CN108892926A - A kind of modified additive, modified epoxy plastic packaging material and preparation method thereof - Google Patents

A kind of modified additive, modified epoxy plastic packaging material and preparation method thereof Download PDF

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CN108892926A
CN108892926A CN201810632063.7A CN201810632063A CN108892926A CN 108892926 A CN108892926 A CN 108892926A CN 201810632063 A CN201810632063 A CN 201810632063A CN 108892926 A CN108892926 A CN 108892926A
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parts
modified
plastic packaging
packaging material
powder
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Naga Taehye Long Xin Mstar Technology Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • 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
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0812—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Epoxy Resins (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention discloses a kind of modified additive, modified epoxy plastic packaging material and preparation method thereof, the plastic packaging material includes following components：Tricyanic epoxy resin, ACR resin, perfluorinated sulfonic resin, 107 rubber powders, silicone powder, modified additive, zinc dialkyl dithiophosphate, pyridine carboxylic acid magnesium, niacin butyl ester (acidum nicotinicum butyl ester), N- methyl -4- cyano benzylamine, cashew nut shell oil, heptadecyl imidazole quinoline, 2,3- difluoro phenyl boric acid, trioctyl trimellitate (TOTM), two iso stearyl metatitanic acid second diester, Polyethylene Glycol Oleate.Linear expansion coefficient, mechanical property and the heat resistance of modified epoxy plastic packaging material provided by the invention reach a higher level, of good reliability, can meet the requirement of Electronic Encapsulating Technology.

Description

A kind of modified additive, modified epoxy plastic packaging material and preparation method thereof
The application is application No. is 201610736090X, and the applying date is on 08 26th, 2016, and invention and created name is The divisional application of the patent of " a kind of integrated circuit modified epoxy plastic packaging material and preparation method thereof ".
Technical field
The invention belongs to technical field of electronic materials, and in particular to a kind of integrated circuit modified epoxy plastic packaging material and its preparation Method.
Background technique
Electronic Packaging is all parts of composition electronic component or integrated circuit by defined requirement reasonable Arrangement, group It fills, connect and be environmentally isolated with, to prevent water point, the erosion of dust and pernicious gas to component, slow down vibration, prevent external force Damage and stable element parameter.Electronic Packaging can substantially be divided into Plastic Package, ceramic package and Metal Packaging.Relative to rear two Kind encapsulating material, Plastic Package is since its is at low cost, is suitable for large-scale production, using more and more extensive in electronics industry.
The wide variety of plastic packaging material mainly carrys out acyl including phenolic resin, epoxy resin, cyanic acid resin, polyimides, span Imines etc..Wherein, for epoxy-plastic packaging material due to its simple production process, low cost, performance reliability is good, and weight is occupied in plastic packaging material Want status.Direction with integrated circuit towards chip enlargement and wiring imperceptibility is developed, and mounting means and packing forms Also in continuous development and change, therefore the performance requirement of epoxy-plastic packaging material is also greatly promoted.In order to meet growth requirement, it is desirable that Epoxy-plastic packaging material has better heat resistance, moisture resistivity, low linear expansion coefficient and higher reliability.
Summary of the invention
For this purpose, the present invention provides a kind of integrated circuit modified epoxy plastic packaging material and preparation method thereof, the above existing skill is solved Technical problem in art.
For this purpose, the present invention provides a kind of integrated circuit modified epoxy plastic packaging material, it include following components by weight：Three 55-70 parts of paracyanogen acid epoxy resin, 11-20 parts of ACR resin, 6-13 parts of perfluorinated sulfonic resin, 3-8 parts of 107 rubber powder, silicone powder 2- 6 parts, modified additive 1-4 parts, 3-7 parts of zinc dialkyl dithiophosphate, 2-5 parts of pyridine carboxylic acid magnesium, niacin butyl ester (3- pyridine first Acid butyl ester) 4-8 parts, 5-15 parts of N- methyl -4- cyano benzylamine, 4-12 parts of cashew nut shell oil, 2-8 parts of heptadecyl imidazole quinoline, 2,3- 1-5 parts of difluoro phenyl boric acid, 3-8 parts of trioctyl trimellitate (TOTM), 2-7 parts of diisostearoyl ethylene titanate, oleic acid polyethylene glycol 5-9 parts of ester；
The modified additive includes that mass ratio is 1:The modified aluminium powder of 2-5 and modified glass powder.
According to embodiment of the present invention, wherein the modified aluminium powder is that aluminium powder first passes through potassium permanganate processing simultaneously Drying, using being milled to changing of obtaining after 50-150 mesh after otoginsenoside, arginine and cocounut oil acyl diethanol amine Combined Treatment Property aluminium powder；The modified glass powder is glass powder by ammonium hydroxide and silane coupling agent KH-602 Combined Treatment and is milled to 60-200 The modification glass powder obtained after mesh.The quality of the aluminium powder, potassium permanganate, otoginsenoside, arginine and cocounut oil acyl diethanol amine Than being 5:0.4-2:0.1-1:0.3-0.6:0.5-2；The glass powder, ammonium hydroxide, silane coupling agent KH-602 mass ratio be 1: 0.2-0.6:0.1-0.3。
According to embodiment of the present invention, wherein the modified additive includes that mass ratio is 1:3.2 modified aluminium Powder and modified glass powder.
According to embodiment of the present invention, wherein include following components by weight：Cyanuric acid asphalt mixtures modified by epoxy resin 57-68 parts of rouge, 7-11 parts of perfluorinated sulfonic resin, 4-7.5 parts of 107 rubber powder, 2.8-5.3 parts of silicone powder, changes 13-17 parts of ACR resin Property 1.6-3.5 parts of additive, 3.2-6 parts of zinc dialkyl dithiophosphate, 3-4.5 parts of pyridine carboxylic acid magnesium, niacin butyl ester (3- pyridine Butyl formate) 4.6-7 parts, 7-13 parts of N- methyl -4- cyano benzylamine, 5-10 parts of cashew nut shell oil, 4-7 parts of heptadecyl imidazole quinoline, 2-4.4 parts of 2,3- difluoro phenyl boric acid, 3.6-7.2 parts of trioctyl trimellitate (TOTM), diisostearoyl ethylene titanate 2.5-6.2 Part, 5.7-8 parts of Polyethylene Glycol Oleate.
For this purpose, the present invention provides the preparation method of integrated circuit modified epoxy plastic packaging material, including following preparation step：
The first step：By tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oil Acid polyethylene glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 70-140 DEG C, stirring is mixed It closes 40-150 minutes, is evacuated to 0.1MPa vacuum degree hereinafter, being cooled to 30-50 DEG C, pyridine carboxylic acid magnesium and inclined benzene is then added Three sour three monooctyl esters, are stirred 1-3 hours, obtain material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, 90-130 DEG C is warming up to, stirs Mixing 30-80 minutes is mixed, is cooled to 70-90 DEG C, adds above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, It is stirred 1 hour or more, obtains material B；
Third step：It is cooled to 40-60 DEG C, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added It in above-mentioned material B, is mixed evenly, obtains material C；
4th step：Material C is put into double screw extruder, at a temperature of 160-230 DEG C, with the screw rod of 50-500rpm Revolving speed squeezes out, and cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
According to embodiment of the present invention, wherein in the first step, be warming up to 120 DEG C, be stirred 85 minutes.
According to embodiment of the present invention, wherein in second step, 110 DEG C are warming up to, is stirred 55 minutes, it is cold But to 85 DEG C.
According to embodiment of the present invention, wherein in the 4th step, at a temperature of 170-210 DEG C, with the spiral shell of 120rpm Bar revolving speed squeezes out.
Beneficial effects of the present invention are：
The linear expansion coefficient of modified epoxy plastic packaging material provided by the invention is low, is lower than 52 × 10-6K, bending strength are relatively up to 92MPa or more, at the same heat resisting temperature be higher than 272 DEG C, linear expansion coefficient, mechanical property and heat resistance reach one it is higher Level, it is of good reliability, the requirement of Electronic Encapsulating Technology can be met.
Specific embodiment
Below with reference to embodiment, present invention is further described in detail.The following examples are intended to illustrate the invention, but not For limiting the scope of the invention.
Embodiment 1
A kind of integrated circuit modified epoxy plastic packaging material includes by weight following components：Tricyanic epoxy resin 55 Part, 11 parts of ACR resin, 6 parts of perfluorinated sulfonic resin, 3 parts of 107 rubber powder, 2 parts of silicone powder, modified 1 part of additive, dialkyl disulfides For 3 parts of trbasic zinc phosphate, 2 parts of pyridine carboxylic acid magnesium, 4 parts of niacin butyl ester (acidum nicotinicum butyl ester), 5 parts of N- methyl -4- cyano benzylamine, waist Shell oil 4 parts, 2 parts of heptadecyl imidazole quinoline, 1 part of 2,3- difluoro phenyl boric acid, 3-8 parts of trioctyl trimellitate (TOTM), two iso stearyls 2 parts of metatitanic acid second diester, 5 parts of Polyethylene Glycol Oleate；
The modified additive includes that mass ratio is 1:2 modified aluminium powder and modified glass powder.
The modified aluminium powder first passes through potassium permanganate for aluminium powder and handles and dry, using otoginsenoside, arginine and coconut palm The modified aluminium powder obtained after 50-150 mesh is milled to after oleoyl diethanol amine Combined Treatment；The modified glass powder is glass powder warp It crosses ammonium hydroxide and silane coupling agent KH-602 Combined Treatment and is milled to the modification glass powder obtained after 60-200 mesh.
The aluminium powder, potassium permanganate, otoginsenoside, arginine and cocounut oil acyl diethanol amine mass ratio be 5:0.4:0.1: 0.3:0.5；The glass powder, ammonium hydroxide, silane coupling agent KH-602 mass ratio be 1:0.2:0.1.
The preparation method of said integrated circuit modified epoxy plastic packaging material, including following preparation step：
The first step：By tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oil Acid polyethylene glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 70 DEG C, are stirred 40 Minute, 0.1MPa vacuum degree is evacuated to hereinafter, being cooled to 30 DEG C, and pyridine carboxylic acid magnesium and trioctyl trimellitate (TOTM) is then added, It is stirred 1 hour, obtains material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, are warming up to 90 DEG C, stirring is mixed It closes 30 minutes, is cooled to 70 DEG C, add above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, it is small to be stirred 1 When more than, obtain material B；
Third step：It is cooled to 40-60 DEG C, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added It in above-mentioned material B, is mixed evenly, obtains material C；
4th step：Material C is put into double screw extruder, at a temperature of 160-230 DEG C, with the screw speed of 50rpm It squeezes out, cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
Embodiment 2
A kind of integrated circuit modified epoxy plastic packaging material includes by weight following components：Tricyanic epoxy resin 70 Part, 20 parts of ACR resin, 13 parts of perfluorinated sulfonic resin, 8 parts of 107 rubber powder, 6 parts of silicone powder, modified 4 parts of additive, dialkyl disulfides For 7 parts of trbasic zinc phosphate, 5 parts of pyridine carboxylic acid magnesium, 8 parts of niacin butyl ester (acidum nicotinicum butyl ester), 15 parts of N- methyl -4- cyano benzylamine, 12 parts of cashew nut shell oil, 8 parts of heptadecyl imidazole quinoline, 5 parts of 2,3- difluoro phenyl boric acid, 8 parts of trioctyl trimellitate (TOTM), two iso stearyls 7 parts of metatitanic acid second diester, 9 parts of Polyethylene Glycol Oleate；
The modified additive includes that mass ratio is 1:5 modified aluminium powder and modified glass powder.
The modified aluminium powder first passes through potassium permanganate for aluminium powder and handles and dry, using otoginsenoside, arginine and coconut palm The modified aluminium powder obtained after 50-150 mesh is milled to after oleoyl diethanol amine Combined Treatment；The modified glass powder is glass powder warp It crosses ammonium hydroxide and silane coupling agent KH-602 Combined Treatment and is milled to the modification glass powder obtained after 60-200 mesh.
The aluminium powder, potassium permanganate, otoginsenoside, arginine and cocounut oil acyl diethanol amine mass ratio be 5:2:1:0.6: 2；The glass powder, ammonium hydroxide, silane coupling agent KH-602 mass ratio be 1:0.6:0.3.
The preparation method of said integrated circuit modified epoxy plastic packaging material, including following preparation step：
The first step：By tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oil Acid polyethylene glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 140 DEG C, are stirred 150 minutes, 0.1MPa vacuum degree was evacuated to hereinafter, being cooled to 50 DEG C, pyridine carboxylic acid magnesium then is added and tri trimellitate is pungent Ester is stirred 3 hours, obtains material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, are warming up to 130 DEG C, stirring is mixed It closes 80 minutes, is cooled to 90 DEG C, add above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, it is small to be stirred 1 When more than, obtain material B；
Third step：60 DEG C are cooled to, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added It states in material B, is mixed evenly, obtain material C；
4th step：Material C is put into double screw extruder, at a temperature of 160-230 DEG C, with the screw speed of 500rpm It squeezes out, cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
Embodiment 3
A kind of integrated circuit modified epoxy plastic packaging material includes by weight following components：Tricyanic epoxy resin 57 Part, 13 parts of ACR resin, 7 parts of perfluorinated sulfonic resin, 4 parts of 107 rubber powder, 2.8 parts of silicone powder, modified 1.6 parts of additive, dialkyl group 3.2 parts of zinc dithiophosphate, 3 parts of pyridine carboxylic acid magnesium, 4.6 parts of niacin butyl ester (acidum nicotinicum butyl ester), N- methyl -4- cyano benzyl 7 parts of amine, 5 parts of cashew nut shell oil, 4 parts of heptadecyl imidazole quinoline, 2 parts of 2,3- difluoro phenyl boric acid, 3.6 parts of trioctyl trimellitate (TOTM), two 2.5 parts, 5.7 parts of Polyethylene Glycol Oleate of iso stearyl metatitanic acid second diester；
The modified additive includes that mass ratio is 1:3.5 modified aluminium powder and modified glass powder.
The modified aluminium powder first passes through potassium permanganate for aluminium powder and handles and dry, using otoginsenoside, arginine and coconut palm The modified aluminium powder obtained after 50-150 mesh is milled to after oleoyl diethanol amine Combined Treatment；The modified glass powder is glass powder warp It crosses ammonium hydroxide and silane coupling agent KH-602 Combined Treatment and is milled to the modification glass powder obtained after 60-200 mesh.
The aluminium powder, potassium permanganate, otoginsenoside, arginine and cocounut oil acyl diethanol amine mass ratio be 5:1.2:0.5: 0.5:1.2；The glass powder, ammonium hydroxide, silane coupling agent KH-602 mass ratio be 1:0.4:0.12.
The preparation method of said integrated circuit modified epoxy plastic packaging material, including following preparation step：
The first step：By tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oil Acid polyethylene glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 110 DEG C, are stirred 65 minutes, 0.1MPa vacuum degree was evacuated to hereinafter, being cooled to 45 DEG C, pyridine carboxylic acid magnesium then is added and tri trimellitate is pungent Ester is stirred 2 hours, obtains material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, are warming up to 110 DEG C, stirring is mixed It closes 55 minutes, is cooled to 65 DEG C, add above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, it is small to be stirred 1 When more than, obtain material B；
Third step：55 DEG C are cooled to, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added It states in material B, is mixed evenly, obtain material C；
4th step：Material C is put into double screw extruder, at a temperature of 160-230 DEG C, with the screw speed of 200rpm It squeezes out, cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
Embodiment 4
A kind of integrated circuit modified epoxy plastic packaging material includes by weight following components：Tricyanic epoxy resin 68 Part, 17 parts of ACR resin, 11 parts of perfluorinated sulfonic resin, 7.5 parts of 107 rubber powder, 5.3 parts of silicone powder, modified 3.5 parts of additive, dioxane 6 parts of base zinc dithiophosphate, 4.5 parts of pyridine carboxylic acid magnesium, 7 parts of niacin butyl ester (acidum nicotinicum butyl ester), N- methyl -4- cyano benzyl 13 parts of amine, 10 parts of cashew nut shell oil, 7 parts of heptadecyl imidazole quinoline, 4.4 parts of 2,3- difluoro phenyl boric acid, trioctyl trimellitate (TOTM) 7.2 Part, 6.2 parts of diisostearoyl ethylene titanate, 8 parts of Polyethylene Glycol Oleate；
The modified additive includes that mass ratio is 1:4 modified aluminium powder and modified glass powder.
The modified aluminium powder first passes through potassium permanganate for aluminium powder and handles and dry, using otoginsenoside, arginine and coconut palm The modified aluminium powder obtained after 50-150 mesh is milled to after oleoyl diethanol amine Combined Treatment；The modified glass powder is glass powder warp It crosses ammonium hydroxide and silane coupling agent KH-602 Combined Treatment and is milled to the modification glass powder obtained after 60-200 mesh.
The aluminium powder, potassium permanganate, otoginsenoside, arginine and cocounut oil acyl diethanol amine mass ratio be 5:0.9:0.4: 0.5:1.3；The glass powder, ammonium hydroxide, silane coupling agent KH-602 mass ratio be 1:0.4:0.15.
The preparation method of said integrated circuit modified epoxy plastic packaging material, including following preparation step：
The first step：By tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oil Acid polyethylene glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 130 DEG C, are stirred 85 minutes, 0.1MPa vacuum degree was evacuated to hereinafter, being cooled to 45 DEG C, pyridine carboxylic acid magnesium then is added and tri trimellitate is pungent Ester is stirred 2 hours, obtains material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, are warming up to 120 DEG C, stirring is mixed It closes 75 minutes, is cooled to 80 DEG C, add above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, it is small to be stirred 1 When more than, obtain material B；
Third step：58 DEG C are cooled to, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added It states in material B, is mixed evenly, obtain material C；
4th step：Material C is put into double screw extruder, at a temperature of 160-230 DEG C, with the screw speed of 150rpm It squeezes out, cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
Embodiment 5
A kind of integrated circuit modified epoxy plastic packaging material includes by weight following components：Tricyanic epoxy resin 62 Part, 15 parts of ACR resin, 9 parts of perfluorinated sulfonic resin, 5.5 parts of 107 rubber powder, 2.8-5.3 parts of silicone powder, modified 2.5 parts of additive, 4.6 parts of zinc dialkyl dithiophosphate, 3.7 parts of pyridine carboxylic acid magnesium, 5.8 parts of niacin butyl ester (acidum nicotinicum butyl ester), N- methyl- 10 parts of 4- cyano benzylamine, 7.5 parts of cashew nut shell oil, 5.5 parts of heptadecyl imidazole quinoline, 3.2 parts of 2,3- difluoro phenyl boric acid, trimellitic acid Three 5.4 parts of monooctyl esters, 4.3 parts of diisostearoyl ethylene titanate, 6.8 parts of Polyethylene Glycol Oleate；
The modified additive includes that mass ratio is 1:3.2 modified aluminium powder and modified glass powder.
The modified aluminium powder first passes through potassium permanganate for aluminium powder and handles and dry, using otoginsenoside, arginine and coconut palm The modified aluminium powder obtained after 50-150 mesh is milled to after oleoyl diethanol amine Combined Treatment；The modified glass powder is glass powder warp It crosses ammonium hydroxide and silane coupling agent KH-602 Combined Treatment and is milled to the modification glass powder obtained after 60-200 mesh.
The aluminium powder, potassium permanganate, otoginsenoside, arginine and cocounut oil acyl diethanol amine mass ratio be 5:0.8:0.6: 0.4:1.3；The glass powder, ammonium hydroxide, silane coupling agent KH-602 mass ratio be 1:0.4:0.2.
The preparation method of said integrated circuit modified epoxy plastic packaging material, including following preparation step：
The first step：By tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oil Acid polyethylene glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 120 DEG C, are stirred 85 minutes, 0.1MPa vacuum degree was evacuated to hereinafter, being cooled to 40 DEG C, pyridine carboxylic acid magnesium then is added and tri trimellitate is pungent Ester is stirred 3 hours, obtains material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, are warming up to 110 DEG C, stirring is mixed It closes 55 minutes, adds above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, be stirred 1 hour or more, obtain Material B；
Third step：52 DEG C are cooled to, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added It states in material B, is mixed evenly, obtain material C；
4th step：Material C is put into double screw extruder, at a temperature of 170-210 DEG C, with the screw speed of 120rpm It squeezes out, cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
Comparative example 1
It is only that in place of this comparative example and the difference of embodiment 1：It does not include niacin butyl ester (acidum nicotinicum butyl ester), N- first Base -4- cyano benzylamine and its correlation step, and modified additive only includes modified aluminium powder.The specific raw material components of this comparative example and Its match, with and preparation method thereof with embodiment 1, do not repeating herein.
Comparative example 2
It is only that in place of this comparative example and the difference of embodiment 1：Do not include pyridine carboxylic acid magnesium, 2,3- difluoro phenyl boric acid, change Property additive and its correlation step.The specific raw material components and its proportion of this comparative example, with and preparation method thereof with embodiment 1, It is not repeating herein.
Performance test
The epoxy-plastic packaging material prepared to above embodiments and comparative example carries out correlated performance test according to professional standard, surveys Test result is：
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Comparative example 1 Comparative example 2
Linear expansion coefficient (× 10-6K) 51.6 52.3 47.5 49.3 46.1 58.7 64.3
Bending strength (MPa) 92.5 104.1 116.4 124.2 131.8 78.3 56.2
Heat resisting temperature/DEG C 272 283 276 281 279 254 241
The linear expansion coefficient of modified epoxy plastic packaging material provided by the invention is low it can be seen from the above test result, is lower than 52×10-6K, bending strength relatively up to 92MPa or more, while heat resisting temperature is higher than 272 DEG C, linear expansion coefficient, mechanical property Reach a higher level with heat resistance, it is of good reliability, the requirement of Electronic Encapsulating Technology can be met.

Claims (9)

1. a kind of modified additive, which is characterized in that including mass ratio be 1:The modified aluminium powder of 2-5 and modified glass powder, it is described Modified aluminium powder first passes through potassium permanganate for aluminium powder and handles and dry, using otoginsenoside, arginine and cocounut oil acyl diethanol amine It is obtained after being milled to 50-150 mesh after Combined Treatment；The modified glass powder is that glass powder passes through ammonium hydroxide and silane coupling agent KH- 602 Combined Treatments simultaneously obtain after being milled to 60-200 mesh.
2. modified additive according to claim 1, which is characterized in that the aluminium powder, potassium permanganate, otoginsenoside, essence The mass ratio of propylhomoserin and cocounut oil acyl diethanol amine is 5:0.4-2:0.1-1:0.3-0.6:0.5-2；The glass powder, ammonium hydroxide, silicon The mass ratio of alkane coupling agent KH-602 is 1:0.2-0.6:0.1-0.3.
3. modified additive according to claim 1, which is characterized in that the modified additive includes that mass ratio is 1: 3.2 modified aluminium powder and modified glass powder.
4. a kind of modified epoxy plastic packaging material using modified additive as described in claim 1, which is characterized in that by weight Meter includes following components：55-70 parts of tricyanic epoxy resin, 11-20 parts of ACR resin, 6-13 parts of perfluorinated sulfonic resin, 107 3-8 parts of rubber powder, 2-6 parts of silicone powder, modified additive 1-4 parts, 3-7 parts of zinc dialkyl dithiophosphate, pyridine carboxylic acid magnesium 2-5 Part, 4-8 parts of niacin butyl ester (acidum nicotinicum butyl ester), 5-15 parts of N- methyl -4- cyano benzylamine, 4-12 parts of cashew nut shell oil, 17 2-8 parts of alkyl imidazoline, 1-5 parts of 2,3- difluoro phenyl boric acid, 3-8 parts of trioctyl trimellitate (TOTM), two isostearoyl base metatitanic acid second two 2-7 parts of ester, 5-9 parts of Polyethylene Glycol Oleate.
5. modified epoxy plastic packaging material according to claim 4, which is characterized in that include following components by weight：Three 57-68 parts of paracyanogen acid epoxy resin, 13-17 parts of ACR resin, 7-11 parts of perfluorinated sulfonic resin, 4-7.5 parts of 107 rubber powder, silicone powder 2.8-5.3 parts, modified additive 1.6-3.5 parts, 3.2-6 parts of zinc dialkyl dithiophosphate, 3-4.5 parts of pyridine carboxylic acid magnesium, cigarette 4.6-7 parts of acid butyl ester (acidum nicotinicum butyl ester), 7-13 parts of N- methyl -4- cyano benzylamine, 5-10 parts of cashew nut shell oil, heptadecyl 4-7 parts of imidazoline, 2-4.4 parts of 2,3- difluoro phenyl boric acid, 3.6-7.2 parts of trioctyl trimellitate (TOTM), two isostearoyl base metatitanic acid second 2.5-6.2 parts of diester, 5.7-8 parts of Polyethylene Glycol Oleate.
6. according to claim 4, the preparation method of 5 described in any item modified epoxy plastic packaging materials, which is characterized in that including following Preparation step：
The first step：Tricyanic epoxy resin, niacin butyl ester (acidum nicotinicum butyl ester), 2,3- difluoro phenyl boric acid, oleic acid is poly- Glycol ester, silicone powder and diisostearoyl ethylene titanate are added in reactor, are warming up to 70-140 DEG C, are stirred 40-150 minutes, 0.1MPa vacuum degree was evacuated to hereinafter, being cooled to 30-50 DEG C, pyridine carboxylic acid magnesium and inclined benzene three is then added Sour three monooctyl esters, are stirred 1-3 hours, obtain material A；
Second step：ACR resin, perfluorinated sulfonic resin and 107 rubber powders are placed in reaction kettle, are warming up to 90-130 DEG C, stirring is mixed It closes 30-80 minutes, is cooled to 70-90 DEG C, add above-mentioned material A, modified additive, zinc dialkyl dithiophosphate, stirring Mixing 1 hour or more, obtain material B；
Third step：It is cooled to 40-60 DEG C, N- methyl -4- cyano benzylamine, cashew nut shell oil and heptadecyl imidazole quinoline are added above-mentioned It in material B, is mixed evenly, obtains material C；
4th step：Material C is put into double screw extruder, at a temperature of 160-230 DEG C, with the screw speed of 50-500rpm It squeezes out, cooling granulation is up to integrated circuit modified epoxy plastic packaging material.
7. the preparation method of modified epoxy plastic packaging material according to claim 6, which is characterized in that in the first step, be warming up to It 120 DEG C, is stirred 85 minutes.
8. the preparation method of modified epoxy plastic packaging material according to claim 6, which is characterized in that in second step, be warming up to It 110 DEG C, is stirred 55 minutes, is cooled to 85 DEG C.
9. the preparation method of modified epoxy plastic packaging material according to claim 6, which is characterized in that in the 4th step, in 170- At a temperature of 210 DEG C, squeezed out with the screw speed of 120rpm.
CN201810632063.7A 2016-08-26 2016-08-26 A kind of modified additive, modified epoxy plastic packaging material and preparation method thereof Pending CN108892926A (en)

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Application publication date: 20181127