CN115521576B - Epoxy resin material and preparation method and application thereof - Google Patents
Epoxy resin material and preparation method and application thereof Download PDFInfo
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- CN115521576B CN115521576B CN202211113183.9A CN202211113183A CN115521576B CN 115521576 B CN115521576 B CN 115521576B CN 202211113183 A CN202211113183 A CN 202211113183A CN 115521576 B CN115521576 B CN 115521576B
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- coupling agent
- melt extrusion
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 107
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 107
- 239000000463 material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 47
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 46
- 238000001125 extrusion Methods 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000007822 coupling agent Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 239000003086 colorant Substances 0.000 claims abstract description 23
- 239000004065 semiconductor Substances 0.000 claims abstract description 17
- 238000004806 packaging method and process Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 60
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000000155 melt Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 24
- 229920003986 novolac Polymers 0.000 claims description 22
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 16
- 239000011256 inorganic filler Substances 0.000 claims description 15
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 15
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- -1 imidazole compound Chemical class 0.000 claims description 9
- 235000010290 biphenyl Nutrition 0.000 claims description 8
- 239000004305 biphenyl Substances 0.000 claims description 8
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 claims description 8
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 229910002026 crystalline silica Inorganic materials 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000002527 isonitriles Chemical class 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 239000012184 mineral wax Substances 0.000 claims description 3
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 3
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000012178 vegetable wax Substances 0.000 claims description 3
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 3
- 239000001993 wax Substances 0.000 claims description 3
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 abstract description 11
- 238000012360 testing method Methods 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000009775 high-speed stirring Methods 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 24
- 239000002994 raw material Substances 0.000 description 15
- 238000010298 pulverizing process Methods 0.000 description 8
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 2
- 229920006336 epoxy molding compound Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- VOGVKUPHFCAFRO-UHFFFAOYSA-N 1-propoxypropane trimethoxysilane Chemical compound O(C)[SiH](OC)OC.C(CC)OCCC VOGVKUPHFCAFRO-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- TVZRAEYQIKYCPH-UHFFFAOYSA-N 3-(trimethylsilyl)propane-1-sulfonic acid Chemical compound C[Si](C)(C)CCCS(O)(=O)=O TVZRAEYQIKYCPH-UHFFFAOYSA-N 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
-
- 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
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to the field of epoxy resin compositions, in particular to an epoxy resin material, a preparation method and application thereof. The method comprises the steps of firstly mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant under high-speed stirring, then carrying out melt extrusion, cooling and crushing to obtain an intermediate, mixing the obtained intermediate with a certain weight part of accelerator under high-speed stirring, carrying out melt extrusion, and then carrying out cooling and crushing to obtain the epoxy resin material. The epoxy resin material prepared by the invention is subjected TO HTRB (high temperature reverse bias) test after packaging the semiconductor device TO-263 and the semiconductor device TO-247, has the characteristic of zero failure proportion, and remarkably improves the HTRB reliability after packaging the semiconductor.
Description
Technical Field
The invention relates to the technical field of epoxy molding compounds, in particular to the technical field of thermosetting plastics, and specifically relates to an epoxy resin material and a preparation method and application thereof.
Background
In recent years, with the rapid development of the semiconductor industry, the integrated circuit and semiconductor device packaging industry has also begun to develop rapidly. At present, as the semiconductor and integrated circuit industries develop towards lighter and thinner terminals, products produced by the epoxy molding compound packaging technology also develop towards miniaturization, thinness and ultra-large scale, and simultaneously, higher requirements are also put on the reliability and appearance of packaged products. HTRB (High Temperature Reverse Bias high temperature reverse bias) is also increasingly required as a way to test the reliability of semiconductor devices, and accordingly, the packaging manufacturers are driven to put higher requirements on the related performance of plastic packaging materials.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides an epoxy resin material, a preparation method and application thereof, wherein the epoxy resin material is subjected TO HTRB (high temperature reverse bias) test after packaging a semiconductor device TO-263 and a semiconductor device TO-247, has the characteristic of zero failure proportion, and remarkably improves the HTRB reliability of the packaged semiconductor device.
In order to achieve the above object, the present invention provides, in one aspect, a method of preparing an epoxy resin material, the method comprising the steps of:
(1) Stirring and mixing epoxy resin, a curing agent, an inorganic filler, a release agent, a coupling agent and a colorant, carrying out melt extrusion, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate prepared in the step (1) with an accelerator, carrying out melt extrusion, and then cooling and crushing to prepare an epoxy resin material;
Wherein, the weight ratio of the dosages of the epoxy resin, the curing agent, the accelerator, the inorganic filler, the release agent, the coupling agent and the colorant is 12.5-35:12.5-35:0.75-3:212-297:0.5-10:1.25-10: 1.
Preferably, the epoxy resin, the curing agent, the accelerator, the inorganic filler, the release agent, the coupling agent and the colorant are used in a weight ratio of 15-27:15-27:1.8-2.5:215-294:3-7:3-6:1.
Preferably, in the step (1), the stirring speed is 180-230rpm, and the stirring time is 20-60min.
Preferably, in the step (1), the stirring speed is 205-215rpm, and the stirring time is 45-55min;
Preferably, in step (1), the melt extrusion temperature is from 100 to 125 ℃, more preferably from 110 to 120 ℃;
preferably, in the step (2), the stirring speed is 180-230rpm, and the stirring time is 20-60min;
Preferably, in the step (2), the stirring speed is 205-215rpm, and the stirring time is 30-50min;
preferably, in step (2), the melt extrusion temperature is 110-120 ℃.
Preferably, the epoxy resin is selected from one or more of a novolac type epoxy resin, a bisphenol a type epoxy resin, a biphenyl type epoxy resin, a naphthalene type epoxy resin, an o-cresol type epoxy resin, a DCPD type epoxy resin, a multifunctional type epoxy resin, and an alicyclic epoxy resin.
Preferably, the curing agent is selected from one or more of a novolac resin, an XY-lock type novolac resin, a bisphenol a type novolac resin, a DCPD type novolac resin, a biphenyl type novolac resin, and a multifunctional type novolac resin.
Preferably, the accelerator is one or more selected from the group consisting of an organic phosphorus compound, an imidazole compound and a tertiary amine compound.
Preferably, the inorganic filler is selected from one or more of silica powder, titania powder, alumina powder and magnesia powder; more preferably, the silica powder is selected from one or more of crystalline silica powder, fused angular silica powder, and fused spherical silica powder.
Preferably, the release agent is selected from one or more of mineral wax, vegetable wax, polyethylene and polyamide wax.
Preferably, the colorant is carbon black.
Preferably, the coupling agent is selected from one or more than two of epoxy silane coupling agent, amino silane coupling agent, mercapto silane coupling agent, isonitrile acid salt silane coupling agent and vinyl silane coupling agent.
The method for preparing the epoxy resin material adopts the raw material formula with specific proportion content, simultaneously carries out first mixing and melt extrusion on other raw materials except the accelerator TO prepare an intermediate, then carries out second mixing and melt extrusion on the accelerator and the intermediate TO prepare the epoxy resin material, so that the epoxy resin material prepared by the method is used for carrying out HTRB (high temperature reverse bias) test after packaging a semiconductor device TO-263 and a semiconductor device TO-247, has the characteristic of zero failure proportion, and obviously improves the HTRB reliability of the packaged semiconductor device. Compared with the conventional production method, the method adds one-time high-speed mixing and one-time melt extrusion process, and is beneficial to the uniformity of material mixing and the combination of an organic resin part and an inorganic filler part.
Detailed Description
The following detailed description is made in connection with specific embodiments of the invention. 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 present invention provides a method of preparing an epoxy resin material, the method comprising the steps of:
(1) Stirring and mixing epoxy resin, a curing agent, an inorganic filler, a release agent, a coupling agent and a colorant, carrying out melt extrusion, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate prepared in the step (1) with an accelerator, carrying out melt extrusion, and then cooling and crushing to prepare an epoxy resin material;
Wherein, the weight ratio of the dosages of the epoxy resin, the curing agent, the accelerator, the inorganic filler, the release agent, the coupling agent and the colorant is 12.5-35:12.5-35:0.75-3:212-297:0.5-10:1.25-10: 1.
In the process according to the invention, in a preferred embodiment, the epoxy resin, the curing agent, the accelerator, the inorganic filler, the mold release agent, the coupling agent and the colorant are used in a weight ratio of 15 to 27:15-27: 1.8-2.5:215-294:3-7:3-6:1.
In the method according to the present invention, in a specific embodiment, in the step (1), the stirring speed may be 180 to 230rpm, for example, 180rpm, 190rpm, 200rpm, 205rpm, 210rpm, 215rpm, 220rpm or 230rpm; the stirring time may be 20-60min, for example, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60min. In a preferred embodiment, the stirring speed is 205-215rpm and the stirring time is 45-55min.
In the method according to the present invention, in a specific embodiment, in the step (1), the melt extrusion temperature may be 100 to 125 ℃, for example, may be 100 ℃, 110 ℃, 120 ℃ or 125 ℃. In a preferred embodiment, the melt extrusion temperature is 110 to 120 ℃.
In the method according to the present invention, in a specific embodiment, in the step (2), the stirring speed may be 180 to 230rpm, for example, 180rpm, 190rpm, 200rpm, 205rpm, 210rpm, 215rpm, 220rpm or 230rpm; the stirring time may be 20-60min, for example, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60min. In a preferred embodiment, the stirring speed is 205-215rpm and the stirring time is 30-50min.
In the method according to the present invention, in a specific embodiment, in the step (2), the melt extrusion temperature may be 110 to 120 ℃, for example, 110 ℃, 115 ℃ or 120 ℃.
In the method of the present invention, in a specific embodiment, the melt extrusion in step (1) and step (2) may use processing equipment conventional in the art, for example, processing equipment such as a twin roll mill, a single screw extruder, a twin screw extruder, a kneader, a stirrer, etc.
In the method of the present invention, in a specific embodiment, the epoxy resin is selected from one or more of a novolac type epoxy resin, a bisphenol a type epoxy resin, a biphenyl type epoxy resin, a naphthalene type epoxy resin, an o-cresol type epoxy resin, a DCPD type epoxy resin, a polyfunctional type epoxy resin, and a cycloaliphatic epoxy resin.
In the method of the present invention, in a specific embodiment, the curing agent is one or more selected from the group consisting of a novolac resin, an XY-lock type novolac resin, a bisphenol a type novolac resin, a DCPD type novolac resin, a biphenyl type novolac resin, and a multifunctional type novolac resin.
In the method of the present invention, in a specific embodiment, the accelerator is selected from one or more of an organic phosphorus compound, an imidazole compound, and a tertiary amine compound.
In the method of the present invention, in a specific embodiment, the inorganic filler is selected from one or two or more of silica powder, titania powder, alumina powder and magnesia powder; in a preferred embodiment, the silica powder is selected from one or two or more of crystalline silica powder, fused angular silica powder and fused spherical silica powder.
In a specific embodiment, the release agent is selected from one or more of mineral wax, vegetable wax, polyethylene and polyamide wax.
In a specific embodiment of the method of the present invention, the colorant is carbon black.
In the method of the present invention, in a specific embodiment, the coupling agent is one or more selected from the group consisting of an epoxy silane coupling agent, an aminosilane coupling agent, a mercapto silane coupling agent, an isonitrile acid salt silane coupling agent and a vinyl silane coupling agent.
In a second aspect, the present invention provides an epoxy resin material prepared by the method described above.
The third aspect of the invention provides an application of the epoxy resin material in semiconductor packaging.
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:
epoxy resin: o-cresol type epoxy resin: the number average molecular weight is 3000, the epoxy equivalent is 205g/mol, the epoxy equivalent is purchased from Shandong holy spring resin, and the product mark is SQCN, 700-1.3;
Epoxy resin: biphenyl type epoxy resin: the number average molecular weight was 2500, the epoxy equivalent was 195g/mol, and the product was obtained from DIC Co., ltd., product brand YX-4000;
curing agent: phenolic novolac resin: the number average molecular weight is 1200, and the product brand is PF8010, which is purchased from Shandong holy spring resin;
Curing agent: biphenyl type phenolic resin: the number average molecular weight is 2000, the new material is purchased from Shanghai scale seal, and the product brand is Resicare3900;
and (3) an accelerator: 2-methylimidazole available from Kagaku Kogyo Co., ltd;
inorganic filler: crystalline silica, available from Jiangsu bian Rui under the product designation DF-1220M;
inorganic filler: fused spherical silica, available from Jiangsu bian Rui under the product designation NQ-101;
Inorganic filler: alumina, available from Tianjin Zeshi;
and (3) a release agent: carnauba wax, available from bang Liu Tongshang, inc;
coupling agent: propyl ether trimethoxysilane (available from Jiangsu morning light);
Coloring agent: carbon black, available from Sichuan.
Example 1
Example 1 the raw material 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) Stirring and mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant at a stirring speed of 210rpm for 50min, extruding at a melt extrusion temperature of 110 ℃ in a double-screw extruder, and finally cooling and crushing to obtain an intermediate;
(2) And (3) stirring and mixing the intermediate prepared in the step (1) and the accelerator according to a certain proportion at a stirring speed of 210rpm for 40min, extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to obtain the epoxy resin material.
Example 2
Example 2 the raw material 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) Mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant at a stirring speed of 205rpm for 55min, extruding at a melt extrusion temperature of 115 ℃ in a double-screw extruder, and finally cooling and crushing to obtain an intermediate;
(2) And (3) stirring and mixing the intermediate prepared in the step (1) and the accelerator according to a certain proportion at a stirring speed of 210rpm for 50min, extruding in a double-screw extruder at a melt extrusion temperature of 110 ℃, and finally cooling and crushing to obtain the epoxy resin material.
Example 3
Example 3 the raw material 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) Mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant at a stirring speed of 215rpm for 50min, extruding at a melt extrusion temperature of 120 ℃ in a double-screw extruder, and finally cooling and crushing to obtain an intermediate;
(2) And (3) stirring and mixing the intermediate prepared in the step (1) and the accelerator according to a certain proportion at a stirring speed of 215rpm for 45min, extruding in a double-screw extruder at a melt extrusion temperature of 120 ℃, and finally cooling and crushing to obtain the epoxy resin material.
Example 4
Example 4 the raw material 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) Stirring and mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant at a stirring speed of 220rpm for 50min, extruding at a melt extrusion temperature of 125 ℃ in a double-screw extruder, and finally cooling and crushing to obtain an intermediate;
(2) And (3) stirring and mixing the intermediate prepared in the step (1) and the accelerator according to a certain proportion at a stirring speed of 220rpm for 50min, extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to obtain the epoxy resin material.
Comparative example 1
Comparative example 1 the raw material components for preparing the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of the comparative example is as follows:
(1) Stirring and mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant at a stirring speed of 210rpm for 50min, extruding at a melt extrusion temperature of 110 ℃ in a double-screw extruder, and finally cooling and crushing to obtain an intermediate;
(2) And (3) stirring and mixing the intermediate prepared in the step (1) and the accelerator according to a certain proportion at a stirring speed of 210rpm for 40min, extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to obtain the epoxy resin material.
Comparative example 2
Comparative example 2 the raw material components for preparing the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of the comparative example is as follows:
(1) Stirring and mixing epoxy resin, a curing agent, a filler, a release agent, a coupling agent and a colorant at a stirring speed of 210rpm for 50min, extruding at a melt extrusion temperature of 110 ℃ in a double-screw extruder, and finally cooling and crushing to obtain an intermediate;
(2) And (3) stirring and mixing the intermediate prepared in the step (1) and the accelerator according to a certain proportion at a stirring speed of 210rpm for 40min, extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to obtain the epoxy resin material.
Comparative example 3
Comparative example 3 the raw material components for preparing the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of the comparative example is as follows:
Pulverizing epoxy resin, a curing agent, an accelerator, a filler, a release agent, a coupling agent and a colorant at room temperature by using a pulverizer, stirring and mixing the pulverized materials at a stirring speed of 210rpm for 40min, extruding at a melt extrusion temperature of 115 ℃ in a twin-screw extruder, cooling, and pulverizing to obtain the epoxy resin material.
Comparative example 4
Comparative example 4 the raw material components for preparing the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of the comparative example is as follows:
Pulverizing epoxy resin, a curing agent, an accelerator, a filler, a release agent, a coupling agent and a colorant at room temperature by using a pulverizer, stirring and mixing the pulverized materials at a stirring speed of 210rpm for 50min, extruding at a melt extrusion temperature of 110 ℃ in a twin-screw extruder, cooling, and pulverizing to obtain the epoxy resin material.
Comparative example 5
Comparative example 5 the raw material components for preparing the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of the comparative example is as follows:
Pulverizing epoxy resin, a curing agent, an accelerator, a filler, a release agent, a coupling agent and a colorant at room temperature by using a pulverizer, stirring and mixing the pulverized materials at a stirring speed of 210rpm for 50min, extruding at a melt extrusion temperature of 110 ℃ in a twin-screw extruder, cooling, and pulverizing to obtain the epoxy resin material.
Comparative example 6
Comparative example 6 the raw material components for preparing the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of the comparative example is as follows:
Pulverizing epoxy resin, a curing agent, an accelerator, a filler, a release agent, a coupling agent and a colorant at room temperature by using a pulverizer, stirring and mixing the pulverized materials at a stirring speed of 210rpm for 50min, extruding at a melt extrusion temperature of 110 ℃ in a twin-screw extruder, cooling, and pulverizing to obtain the epoxy resin material.
TABLE 1 raw material components of epoxy resin materials of examples 1-4 and comparative examples 1-6
Test case
HTRB (high temperature reverse bias): according to JESD22-A108, the test conditions were as follows: 150 ℃, 80% BVDSRating, 500hrs, wherein the failure criterion is leakage current I DSS. Gtoreq.1 mA.
The epoxy resin materials prepared in examples 1 TO 4 and comparative examples 1 TO 6 were subjected TO HTRB (high temperature reverse bias) test after packaging TO-263 and TO-247, respectively, and the test results are shown in Table 2, table 3.
TABLE 2 HTRB test results of epoxy resin Material encapsulation semiconductor device TO-263 prepared in examples 1-4 and comparative examples 1-6
TABLE 3 HTRB test results of epoxy resin Material encapsulation semiconductor device TO-247 prepared in examples 1-4 and comparative examples 1-6
As can be seen from the test results of examples 1-4 and comparative examples 1-6, the preparation method of the epoxy resin material after combination improvement simultaneously uses the raw material components in a specific ratio, namely, the raw materials except the accelerator are mixed for the first time and are subjected TO melt extrusion TO prepare an intermediate, and then the accelerator and the intermediate in a certain weight ratio are mixed for the second time and are subjected TO melt extrusion TO prepare the epoxy resin material.
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 (14)
1. A method of preparing an epoxy resin material, the method comprising the steps of:
(1) Stirring and mixing epoxy resin, a curing agent, an inorganic filler, a release agent, a coupling agent and a colorant, carrying out melt extrusion, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate prepared in the step (1) with an accelerator, carrying out melt extrusion, and then cooling and crushing to prepare an epoxy resin material;
Wherein, the weight ratio of the dosages of the epoxy resin, the curing agent, the accelerator, the inorganic filler, the release agent, the coupling agent and the colorant is 15-27:15-27:1.8-2.5:215-294:3-7:3-6:1, a step of;
In the step (1), the stirring speed is 180-230rpm, and the stirring time is 20-60min;
in the step (1), the melt extrusion temperature is 100-125 ℃;
In the step (2), the stirring speed is 180-230rpm, and the stirring time is 20-60min;
in the step (2), the melt extrusion temperature is 110-120 ℃.
2. The method according to claim 1, wherein in the step (1), the stirring speed is 205 to 215rpm and the stirring time is 45 to 55min.
3. The method of claim 1, wherein in step (1), the melt extrusion temperature is 110-120 ℃.
4. The method according to claim 1 or 2, wherein in step (2), the stirring speed is 205-215rpm and the stirring time is 30-50min.
5. The method according to any one of claims 1 to 4, wherein the epoxy resin is one or two or more selected from the group consisting of a novolac type epoxy resin, a bisphenol a type epoxy resin, a biphenyl type epoxy resin, a naphthalene type epoxy resin, an o-cresol type epoxy resin, a DCPD type epoxy resin, a polyfunctional type epoxy resin, and a cycloaliphatic epoxy resin.
6. The method according to any one of claims 1 to 4, wherein the curing agent is one or more selected from the group consisting of a novolac resin, an XY-lock type novolac resin, a bisphenol a type novolac resin, a DCPD type novolac resin, a biphenyl type novolac resin, and a multifunctional type novolac resin.
7. The method according to any one of claims 1 to 4, wherein the accelerator is one or two or more selected from the group consisting of an organic phosphorus compound, an imidazole compound and a tertiary amine compound.
8. The method according to any one of claims 1 to 4, wherein the inorganic filler is one or two or more selected from the group consisting of silica powder, titania powder, alumina powder and magnesia powder.
9. The method according to claim 8, wherein the silica powder is one or more selected from the group consisting of crystalline silica powder, fused angular silica powder and fused spherical silica powder.
10. The method according to any one of claims 1 to 4, wherein the release agent is one or two or more selected from the group consisting of mineral wax, vegetable wax, polyethylene and polyamide wax.
11. The method of any one of claims 1-4, wherein the colorant is carbon black.
12. The method according to any one of claims 1 to 4, wherein the coupling agent is one or more selected from the group consisting of an epoxy silane coupling agent, an aminosilane coupling agent, a mercapto silane coupling agent, an isonitrile acid salt silane coupling agent and a vinyl silane coupling agent.
13. An epoxy resin material, characterized in that it is prepared by the method according to any one of claims 1 to 12.
14. Use of the epoxy resin material prepared by the method of any one of claims 1-12 or the epoxy resin material of claim 13 in semiconductor packaging.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105778409A (en) * | 2014-12-18 | 2016-07-20 | 北京首科化微电子有限公司 | Epoxy resin composition for semiconductor packaging, and preparation method thereof |
| CN112679141A (en) * | 2020-12-23 | 2021-04-20 | 江苏科化新材料科技有限公司 | Epoxy resin composition for improving appearance of semiconductor package and preparation method thereof |
| CN114350295A (en) * | 2021-12-30 | 2022-04-15 | 江苏科化新材料科技有限公司 | Epoxy resin composition, preparation method and application thereof, epoxy resin and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105778409A (en) * | 2014-12-18 | 2016-07-20 | 北京首科化微电子有限公司 | Epoxy resin composition for semiconductor packaging, and preparation method thereof |
| CN112679141A (en) * | 2020-12-23 | 2021-04-20 | 江苏科化新材料科技有限公司 | Epoxy resin composition for improving appearance of semiconductor package and preparation method thereof |
| CN114350295A (en) * | 2021-12-30 | 2022-04-15 | 江苏科化新材料科技有限公司 | Epoxy resin composition, preparation method and application thereof, epoxy resin and application thereof |
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