CN113831878A - Epoxy resin composition and application thereof - Google Patents
Epoxy resin composition and application thereof Download PDFInfo
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- CN113831878A CN113831878A CN202111232864.2A CN202111232864A CN113831878A CN 113831878 A CN113831878 A CN 113831878A CN 202111232864 A CN202111232864 A CN 202111232864A CN 113831878 A CN113831878 A CN 113831878A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to an epoxy resin composition and application thereof. The epoxy resin composition comprises the following components in parts by weight: 2-15 parts of epoxy resin, 2-10 parts of a hardening agent, 0.01-1 part of a hardening accelerator, 70-95 parts of an inorganic filling material, 0.1-0.8 part of a coupling agent, 0.1-1.0 part of organic indene modified bentonite, 0.1-0.6 part of a release agent, 0.1-1 part of a stress modifier and 0.01-1 part of a coloring agent. The epoxy resin composition provided by the invention has the advantages that the effective control and good adherence to the pores of a large PAD product are realized, and the reliability and the electrical performance of the product are stable; in addition, the product has good processability. The epoxy resin composition of the present invention is suitable for discrete devices and integrated circuit packages.
Description
Technical Field
The invention relates to the field of discrete devices and integrated circuit packaging electronic packaging, in particular to an epoxy resin composition and application thereof.
Background
In recent years, epoxy molding compounds, which are polymer composite materials using epoxy resin as matrix resin, have advantages of low cost, thinness, simple production process, suitability for automatic production and the like, and are widely applied to packaging in the microelectronic industry, and become main packaging materials for consumer electronics and higher-density electronic packaging. With the increasing integration of electronic packaging, the chip size is also increasing, the internal wiring is also becoming denser, and the performance requirements for epoxy resin compositions are also becoming higher. For the plastic package body, the problems of appearance, productivity, wire punching, reliability and the like need to be considered.
For packaging discrete devices and integrated circuits, the adhesion fastness of the epoxy resin composition and a frame is ensured, the problems of operability during packaging, electrical property after water absorption and the like are also considered, and the influence on the reliability and the productivity of products due to water absorption and frame adhesion is avoided.
In the present stage, the customer packaging integrated circuit pursues simple packaging of low-cost and high-efficiency chips, for example, the size of the existing packaging form is enlarged and the more integrated circuit chip is enlarged, so that the requirements on the material frame, the silver colloid, the wire and the EMC (epoxy resin composition) of the packaging are all higher. The chip is large, the PAD loaded with the chip is larger, but the overall dimension is unchanged, so the volume ratio is changed, the overall dimension of the plastic packaging material is closer to the dimension ratio of the PAD, the general ratio is more than 80 percent, the condition can influence the mold flow of the plastic packaging material, the plastic packaging material enters the cavity and has two different flow paths of the PAD, because the pad is larger, the flowing speed of the epoxy resin composition on the upper and lower layers of the pad is different, the epoxy resin composition in the upper and lower layers of flowing paths is healed before exhausting, so that the gas in the cavity and the EMC body can not be exhausted, and air holes are remained on the surface or inside of the packaged product, further packaging plants are also increasing the number of single-mode and monolithic products from a cost and efficiency standpoint, for example, the SOP8 is changed from 5 rows to 8 rows to 12 rows, even more, the SOP8 is designed into 15 rows, so that the EMC flowability control requirement is higher. The flow channel is long and thin, the wire diameter is thin, therefore, the EMC viscosity is low, the reaction can not be too fast, but the solidification can not be too slow, but the low-viscosity plastic package material can easily cause reverse wrapping in the cavity, the air hole control is not easy, therefore, when designing the plastic package material, the EMC needs to flow fast under high pressure and the flow length is long enough, after the EMC enters the cavity, because the size of the glue opening is far smaller than the size of the flow channel and the cavity, the EMC is quickly changed from the high-pressure state to the low-pressure state, the flow rate of the material is slow at the moment, the low-pressure high-viscosity property is shown, the healing position of the material after flowing in the cavity is closer to the exhaust end of the cavity, and the material and the air in the cavity are easier to exhaust, so that the problem of no inner and outer air holes after the material is packaged is ensured.
The epoxy resin composition has more factors influencing the reliability, such as mechanical, thermal, electrical, radiation, chemical factors and the like, the mechanical factor is mainly influenced by the stress change of a product, the thermal influence is mainly caused by the temperature in a production process, the electrical influence is mainly caused by the problems of electric energy heat loss, electromigration and the like caused by performance abnormality in the using process, and the chemical influence is mainly caused by corrosion, oxidation, ion migration and the like caused by the environment; the epoxy resin composition absorbs moisture under a high-temperature and high-humidity environment, extracts partial substances which do not participate in the reaction, and forms byproducts which enter an interface between a metal base bonded with the chip and the plastic package material, wherein the performance of the device is degraded or even loses efficacy due to corrosion, oxidation and ion migration. The above failure modes can also cross over, such as thermal failure leading to mechanical failure, which exacerbates corrosion.
The organic bentonite is an inorganic mineral/organic ammonium compound, takes bentonite as a raw material, and is prepared by inserting an organic covering agent through an ion exchange technology by utilizing the lamellar structure of montmorillonite in the bentonite and the characteristic that the lamellar structure can be swelled and dispersed into colloidal clay in water or an organic solvent. The organic bentonite can form gel in various organic solvents, oils and liquid resins, has good thickening property, thixotropy, suspension stability, high-temperature stability, lubricity, film-forming property, water resistance and chemical stability, and has important application value in the paint industry. The method is also widely applied to industries such as paint ink, aviation, metallurgy, chemical fiber, petroleum and the like. However, if the bentonite is used directly, the properties of the epoxy resin composition are affected by the high content of bentonite ions, the basicity, the inactivation of terminal hydroxyl groups and the high water absorption.
Disclosure of Invention
The invention aims to overcome the defects of air holes, poor interface adhesion, poor reliability and the like of the conventional epoxy resin composition during large Pad packaging, and provides the epoxy resin composition suitable for large Pad packaging.
The inventor finds that the indene oligomer modified bentonite can give consideration to the characteristics of the bentonite, plays roles in low-pressure thickening and high-pressure thixotropic property, and solves the problems of high sodium ion content in the bentonite and passivation of hydroxyl groups at the indene oligomer terminal. The indene oligomer and the bentonite are connected in a hydrogen bond form in the organic indene modified bentonite, so that the decrease of adhesion force caused by the passivation of the terminal hydroxyl of the indene oligomer in the production process of the epoxy resin composition is avoided, the introduction of the indene oligomer enables the interface connection to have not only hydrogen bond acting force but also bonding force of polycondensation reaction in the packaging process, and the interface delamination caused by the decrease of the hydrogen bond acting force at high temperature is avoided, so that the introduction of the organic indene oligomer bentonite in the epoxy resin composition can effectively solve the problems of abnormal mold flow and interface adhesion.
An epoxy resin composition comprises, by mass, 2-15 parts of an epoxy resin, 2-10 parts of a curing agent, 0.01-1 part of a curing accelerator, 70-95 parts of an inorganic filling material, 0.1-0.8 part of a coupling agent, 0.1-1.0 part of organic indene modified bentonite, 0.1-0.6 part of a mold release agent, 0.1-1 part of a stress modifier and 0.01-1 part of a coloring agent.
The epoxy resin is one or a mixture of several of bisphenol epoxy resin, biphenyl epoxy resin, triphenol methane epoxy resin, naphthol epoxy resin, stilbene epoxy resin, epoxy resin containing a triazine core structure, novolac epoxy resin, modified novolac epoxy resin and dicyclopentadiene epoxy resin in any proportion.
The hardener is one or a mixture of several of novolac resin, cresol novolac resin, naphthalene type phenolic resin and cyclopentadiene type phenolic resin according to any proportion; the hardening accelerator is one or a mixture of several of amines and nitrogen-containing heterocyclic compounds according to any proportion.
The inorganic filling material is one or a mixture of two of silica micropowder and alumina in any proportion; the silicon micro powder and the alumina are spherical, and the maximum grain diameter of the silicon micro powder and the maximum grain diameter of the alumina are both less than 75 microns.
The coupling agent is a silane coupling agent; the release agent is one or a mixture of several of carnauba wax, montan wax and synthetic wax in any proportion.
The preparation method of the organic indene modified bentonite comprises the following steps,
adding organic bentonite and indene oligomer into n-heptane, stirring uniformly, adding a proper amount of silane coupling agent, stirring fully for 1-3 h, placing in a blowing box with the temperature of 80-90 ℃ after stirring is finished until the mixture is dried and agglomerated, crushing the prepared lumps, sieving and bagging for later use.
The indene oligomer has the following molecular formula structure:
r represents a hydrogen atom, a methyl group or an ethyl group; m is 5-10; n is 5-15; the molecular weight is 2000-3000;
the stress modifier is one or a mixture of several of nitrile rubber, ABS rubber copolymer and organic silicone oil in any proportion.
The application of the epoxy resin composition as an encapsulating material for packaging discrete devices and integrated circuits.
The invention has the advantages that: the epoxy resin composition adopts the organic indene modified bentonite, has good dispersion compatibility in the epoxy resin composition, improves the low-pressure and high-viscosity characteristics and the low-ion and high-interface cohesiveness of products, can solve the problems of internal and external air holes of packaged products and the cohesiveness of metal interfaces, and has the characteristics of good appearance and high reliability when being used as a packaging material for packaging discrete devices and integrated circuits.
Detailed Description
In order to enhance the understanding of the present invention, the present invention will be described in further detail with reference to the following examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
The first embodiment is as follows: the embodiment provides an epoxy resin composition which is prepared from 2-15 parts of epoxy resin, 2-10 parts of a curing agent, 0.01-1 part of a curing accelerator, 70-95 parts of an inorganic filling material, 0.1-0.8 part of a coupling agent, 0.1-1.0 part of organic indene modified bentonite, 0.1-0.6 part of a release agent, 0.1-1 part of a stress modifier and 0.01-1 part of a coloring agent in parts by weight.
The epoxy resin composition of the embodiment is prepared by the following steps: weighing the components, uniformly mixing the coupling agent and the filler, uniformly mixing the mixture with the epoxy resin, the hardening agent, the hardening accelerator, the release agent, the organic indene modified bentonite, the stress modifier and the coloring agent, mixing the mixture on a rubber mixing machine at the mixing temperature of 80-110 ℃ for 2-10 minutes, pulling sheets, cooling, crushing and forming cakes after uniform mixing.
In the epoxy resin composition of the present embodiment, the epoxy resin is subjected to ring opening of epoxy groups under the action of the curing accelerator at a high temperature and is subjected to a crosslinking reaction with phenolic hydroxyl groups in the curing agent to form a network structure; in the high-temperature reaction process, the wetting of the surface of the filler is increased, and the good dispersibility is shown.
According to the epoxy resin composition, the organic indene modifier bentonite is introduced, so that free Na ions can be removed, the problem of terminal hydroxyl passivation of indene oligomer can be solved, the low-pressure high-viscosity property can be solved, the poor electrical property caused by high ions is not influenced, and meanwhile, the insufficient adhesion of the epoxy resin composition due to the terminal hydroxyl passivation is improved, so that the internal and external pores of a customer packaging product are improved, and the reliability of the product is improved.
The second embodiment is as follows: the present embodiment is different from the specific embodiment in that: the epoxy resin is one or a mixture of more of bisphenol epoxy resin, biphenyl epoxy resin, triphenol methane epoxy resin, naphthol epoxy resin, stilbene epoxy resin, epoxy resin containing a triazine core structure, novolac epoxy resin, modified novolac epoxy resin and dicyclopentadiene epoxy resin in any proportion.
The third concrete implementation mode: the present embodiment is different from the specific embodiment in that: the hardener is one or a mixture of several of novolac resin, cresol novolac resin, naphthalene type phenolic resin and cyclopentadiene type phenolic resin according to any proportion; the hardening accelerator is one or a mixture of several of amines, imidazole compounds and nitrogen-containing heterocyclic compounds according to any proportion.
The fourth concrete implementation mode: the present embodiment is different from the specific embodiment in that: the inorganic filling material is one or a mixture of two of silica micropowder and alumina in any proportion; the silicon micro powder and the alumina are spherical, and the maximum grain diameter of the silicon micro powder and the maximum grain diameter of the alumina are both less than 75 microns.
The fifth concrete implementation mode: the present embodiment is different from the specific embodiment in that: the coupling agent is a silane coupling agent; the release agent is one or a mixture of several of carnauba wax, montan wax and synthetic wax in any proportion.
The sixth specific implementation mode: the present embodiment is different from the specific embodiment in that: the organic indene modified bentonite is prepared by the following method:
putting the organic bentonite and the indene oligomer into n-heptane, stirring uniformly, adding a proper amount of silane coupling agent, stirring fully for 1-3 h, putting in a blower box with the temperature of 80-90 ℃ after stirring till drying and caking, crushing the prepared blocky materials, sieving, and bagging for later use.
The indene oligomer has the following molecular formula structure:
r represents a hydrogen atom, a methyl group or an ethyl group; m is 5-10; n is 5-15; the molecular weight is 2000-3000;
in the embodiment, the organic indene modified bentonite is adopted to improve the high viscosity characteristic of the product at low pressure and the low ion high interface cohesiveness, and simultaneously, the problems of internal and external air holes of the packaged product and the cohesiveness of a metal interface can be solved.
The seventh embodiment: the present embodiment is different from the specific embodiment in that: the stress modifier is one or a mixture of several of nitrile rubber, ABS rubber copolymer and organic silicone oil in any proportion.
The specific implementation mode is eight: the embodiment provides an application of the epoxy resin composition: the epoxy resin composition is used as an encapsulating material for discrete devices and integrated circuit packages.
The following examples were used to demonstrate the beneficial effects of the present invention:
this example provides an epoxy resin composition, which can be used to test the performance difference of products by adding different amounts.
The evaluation methods of the examples are as follows:
and (3) viscosity testing: taking a proper amount of epoxy resin composition powder to perform into a cylinder with the diameter of 10 +/-0.3 mm, and testing by adopting a high-change rheometer.
Adhesion force: cylindrical black paste (bottom surface diameter 3.5mm x height 5mm) was prepared by transfer molding, bonded to Ag/Cu/Ni plated metal sheets (6.5mm x 6.5mm), and tested by a crystal pusher while heated to 75 degrees.
Air holes: adopting an SOP8 five-row frame die, making epoxy resin composition powder into 43 x 50g cake materials, preheating, putting into a heated die, performing injection molding through a punch, cooling after curing, taking out, and observing inner and outer air holes and layering through a microscope and a scanner.
Disc flow: taking 8-10 g of epoxy resin composition powder, vertically pouring the epoxy resin composition powder on a heating platform, directly pressing the epoxy resin composition powder on a conical powder through a 5-10 kg flat plate, taking down the flat plate after curing, and testing the diameter of the cured epoxy resin composition cake by using a ruler.
The evaluation results are shown in Table 1.
The component codes referred to in table 1 of this example are illustrated below:
epoxy resin E: polyaromatic epoxy HP5000, available from Japan DIC
Hardening agent P: phenol formaldehyde type phenolic resin TD-2090 available from DIC of Japan
Inorganic filler S: silica micropowder SS-0183R, available from Korea KOSEM
Hardening accelerator C1: triphenylphosphine
Coupling agent C2: silane coupling agent KH560
The organic indene modified bentonite F is prepared from organic bentonite (GEL-1) and indene oligomer (IP100 Nissie iron)
Organic bentonite H organic bentonite GEL-1
Release agent W: carnauba No.1, available from Doya chemical company
Carbon black C3: MA-600, available from Mitsubishi, Japan.
Examples 1 to 4, the method steps of the above-mentioned embodiments one to eight were used to introduce the substances of the respective component codes into the specific method, and the specific content data are shown in the chart, wherein the organic bentonite is used in example 1 without using the organic indene oligomer bentonite, the organic indene oligomer bentonite is used in comparative example 1 without using the bentonite, and the organic indene oligomer bentonite is added in different contents in examples 2 to 4.
Watch 1
Where SF is the helical flow length, GT is the gel time, and Vis is the melt viscosity.
As can be seen from Table 1, the epoxy resin compositions of examples 1-4 showed a slightly lower high pressure SF and a slightly higher viscosity, but a significantly lower low die flow Disc flow; compared with the comparative examples, the low-pressure mold flow of the material added with the organic indene modified bentonite is obviously reduced, and the increase is also obvious from the view of adhesion; however, the adhesion of the organic bentonite which is not modified by indene oligomer is obviously reduced, so that the epoxy resin composition can effectively improve the reliability of products. The above embodiments should not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent transformations fall within the protection scope of the present invention.
Claims (8)
1. An epoxy resin composition characterized by: the composite material comprises the following components in percentage by mass: 2-15 parts of epoxy resin, 2-10 parts of a hardening agent, 0.01-1 part of a hardening accelerator, 70-95 parts of an inorganic filling material, 0.1-0.8 part of a coupling agent, 0.1-1 part of organic indene modified bentonite, 0.1-0.6 part of a release agent, 0.1-1 part of a stress modifier and 0.01-1 part of a coloring agent.
2. The epoxy resin composition according to claim 1, wherein: the epoxy resin is one or a mixture of several of bisphenol epoxy resin, biphenyl epoxy resin, triphenol methane epoxy resin, naphthol epoxy resin, stilbene epoxy resin, epoxy resin containing a triazine core structure, novolac epoxy resin, modified novolac epoxy resin and dicyclopentadiene epoxy resin in any proportion.
3. The epoxy resin composition according to claim 1, wherein: the hardener is one or a mixture of several of novolac resin, cresol novolac resin, naphthalene type phenolic resin and cyclopentadiene type phenolic resin according to any proportion; the hardening accelerator is one or a mixture of several of amines and nitrogen-containing heterocyclic compounds.
4. The epoxy resin composition according to claim 1, wherein: the inorganic filling material is one or a mixture of two of silicon micropowder and alumina; the silicon micro powder and the alumina are spherical, and the maximum grain diameter of the silicon micro powder and the maximum grain diameter of the alumina are both less than 75 microns.
5. The epoxy resin composition according to claim 1, wherein: the coupling agent is a silane coupling agent; the release agent is one or a mixture of several of carnauba wax, montan wax and synthetic wax.
6. The epoxy resin composition according to claim 1, wherein: the organic indene modified bentonite is prepared by the following method:
putting the organic bentonite and indene oligomer into n-heptane, adding a proper amount of silane coupling agent after uniformly stirring, fully stirring for 1-3 h, putting the mixture into a blower box with the temperature of 80-90 ℃ after stirring till the mixture is dried and agglomerated, and crushing and sieving the prepared massive material for later use;
the indene oligomer has the following molecular formula structure:
r represents a hydrogen atom, a methyl group or an ethyl group; m is 5-10; n is 5-15; the molecular weight is 2000-3000.
7. The epoxy resin composition according to claim 1, wherein: the stress modifier is one or a mixture of more of nitrile rubber, ABS rubber copolymer and organic silicone oil.
8. Use of the epoxy resin composition according to any one of claims 1 to 9, wherein: the epoxy resin composition is used as an encapsulating material for discrete devices and integrated circuit packages.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276651A (en) * | 2021-12-24 | 2022-04-05 | 江苏华海诚科新材料股份有限公司 | Epoxy resin composition suitable for low-voltage packaging and preparation method thereof |
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| JP2004043522A (en) * | 2002-07-08 | 2004-02-12 | Nippon Steel Chem Co Ltd | Aromatic oligomer, epoxy resin composition, and its cured product |
| JP2012167141A (en) * | 2011-02-10 | 2012-09-06 | Nippon Steel Chem Co Ltd | Epoxy resin composition and cured product |
| CN111315820A (en) * | 2017-11-14 | 2020-06-19 | 松下知识产权经营株式会社 | Resin composition for encapsulating semiconductor chip and semiconductor package |
| CN113897163A (en) * | 2021-12-09 | 2022-01-07 | 武汉市三选科技有限公司 | Adhesive, chip bonding film and preparation method thereof |
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- 2021-10-22 CN CN202111232864.2A patent/CN113831878B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004043522A (en) * | 2002-07-08 | 2004-02-12 | Nippon Steel Chem Co Ltd | Aromatic oligomer, epoxy resin composition, and its cured product |
| JP2012167141A (en) * | 2011-02-10 | 2012-09-06 | Nippon Steel Chem Co Ltd | Epoxy resin composition and cured product |
| CN111315820A (en) * | 2017-11-14 | 2020-06-19 | 松下知识产权经营株式会社 | Resin composition for encapsulating semiconductor chip and semiconductor package |
| CN113897163A (en) * | 2021-12-09 | 2022-01-07 | 武汉市三选科技有限公司 | Adhesive, chip bonding film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114276651A (en) * | 2021-12-24 | 2022-04-05 | 江苏华海诚科新材料股份有限公司 | Epoxy resin composition suitable for low-voltage packaging and preparation method thereof |
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