CN115521576A - 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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- CN115521576A CN115521576A CN202211113183.9A CN202211113183A CN115521576A CN 115521576 A CN115521576 A CN 115521576A CN 202211113183 A CN202211113183 A CN 202211113183A CN 115521576 A CN115521576 A CN 115521576A
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- epoxy resin
- coupling agent
- resin material
- agent
- stirring
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 104
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 104
- 239000000463 material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 43
- 238000001125 extrusion Methods 0.000 claims abstract description 29
- 239000007822 coupling agent Substances 0.000 claims abstract description 26
- 239000003086 colorant Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000004065 semiconductor Substances 0.000 claims abstract description 18
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 58
- 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 24
- 239000000843 powder Substances 0.000 claims description 24
- 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 16
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 16
- 239000005011 phenolic resin Substances 0.000 claims description 16
- 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
- 239000004593 Epoxy Substances 0.000 claims description 8
- 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
- 229920003986 novolac Polymers 0.000 claims description 7
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical compound C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 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
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 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
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000011353 cycloaliphatic epoxy resin Substances 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
- 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
- 239000004408 titanium dioxide Substances 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
- ULAHYQPCISGAFW-UHFFFAOYSA-N [C-]#N.[SiH4] Chemical compound [C-]#N.[SiH4] ULAHYQPCISGAFW-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- 239000000203 mixture Substances 0.000 abstract description 21
- 238000012360 testing method Methods 0.000 abstract description 12
- 239000000945 filler Substances 0.000 abstract description 11
- 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
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920006336 epoxy molding compound Polymers 0.000 description 2
- 238000004519 manufacturing process 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
- 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
- 239000002253 acid Substances 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
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 150000002527 isonitriles Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 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
Abstract
The invention relates to the field of epoxy resin compositions, in particular to an epoxy resin material and 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 coloring agent under high-speed stirring, then carrying out melt extrusion, cooling and crushing to obtain an intermediate, mixing the prepared intermediate with a certain weight part of an accelerator under high-speed stirring, carrying out melt extrusion, then cooling and crushing to obtain the epoxy resin material. The epoxy resin material prepared by the invention is used for carrying out 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 ratio, and obviously 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 light and thin terminals, products produced by the epoxy molding compound packaging technology also develop towards miniaturization, thinness and super large scale, and meanwhile, higher requirements are provided for the reliability and appearance of the packaged products. HTRB (High Temperature Reverse Bias) is a way of testing the reliability of semiconductor devices, and its requirements are increasing, and along with this, it also drives the package test manufacturers to put forward higher requirements on the related performance of the molding compound.
Disclosure of Invention
The epoxy resin material is subjected TO HTRB (high temperature reverse bias) test after a semiconductor device TO-263 and a semiconductor device TO-247 are packaged, has the characteristic of zero failure rate, and obviously improves the HTRB reliability of the packaged semiconductor device.
In order to accomplish the above object, one 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 coloring agent, melting and extruding, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate prepared in the step (1) and an accelerator, melting and extruding, cooling and crushing to prepare an epoxy resin material;
wherein the weight ratio of the dosage 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 to 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 100 to 125 ℃, more preferably 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 one 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, a DCPD type epoxy resin, a polyfunctional epoxy resin, and a cycloaliphatic epoxy resin.
Preferably, the curing agent is one or more selected from the group consisting of phenol novolac resin, XY-lock type phenol resin, bisphenol a type phenol resin, DCPD type phenol resin, biphenyl type phenol resin, and multifunctional type phenol resin.
Preferably, the accelerator is selected from one or two or more of an organophosphorus compound, an imidazole compound and a tertiary amine compound.
Preferably, the inorganic filler is selected from one or more of silica powder, titanium dioxide powder, alumina powder and magnesia powder; more preferably, the silica powder is one or more selected from the group consisting of crystalline silica powder, fused angle silica powder and fused sphere 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 one or more than two groups selected from epoxy silane coupling agent, amino silane coupling agent, mercapto silane coupling agent, isonitrile acid salt silane coupling agent and vinyl silane coupling agent.
According TO the method for preparing the epoxy resin material, the raw material formula with specific proportion content is adopted, meanwhile, other raw materials except the accelerator are mixed for the first time and are subjected TO melt extrusion TO prepare the intermediate, then the accelerator and the intermediate are mixed for the second time, and the epoxy resin material is prepared through melt extrusion, so that HTRB (high temperature reverse bias) test is performed after the semiconductor device TO-263 and the semiconductor device TO-247 are packaged by the epoxy resin material prepared through the method, the characteristic of zero failure proportion is achieved, and the HTRB reliability of the semiconductor device after the semiconductor device is packaged is remarkably improved. Compared with the conventional production method, the method increases one-time high-speed mixing and one-time melt extrusion process, and is beneficial to the uniformity of material mixing and the combination of the organic resin part and the inorganic filler part.
Detailed Description
The following detailed description will be given with reference to specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In a first aspect, the present invention provides a process for preparing an epoxy resin material, the process comprising the steps of:
(1) Stirring and mixing epoxy resin, a curing agent, an inorganic filler, a release agent, a coupling agent and a coloring agent, melting and extruding, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate prepared in the step (1) and an accelerant, melting and extruding, cooling and crushing to prepare an epoxy resin material;
wherein the weight ratio of the dosage 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 method of the present invention, in a preferred embodiment, 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 to 27:15-27:1.8-2.5:215-294:3-7:3-6:1.
in the method of 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 of 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 in the range of 110 to 120 ℃.
In the method of 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 of the present invention, in a specific embodiment, in the step (2), the melt extrusion temperature may be 110 to 120 ℃, for example, may be 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 be performed using a processing apparatus conventional in the art, for example, a two-roll mill, a single screw extruder, a twin screw extruder, a kneader, a stirrer, and the like.
In the method of the present invention, in a specific embodiment, the epoxy resin is one 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, a DCPD type epoxy resin, a multifunctional type epoxy resin, and a cycloaliphatic epoxy resin.
In a specific embodiment of the method of the present invention, the curing agent is one or more selected from the group consisting of a phenol novolac resin, an XY-lock type phenol resin, a bisphenol a type phenol resin, a DCPD type phenol resin, a biphenyl type phenol resin, and a multifunctional type phenol resin.
In the method of the present invention, in a specific embodiment, the accelerator is one or two or more selected from the group consisting of an organophosphorus 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, titanium dioxide powder, alumina powder and magnesia powder; in a preferred embodiment, the silica powder is one or more selected from the group consisting of crystalline silica powder, fused angle silica powder and fused sphere silica powder.
In a specific embodiment of the method of the present invention, the release agent is selected from one or two or more of mineral wax, vegetable wax, polyethylene and polyamide wax.
In a particular embodiment, in the method of the present invention, the colorant is carbon black.
In a specific embodiment of the method of the present invention, the coupling agent is one or more selected from the group consisting of an epoxy silane coupling agent, an aminosilane coupling agent, a mercaptosilane coupling agent, an isonitrile silane coupling agent, and a vinyl silane coupling agent.
In a second aspect, the present invention provides an epoxy resin material prepared by the foregoing method.
The third aspect of the present invention provides a use of the above epoxy resin material in a semiconductor package.
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 product is purchased from Shandong Shengquan resin, and the product brand is SQCN700-1.3;
epoxy resin: biphenyl type epoxy resin: number average molecular weight of 2500, epoxy equivalent of 195g/mol, available from Nippon DIC under the trade name YX-4000;
curing agent: phenol novolac resin: the product has a number average molecular weight of 1200, is purchased from Shandong Shengquan resin and has a product brand of PF8010;
curing agent: biphenyl type phenol resin: the number average molecular weight is 2000, the new material is purchased from Shanghai balance seal, and the product brand is Resicare3900;
accelerator (b): 2-methylimidazole, available from chemical industries of four kingdoms, japan;
inorganic filler: crystalline silica, available from Jiangsu Union, with a product designation of DF-1220M;
inorganic filler: the fused spherical silicon dioxide is purchased from Jiangsu Lirui, and the product brand is NQ-101;
inorganic filler: alumina, available from tianjinze;
releasing agent: carnauba wax, available from bunton corporation;
coupling agent: propyl ether trimethoxysilane (available from Jiangsu morning light);
colorant: carbon black, available from Sichuan.
Example 1
Example 1 the raw material components for the preparation of the epoxy resin material are 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 the stirring speed of 210rpm for 50min, then extruding the mixture in a double-screw extruder at the melt extrusion temperature of 110 ℃, and finally cooling and crushing the mixture to prepare an intermediate;
(2) And (2) stirring and mixing the intermediate prepared in the step (1) and an accelerator according to a certain proportion at a stirring speed of 210rpm for 40min, then extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to prepare the epoxy resin material.
Example 2
Example 2 the raw material components for the preparation of the epoxy resin material are 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 205rpm for 55min, then extruding the mixture in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing the mixture to prepare an intermediate;
(2) And (2) stirring and mixing the intermediate prepared in the step (1) and an accelerator according to a certain proportion at a stirring speed of 210rpm for 50min, then extruding in a double-screw extruder at a melt extrusion temperature of 110 ℃, and finally cooling and crushing to prepare the epoxy resin material.
Example 3
Example 3 the raw material components for the preparation of the epoxy resin material are 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 the stirring speed of 215rpm for 50min, then extruding the mixture in a double-screw extruder at the melt extrusion temperature of 120 ℃, and finally cooling and crushing the mixture to prepare an intermediate;
(2) And (2) stirring and mixing the intermediate prepared in the step (1) and an accelerator according to a certain proportion at a stirring speed of 215rpm for 45min, then extruding in a double-screw extruder at a melt extrusion temperature of 120 ℃, and finally cooling and crushing to prepare the epoxy resin material.
Example 4
Example 4 the raw material components for the preparation of the epoxy resin material are 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, then extruding the mixture in a double-screw extruder at a melt extrusion temperature of 125 ℃, and finally cooling and crushing the mixture to prepare an intermediate;
(2) And (2) stirring and mixing the intermediate prepared in the step (1) and an accelerator according to a certain proportion at a stirring speed of 220rpm for 50min, then extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to prepare the epoxy resin material.
Comparative example 1
Comparative example 1 the raw material components for the preparation of the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of this 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 the stirring speed of 210rpm for 50min, then extruding the mixture in a double-screw extruder at the melt extrusion temperature of 110 ℃, and finally cooling and crushing the mixture to prepare an intermediate;
(2) And (2) stirring and mixing the intermediate prepared in the step (1) and an accelerator according to a certain proportion at a stirring speed of 210rpm for 40min, then extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to prepare 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 this 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 the stirring speed of 210rpm for 50min, then extruding in a double-screw extruder at the melt extrusion temperature of 110 ℃, and finally cooling and crushing to obtain an intermediate;
(2) And (2) stirring and mixing the intermediate prepared in the step (1) and an accelerator according to a certain proportion at a stirring speed of 210rpm for 40min, then extruding in a double-screw extruder at a melt extrusion temperature of 115 ℃, and finally cooling and crushing to prepare the epoxy resin material.
Comparative example 3
Comparative example 3 the raw material components for the preparation of the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of this comparative example is as follows:
the epoxy resin, the curing agent, the accelerator, the filler, the release agent, the coupling agent and the colorant are crushed by a crusher at room temperature, the crushed materials are stirred and mixed at the stirring speed of 210rpm for 40min, then the mixture is extruded in a double-screw extruder at the melt extrusion temperature of 115 ℃, and finally the mixture is cooled and crushed to obtain the epoxy resin material.
Comparative example 4
Comparative example 4 the raw material components for the preparation of the epoxy resin material are shown in table 1.
The method for preparing the epoxy resin material of this comparative example is as follows:
the epoxy resin, the curing agent, the accelerator, the filler, the release agent, the coupling agent and the colorant are crushed by a crusher at room temperature, the crushed materials are stirred and mixed at the stirring speed of 210rpm for 50min, then the mixture is extruded in a double-screw extruder at the melt extrusion temperature of 110 ℃, and finally the mixture is cooled and crushed 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 this comparative example is as follows:
the epoxy resin, the curing agent, the accelerator, the filler, the release agent, the coupling agent and the colorant are crushed by a crusher at room temperature, the crushed materials are stirred and mixed at the stirring speed of 210rpm for 50min, then the mixture is extruded in a double-screw extruder at the melt extrusion temperature of 110 ℃, and finally the mixture is cooled and crushed 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 this comparative example is as follows:
the epoxy resin, the curing agent, the accelerator, the filler, the release agent, the coupling agent and the colorant are crushed by a crusher at room temperature, the crushed materials are stirred and mixed at the stirring speed of 210rpm for 50min, then the mixture is extruded in a double-screw extruder at the melt extrusion temperature of 110 ℃, and finally the mixture is cooled and crushed to obtain the epoxy resin material.
TABLE 1 raw Material Components of epoxy resin materials of examples 1 to 4 and comparative examples 1 to 6
Test example
HTRB (high temperature reverse bias): according to JESD22-A108, the test conditions were as follows: 150 ℃, 80% BVdsSRating,500hrs, wherein the criterion for failure is the leakage current I DSS ≥1mA。
HTRB (high temperature reverse bias) tests were performed on the epoxy resin materials prepared in examples 1-4 and comparative examples 1-6 after encapsulation of TO-263 and TO-247, respectively, and the test results are shown in Table 2 and Table 3.
TABLE 2 HTRB test results of TO-263, an epoxy resin material-encapsulated semiconductor device prepared in examples 1-4 and comparative examples 1-6
TABLE 3 HTRB test results of TO-247 epoxy resin material-encapsulated semiconductor devices prepared in examples 1-4 and comparative examples 1-6
It can be seen from the test results of examples 1 TO 4 and comparative examples 1 TO 6 that the epoxy resin material prepared by using the raw material components in a specific ratio and simultaneously combining the improved epoxy resin materials is prepared by mixing the raw materials except the accelerator for the first time and melt-extruding the mixture TO prepare an intermediate, mixing the accelerator for the second time and the intermediate in a specific weight ratio, and melt-extruding the mixture TO prepare the epoxy resin material.
The above description is only an example of the present invention and is not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention as described in the specification of the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
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 coloring agent, melting and extruding, cooling and crushing to obtain an intermediate;
(2) Stirring and mixing the intermediate prepared in the step (1) and an accelerant, melting and extruding, cooling and crushing to prepare an epoxy resin material;
wherein the weight ratio of the dosage 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.
2. the method according to claim 1, wherein 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 to 27:15-27:1.8-2.5:215-294:3-7:3-6:1.
3. the method according to claim 1, wherein 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 100 to 125 ℃, more preferably 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 to 120 ℃.
4. The method according to claim 1 or 3, wherein the epoxy resin is one 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, a DCPD type epoxy resin, a polyfunctional type epoxy resin, and a cycloaliphatic epoxy resin;
preferably, the curing agent is one or more selected from the group consisting of a phenol novolac resin, an XY-lock type phenol resin, a bisphenol a type phenol resin, a DCPD type phenol resin, a biphenyl type phenol resin, and a multifunctional type phenol resin.
5. The method according to claim 1 or 3, 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.
6. The method according to claim 1 or 3, wherein the inorganic filler is selected from one or more of silica powder, titanium dioxide powder, alumina powder, and magnesia powder;
preferably, the silica powder is one or more selected from the group consisting of crystalline silica powder, fused angle silica powder and fused sphere silica powder.
7. The method according to claim 1 or 3, wherein the release agent is selected from one or more of mineral wax, vegetable wax, polyethylene and polyamide wax;
preferably, the colorant is carbon black.
8. The method according to claim 1 or 3, wherein the coupling agent is one or more selected from the group consisting of an epoxy silane coupling agent, an amino silane coupling agent, a mercapto silane coupling agent, an isonitrile silane coupling agent, and a vinyl silane coupling agent.
9. An epoxy resin material, characterized in that it is prepared by the process according to any one of claims 1 to 8.
10. Use of an epoxy resin material prepared by the method of any one of claims 1 to 8 or the epoxy resin material of claim 9 in semiconductor packaging.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| 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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