CN105462173A - Environment-friendly epoxy resin composition and preparation method thereof - Google Patents
Environment-friendly epoxy resin composition and preparation method thereof Download PDFInfo
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- CN105462173A CN105462173A CN201510994440.8A CN201510994440A CN105462173A CN 105462173 A CN105462173 A CN 105462173A CN 201510994440 A CN201510994440 A CN 201510994440A CN 105462173 A CN105462173 A CN 105462173A
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with 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
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- 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
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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- 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)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention provides an environment-friendly epoxy resin composition which comprises the following components in percentage by weight: 4-6wt% of epoxy resin, 3.5-6wt% of phenolic resin, 85-89wt% of inorganic filler and 0.1-1wt% of a curing promoter, as well as one or more of a flame retardant, a releasing agent, an inorganic ion capturing agent, a silane coupling agent, a coloring agent and a low-stress modifying agent. The environment-friendly epoxy resin composition is a semiconductor packaging material with good storage property and curing property, and simultaneously has essential flowability, high reliability, flame retardance, and warping resistance. The improved resin composition can meet the QFN packaging requirement.
Description
Technical field
The present invention relates to a kind of environment-friendly epoxy resin combination and preparation method thereof, particularly one and there is high workability, building-up properties well, good preservation performance, be applicable to the environment-friendly epoxy resin combination of QFN encapsulation.
Background technology
Along with the fast development of semicon industry, the structure of Electronic Packaging also has the packing forms of early stage through hole installation, as double-row type encapsulation (DIP), single-column type encapsulation (SIP/SIP) and pin grid array package (PGA) etc., develop into four limits lead-in wire flat package (QFP) of surface-adhered type, little outline packages (SOP/SOJ), thin small outline packages (TSOP), without lead-in wire chip carrier (LCC), quad flat non-pin package (QFN), BGA Package (BGA) etc. and more senior directly bonded direct chip attachment (COB), belt carrier tape package (TCP) etc., and with Chip Size Package, the novel encapsulated technique of 3-D stacks encapsulation and the encapsulation of total silicon wafer type also just progressively enters into market.
Wherein, QFN is a kind of without pin package, and in square or rectangle, package bottom middle position has a big area exposed pads to be used for heat conduction, and the encapsulation periphery around large bonding pad has the conductive welding disk realizing electrical connection.Because QFN encapsulation has gull wing lead-in wire unlike traditional SOP and TSOP encapsulates, the conductive path between inner pin and pad is short, and in coefficient of self-induction and package, routing resistance is very low, so it can provide the electrical property of brilliance.In addition, it also provides outstanding heat dispersion by the leadframe pad exposed.Because volume is little, lightweight, add outstanding electrical property and thermal characteristics, this encapsulation is particularly suitable for any one application to the requirement that size, weight and performance have.As the main flow of middle and high-end market, under the condition that packaging process and market reach its maturity, competition is also day by day fierce, not only requires that epoxy molding plastic will meet the Reflow Soldering condition of 260 DEG C, use environmental protection fire retarding agent etc., low cost become participate in the competition requisite counterweight.Therefore the composition epoxy resin of developing low-cost, environmental protection high reliability is imperative.
In the middle of disclosed technology, silane coupling agent is adopted to carry out surface treatment to mineral filler and increase the content (for example, referring to Unexamined Patent 8-20673 publication) of mineral filler, low viscosity when can keep shaping and high workability.But the conventional silanes coupling agent molecule amount used in the method is less, and bonding force between mineral filler is poor, does not have certain toughening effect, thus makes composition epoxy resin melt viscosity little not enough, therefore require further improvement technology.Disclose a kind of composition epoxy resin in Japanese Unexamined Patent Publication 2002-220515, amount of filler reaches 80%, and melting viscosity is higher, and Spiral flow length is lower.Building-up properties is bad, and there is pore on plastic cement packaging surface.In order to improve the soldering resistance of packaged material, amount of filler can reach 85-90%, and when using low viscous resin system, melt viscosity also can be very low, and Spiral flow length also can be accomplished very long.But use existing encapsulation system and curing catalyst, the curing speed of packaged material is comparatively slow, easily causes demoulding difficulty, affects the reliability of QFN packaging.Especially, in green encapsulation system situation, the general shelf lives is bad.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, a kind of composition epoxy resin for semiconductor packages and preparation method thereof is proposed, by adding new type curative accelerant, improve the solidified nature of resin combination, storage characteristics and flowing property, the requirement of QFN can be met.
Environment-friendly epoxy resin combination of the present invention, comprise epoxy resin, resol, filler and curing catalyst, also include one or more in fire retardant, releasing agent, inorganic ion scavenger, silane coupling agent, tinting material and low stress modified dose, described epoxy resin is 4 ~ 6wt% at the weight percentage of composition, described resol is 3.5 ~ 6wt% at the weight percentage of composition, and described mineral filler is 85 ~ 89wt% at the weight percentage of composition; Described curing catalyst is 0.1 ~ 1wt% at the weight percentage of composition;
In described curing catalyst, total content containing the mixture of the compound of structure shown in formula (1) and formula (2) accounts for more than 50% of curing catalyst gross weight, the mol ratio of formula (1) and (2) compound is 2:1, remaining curing catalyst is selected from one or more in imidazolium compounds, tertiary amine compound and organic phosphine compound
Described imidazolium compounds is selected from one or more in glyoxal ethyline, 2,4-methylimidazoles, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole and 2-(heptadecyl) imidazoles etc.
Described tertiary amine compound is selected from triethylamine Bian Ji dimethylamine, Alpha-Methyl Bian Ji dimethylamine, 2-(dimethylamino methyl) phenol, 2,4,6-tri-(dimethylamino methyl) phenol and 1,8-diazabicyclo (5,4,0) one or more in undecylene-7 grade.
Described organic phosphine compound is selected from one or more in triphenylphosphine, trimethyl-phosphine, triethyl phosphine, tributylphosphine, three (p-methylphenyl) phosphines and three (nonyl phenyl) phosphine etc.
Described epoxy resin be selected from the epoxy resin shown in following formula (3) and formula (4) one or both:
Above-mentioned various in, n is any one integer in 1-5.
Described resol be selected from the resol shown in following formula (5) and formula (6) one or both:
Above-mentioned various in, n is any one integer in 1-5.
The weight percentage of described fire retardant in composition epoxy resin is 0-3.1wt%; Of the present invention to comprise in environment-friendly epoxy resin combination use the fire retardant of not brominated antimony, available metal oxyhydroxide, water and metallic compound, metal oxide, molybdate, borate, phosphoric acid salt, containing phosphine compound nitrogenous compound, these compounds can be used alone or two or more used in combination.
The weight percentage of described releasing agent in composition epoxy resin is 0.01 ~ 1wt%; Be selected from one or more in carnauba wax, synthetic wax and mineral substance wax.
The weight percentage of described inorganic ion scavenger in composition epoxy resin is 0.05 ~ 0.5wt%; Include but not limited to be selected from hydrated metal oxide (as Bi
2o
33H2O), acid metal salt (as: Zr (HPO
4) 2H2O) and the compound (as: Mg6Al of magnalium
2(CO
3) (OH) 164H2O) and in one or more.
The weight percentage of described silane coupling agent in composition epoxy resin is 0.3 ~ 1wt%; Be selected from one or more in γ-epoxypropyl propyl ether Trimethoxy silane, γ aminopropyltriethoxy silane, γ mercaptopropyitrimethoxy silane and γ-aminopropyltrimethoxysilane.
The weight percentage of described tinting material in composition epoxy resin is 0.2 ~ 0.8wt%; As carbon black.
The described low stress modified dose weight percentage in composition epoxy resin is 0.1 ~ 2wt%; As liquid silicone oil, silicone rubber powder or their mixture etc.
Preferably,
The weight percentage of described releasing agent in composition epoxy resin is 0.5wt%;
The weight percentage of described inorganic ion scavenger in composition epoxy resin is 0.4wt%;
The weight percentage of described silane coupling agent in composition epoxy resin is 0.5wt%;
The weight percentage of described tinting material in composition epoxy resin is 0.5wt%;
The described low stress modified dose weight percentage in composition epoxy resin is 1wt%.
Described filler is preparing spherical SiO 2 powder filler, and its surface uses silane coupling agent to carry out surface treatment.
Described filler is preparing spherical SiO 2 powder filler, and its meso-position radius D50 is 10 ~ 30 microns.
The preparation method comprising environment-friendly epoxy resin combination of the present invention: by epoxy resin, resol, preparing spherical SiO 2 powder filler and curing catalyst, as other composition mixed with mentioned component when comprising other composition simultaneously, then be that on two roll mills of 70 ~ 100 DEG C, melting mixing is even in temperature, the material mixed is taken off naturally cooling from two roll mills, pulverize and obtain the described powder-material comprising environment-friendly epoxy resin combination; Be pre-formed as biscuit further, obtain the formed material comprising environment-friendly epoxy resin combination.
After the present invention adopts above-mentioned composition and preparation method, its beneficial effect is: the environment-friendly epoxy resin combination that comprises of the present invention is the semiconductor-sealing-purpose material that a kind of storage characteristics and solidified nature are excellent, and said composition has also possessed necessary mobility, high reliability, flame retardant resistance, resistance to warpage simultaneously.Improve the requirement that resin combination can meet QFN encapsulation.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but this is only citing, is not limitation of the present invention.
The each composition related in the present invention and code name as follows:
A1: epoxy resin (Japanese chemical drug system " NC3000P ")
A2: epoxy resin (Mitsubishi chemistry system " YX-4000H ")
B1: biphenyl phenol linear phenolic resin (Japan is bright and change into system " MEH7851SS ")
B2: phenol alkyl phenolic resin (Japan is bright and change into system " MEH7800SS ")
C1: curing catalyst KM-188 (Japanese Cao Da Inc.) is the mixture of the compound of structure shown in formula (1) and formula (2);
C2: curing catalyst TPP-BQ (mixture of triphenylphosphine and Resorcinol)
C3: curing catalyst 2-phenyl-4-methylimidazole (Japanese four countries change into system)
C4: curing catalyst 2-ethyl-4 Methylimidazole (Japanese four countries change into system)
D: preparing spherical SiO 2 micro mist (connection auspicious DQ1150B, d50 processed are 18 μm in Jiangsu, maximum particle diameter 75 microns)
Fire retardant: magnesium hydroxide powder, D50=1 micron
Inorganic ion scavenger: Mg
6al
2(CO
3) (OH) 164H2O
Embodiment 1-10
In embodiment 1-10, material composition, proportioning, preparation process, process parameter and evaluation result are as shown in table 1:
Table 1: the composition of embodiment 1-10 composition and evaluation result (by weight percentage)
The preparation method of embodiment 1-10 composition is as follows:
To weigh according to said ratio and after mixing, in temperature be again 70 ~ 100 DEG C of preheatings two roll mills on melting mixing even, the material mixed is taken off naturally cooling from two roll mills, pulverizes to obtain powder-material, be pre-formed as biscuit, obtain and comprise high thermal conductance environment-friendly epoxy resin combination formed material.
The evaluation method of embodiment 1-10 composition is as follows, and evaluation result is in table 1.
Gel time: hot plate method, is heated to 175 ± 1 DEG C by hot plate, get 0.3-0.5g sample powder and be placed on hot plate, is terminal when powder becomes colloidal state by fluid gradually, reads required time.
Spiral flow length: on transfer mould press by EMMI-1-66 helicoidal flow metal die measure, forming pressure be 70 ± 2Kgf/cm2 die temperature at 175 ± 2 DEG C, sample thief 20 ± 5g tests.
Melt viscosity: utilize the height Flow Meter of Japanese Shimadzu Corporation to measure the melt viscosity of described epoxy composite.
Storage characteristics: during storing temp 25 DEG C, Spiral flow length reduces to initial value 80% required time.
Flame retardant resistance: sample block sample being made under 175 DEG C/25Mpa condition 1/16 inch thickness, then carries out after fixing under the condition of 175 DEG C/6h, finally carries out flame retardant test with vertical combustion by GB4609-84.
Warpage: encapsulated on the silver-plated framework of QFN4*4mm respectively by sample, to after fixing at packaged sample 175 DEG C 6 hours after the demoulding.Use ShadowMorrie equipment to carry out warpage test, during test, plastic-sealed body faces up, and test value is timing be warpage is smiling face, test value for warpage time negative be face of crying.
Reliability (high temperature resistant Reflow Soldering, wet fastness): encapsulate the silver-plated framework of QFN4*4 at 175 DEG C, after the demoulding, packaged sample after fixing 6 hours at 175 DEG C, carries out MSL1 rank by JESD22-A113D requirement and examines respectively.Ultrasound scanning unit is used to carry out absciss layer scanning afterwards.Layering is fewer, and reliability is better.
Reference examples 1-3
In reference examples 1-3, material composition, proportioning, preparation process, process parameter and evaluation result are as shown in table 2, and preparation method is with embodiment 1, and evaluation method is with embodiment 1, and evaluation result is in table 2.
Table 2: the composition of comparative example composition and evaluation result (by weight percentage)
Can be found out by above-described embodiment and comparative example, comprise the storge quality of the composition epoxy resin of novel promotor, resistance to warpage performance silk performance, soldering resistance aspect be obviously better than not containing the performance of the composition epoxy resin of this promotor.
Claims (10)
1. an environment-friendly epoxy resin combination, it is characterized in that, comprise epoxy resin, resol, filler and curing catalyst, also include one or more in fire retardant, releasing agent, inorganic ion scavenger, silane coupling agent, tinting material and low stress modified dose, described epoxy resin is 4 ~ 6wt% at the weight percentage of composition, described resol is 3.5 ~ 6wt% at the weight percentage of composition, and described mineral filler is 85 ~ 89wt% at the weight percentage of composition; Described curing catalyst is 0.1 ~ 1wt% at the weight percentage of composition;
In described curing catalyst, total content containing the mixture of the compound of structure shown in formula (1) and formula (2) accounts for more than 50% of curing catalyst gross weight, the mol ratio of formula (1) and (2) compound is 2:1, remaining curing catalyst is selected from one or more in imidazolium compounds, tertiary amine compound and organic phosphine compound
2. environment-friendly epoxy resin combination according to claim 1, it is characterized in that, described imidazolium compounds is selected from one or more in glyoxal ethyline, 2,4-methylimidazoles, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole and 2-(heptadecyl) imidazoles etc.
Described tertiary amine compound is selected from triethylamine Bian Ji dimethylamine, Alpha-Methyl Bian Ji dimethylamine, 2-(dimethylamino methyl) phenol, 2,4,6-tri-(dimethylamino methyl) phenol and 1,8-diazabicyclo (5,4,0) one or more in undecylene-7 grade.
Described organic phosphine compound is selected from one or more in triphenylphosphine, trimethyl-phosphine, triethyl phosphine, tributylphosphine, three (p-methylphenyl) phosphines and three (nonyl phenyl) phosphine etc.
3. environment-friendly epoxy resin combination according to claim 1, is characterized in that, described epoxy resin be selected from the epoxy resin shown in following formula (3) and formula (4) one or both:
Above-mentioned various in, n is any one integer in 1-5.
4. environment-friendly epoxy resin combination according to claim 1, is characterized in that, described resol be selected from the resol shown in following formula (5) and formula (6) one or both:
Above-mentioned various in, n is any one integer in 1-5.
5. environment-friendly epoxy resin combination according to claim 1, is characterized in that,
The weight percentage of described fire retardant in composition epoxy resin is 0-3.1wt%; Described fire retardant be selected from metal hydroxides, water and metallic compound, metal oxide, molybdate, borate, phosphoric acid salt, containing one or more in phosphine compound nitrogenous compound;
The weight percentage of described releasing agent in composition epoxy resin is 0.01 ~ 1wt%; Be selected from one or more in carnauba wax, synthetic wax and mineral substance wax.
The weight percentage of described inorganic ion scavenger in composition epoxy resin is 0.05 ~ 0.5wt%; Be selected from one or more in the compound of hydrated metal oxide, acid metal salt and magnalium;
The weight percentage of described silane coupling agent in composition epoxy resin is 0.3 ~ 1wt%; Be selected from one or more in γ-epoxypropyl propyl ether Trimethoxy silane, γ aminopropyltriethoxy silane, γ mercaptopropyitrimethoxy silane and γ-aminopropyltrimethoxysilane;
The weight percentage of described tinting material in composition epoxy resin is 0.2 ~ 0.8wt%; Be selected from carbon black;
The described low stress modified dose weight percentage in composition epoxy resin is 0.1 ~ 2wt%; Be selected from liquid silicone oil, silicone rubber powder or their mixture.
6. environment-friendly epoxy resin combination according to claim 5, is characterized in that, described hydrated metal oxide is Bi2O33H2O; Described acid metal salt is Zr (HPO
4) 2H2O; The compound of described magnalium is Mg
6al
2(CO
3) (OH) 164H2O.
7. environment-friendly epoxy resin combination according to claim 5, is characterized in that,
The weight percentage of described releasing agent in composition epoxy resin is 0.5wt%;
The weight percentage of described inorganic ion scavenger in composition epoxy resin is 0.4wt%;
The weight percentage of described silane coupling agent in composition epoxy resin is 0.5wt%;
The weight percentage of described tinting material in composition epoxy resin is 0.5wt%;
The described low stress modified dose weight percentage in composition epoxy resin is 1wt%.
8. environment-friendly epoxy resin combination according to claim 1, is characterized in that, described filler is preparing spherical SiO 2 powder filler, and its surface uses silane coupling agent to carry out surface treatment.
9. environment-friendly epoxy resin combination according to claim 1, is characterized in that, described filler is preparing spherical SiO 2 powder filler, and its meso-position radius D50 is 10 ~ 30 microns.
10. the preparation method of the environment-friendly epoxy resin combination as described in claim 1-9, it is characterized in that, comprise the steps: epoxy resin, resol, preparing spherical SiO 2 powder filler and curing catalyst, as other composition mixed with mentioned component when comprising other composition simultaneously, then be that on two roll mills of 70 ~ 100 DEG C, melting mixing is even in temperature, the material mixed is taken off naturally cooling from two roll mills, pulverize and obtain the described powder-material comprising environment-friendly epoxy resin combination; Be pre-formed as biscuit further, obtain the formed material comprising environment-friendly epoxy resin combination.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108070212A (en) * | 2016-11-16 | 2018-05-25 | 北京科化新材料科技有限公司 | A kind of composition epoxy resin and its application |
| CN108070213A (en) * | 2016-11-16 | 2018-05-25 | 北京科化新材料科技有限公司 | A kind of composition epoxy resin and its application |
| CN114437511A (en) * | 2021-12-31 | 2022-05-06 | 江苏科化新材料科技有限公司 | Epoxy resin composition and application thereof, epoxy resin molding material and preparation method and application thereof |
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Application publication date: 20160406 |