multifunctional epoxy resin is 1:4.
the epoxy equivalent of the bisphenol A type epoxy resin is 176-184g/eq.
The epoxy equivalent of the multifunctional epoxy resin is 165-174g/eq.
The types of the bisphenol A type epoxy resin and the multifunctional epoxy resin are NPEL-127 (Nanya) and 1032H60 (Mitsubishi chemical).
The curing agent is a combination of linear phenolic resin and multifunctional phenolic resin; the mass ratio of the linear phenolic resin to the multifunctional phenolic resin is 2:1.
the model of the linear phenolic resin is PF-8011 (Shandong holy spring); the model of the multifunctional phenolic resin is MEH-7500 (Ming He Chemicals).
The maximum particle size of the silica was 20. Mu.m (SO-C4 of Admatechs, japan).
The high dielectric constant filler is aluminum oxide; the maximum particle size of the aluminum oxide is 25 μm (NA 1045W of Jiangsu-associated rayl).
In another aspect, embodiment 3 of the present invention provides a method for preparing a high dielectric constant powdered epoxy molding compound, which includes the following steps:
(1) Respectively pulverizing epoxy resin and curing agent with a resin pulverizer to obtain powder, packaging, and sealing at low temperature for use;
(2) Adding silicon dioxide, aluminum oxide, a coupling agent and an additive into a high-speed stirrer in batches for mixing, and then adding the epoxy resin and the curing agent which are crushed in the step (1) for mixing again to obtain a mixed material;
(3) And (3) mixing the mixed material in the step (2) by adopting a double-screw extruder, and cooling, crushing and screening to obtain a powdery epoxy plastic package material product.
The fineness of the crushing in the step (1) is 0.3mm;
the mixing and remixing time in the step (2) is 20min;
the extrusion temperature of the twin-screw extruder in the step (3) is 100 DEG C
The powder epoxy plastic package material product in the step (4) is obtained with the grain diameter of 0.5-2.0 mm.
Example 4
The embodiment 4 of the invention provides a high-dielectric-constant powdery epoxy molding compound, which is prepared from 5 parts by weight of epoxy resin, 3 parts by weight of curing agent, 0.3 part by weight of silane coupling agent, 0.5 part by weight of additive, 77 parts by weight of silicon dioxide and 85 parts by weight of high-dielectric-constant filler.
The additive is a release agent; the release agent is high-density polyethylene oxidized wax (Honeywell AC 316A);
the silane coupling agent is an epoxy silane coupling agent; the epoxy silane coupling agent is 3- (2, 3-glycidoxy) propyl trimethoxy silane (KH-560).
The epoxy resin is a combination of bisphenol A epoxy resin and multifunctional epoxy resin; the mass ratio of the bisphenol A type epoxy resin to the multifunctional epoxy resin is 4:1.
the epoxy equivalent of the bisphenol A type epoxy resin is 176-184g/eq.
The epoxy equivalent of the multifunctional epoxy resin is 165-174g/eq.
The types of the bisphenol A type epoxy resin and the multifunctional epoxy resin are NPEL-127 (Nanya) and 1032H60 (Mitsubishi chemical).
The curing agent is a combination of linear phenolic resin and multifunctional phenolic resin; the mass ratio of the linear phenolic resin to the multifunctional phenolic resin is 2:1.
the model of the linear phenolic resin is PF-8011 (Shandong holy spring); the model of the multifunctional phenolic resin is MEH-7500 (Ming He Chemicals).
The maximum particle size of the silica was 20. Mu.m (SO-C4 of Admatechs, japan).
The high dielectric constant filler is aluminum oxide; the maximum particle size of the aluminum oxide is 25 μm (NA 1045W of Jiangsu-associated rayl).
The embodiment 4 of the invention provides a preparation method of a high-dielectric-constant powdery epoxy molding compound, which comprises the following steps:
(1) Respectively pulverizing epoxy resin and curing agent with a resin pulverizer to obtain powder, packaging, and sealing at low temperature for use;
(2) Adding silicon dioxide, aluminum oxide, a coupling agent and an additive into a high-speed stirrer in batches for mixing, and then adding the epoxy resin and the curing agent which are crushed in the step (1) for mixing again to obtain a mixed material;
(3) And (3) mixing the mixed material in the step (2) by adopting a double-screw extruder, and cooling, crushing and screening to obtain a powdery epoxy plastic package material product.
The fineness of the crushing in the step (1) is 0.3mm;
the mixing and remixing time in the step (2) is 20min;
the extrusion temperature of the twin-screw extruder in the step (3) is 100 DEG C
The powder epoxy plastic package material product in the step (4) is obtained with the grain diameter of 0.5-2.0 mm.
Performance test method
1. Referring to GB/T33316-2016, the curing time of the powdered epoxy molding compound of the examples is tested and the test results are shown in Table 1.
2. Referring to ASTM D3123-09, the helical flow length of the example powdered epoxy molding compound is tested and the test results are shown in table 1.
3. Referring to GB/T22567-2008, the glass transition temperatures of the powdered epoxy molding compounds of the examples were tested, and the test results are shown in Table 1.
4. With reference to ASTM 790D-17, the flexural modulus and flexural strength of the example powdered epoxy molding compounds were tested, and the test results are shown in Table 1.
5. Injection pressure at a molding temperature of 175 degrees: the epoxy resin composition was charged into a molding cylinder under 6.86MPa (70 kgf/cm 2), compression molded into a cylinder having a diameter of 5mm and a height of 5mm, and after curing at 175 degrees for 6 hours, the thermal expansion coefficient 1 (temperature interval: 40 to 80 deg-c) and the thermal expansion coefficient 2 (200 to 240 deg-c) were measured using a PerkingElmer TMA4000, and the measurement results are shown in Table 1.
6. Referring to GB/T40564-2021, the molding shrinkage of the powdered epoxy molding compound of the example is tested, and the test results are shown in Table 1.
7. Referring to GB/T3139-2005, the thermal conductivity of the powdered epoxy molding compound of the example was tested, and the test results are shown in Table 1.
8. Injection pressure at molding temperature of 175 ℃): 6.86MPa (70 kgf/cm) 2 ) The epoxy resin composition was put into an injection molding cylinder, compression molded into a sample block having a diameter of 50mm and a thickness of 3mm, and after curing at 175℃for 6 hours, dielectric constant and dielectric loss were measured using a QBG-3E full-digital high-frequency Q meter of Shanghai Seiki electronic equipment Co., ltd, and the results are recorded in Table 1.
TABLE 1,
Claims (10)
1. The high-dielectric-constant powdery epoxy molding compound is characterized by comprising the following preparation raw materials in parts by weight: 3-8 parts of epoxy resin, 2-5 parts of curing agent, 0.2-0.5 part of silane coupling agent, 0.1-1 part of additive, 0-30 parts of silicon dioxide and 50-92 parts of high dielectric constant filler.
2. The high dielectric constant powdered epoxy molding compound of claim 1, wherein the additive is at least one of a mold release agent, an ion scavenger, a colorant, a bonding agent, and a low stress agent.
3. The high dielectric constant powder epoxy molding compound according to claim 1 or 2, wherein the silane coupling agent is an epoxy silane coupling agent.
4. The high dielectric constant powder epoxy molding compound according to claim 3, wherein the epoxy resin is at least one of a polyaromatic epoxy resin, a polyfunctional epoxy resin, a bisphenol a epoxy resin, and a phenol biphenyl epoxy resin.
5. The high dielectric constant powdered epoxy molding compound of claim 4, wherein the epoxy resin is a combination of bisphenol a type epoxy resin and multifunctional epoxy resin; the mass ratio of the bisphenol A type epoxy resin to the multifunctional epoxy resin is (1-4): (4-1).
6. The high dielectric constant powder epoxy molding compound according to claim 5, wherein the bisphenol a type epoxy resin has an epoxy equivalent of 176-184g/eq; the epoxy equivalent of the multifunctional epoxy resin is 165-174g/eq.
7. A high dielectric constant powdered epoxy molding compound according to claim 3, wherein said curing agent is a combination of a phenolic novolac resin and a multifunctional phenolic resin; the mass ratio of the linear phenolic resin to the multifunctional phenolic resin is (1-3): (1-2).
8. A high dielectric constant powdered epoxy molding compound according to claim 3, wherein said high dielectric constant filler is at least one selected from the group consisting of aluminum oxide, barium titanate, calcium titanate, and strontium titanate.
9. The high-dielectric-constant powdery epoxy molding compound according to claim 8, wherein the mass ratio of the silicon dioxide to the high-dielectric-constant filler is (5-10): (82-87).
10. A method for preparing a high dielectric constant powdered epoxy molding compound according to any one of claims 1-9, comprising at least the steps of:
(1) Respectively pulverizing epoxy resin and curing agent with a resin pulverizer to obtain powder, packaging, and sealing at low temperature for use;
(2) Adding silicon dioxide, aluminum oxide, a coupling agent and an additive into a high-speed stirrer in batches for mixing, and then adding the epoxy resin and the curing agent which are crushed in the step (1) for mixing again to obtain a mixed material;
(3) And (3) mixing the mixed material in the step (2) by adopting a double-screw extruder, and cooling, crushing and screening to obtain a powdery epoxy plastic package material product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109517336A (en) * | 2018-10-31 | 2019-03-26 | 科化新材料泰州有限公司 | A kind of super heat-resisting, high thermal conductivity epoxy-plastic packaging material preparation method of semiconductor-sealing-purpose |
| CN111073217A (en) * | 2019-12-23 | 2020-04-28 | 科化新材料泰州有限公司 | High-thermal-conductivity low-stress epoxy plastic packaging material for semiconductor packaging |
| CN112538236A (en) * | 2020-12-10 | 2021-03-23 | 深圳先进电子材料国际创新研究院 | Epoxy plastic packaging material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109517336A (en) * | 2018-10-31 | 2019-03-26 | 科化新材料泰州有限公司 | A kind of super heat-resisting, high thermal conductivity epoxy-plastic packaging material preparation method of semiconductor-sealing-purpose |
| CN111073217A (en) * | 2019-12-23 | 2020-04-28 | 科化新材料泰州有限公司 | High-thermal-conductivity low-stress epoxy plastic packaging material for semiconductor packaging |
| CN112538236A (en) * | 2020-12-10 | 2021-03-23 | 深圳先进电子材料国际创新研究院 | Epoxy plastic packaging material and preparation method and application thereof |
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