CN1590498A - Liquid epoxy packaging material and its preparation method and application - Google Patents
Liquid epoxy packaging material and its preparation method and application Download PDFInfo
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- CN1590498A CN1590498A CN 03157937 CN03157937A CN1590498A CN 1590498 A CN1590498 A CN 1590498A CN 03157937 CN03157937 CN 03157937 CN 03157937 A CN03157937 A CN 03157937A CN 1590498 A CN1590498 A CN 1590498A
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- epoxy
- liquid epoxy
- resins
- encapsulating compound
- liquid
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 74
- 239000007788 liquid Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000005022 packaging material Substances 0.000 title 1
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 238000004377 microelectronic Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims abstract description 3
- 150000001875 compounds Chemical class 0.000 claims description 35
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- 239000012764 mineral filler Substances 0.000 claims description 19
- -1 4-epoxycyclohexyl methyl Chemical group 0.000 claims description 17
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 17
- 229920000647 polyepoxide Polymers 0.000 claims description 14
- 239000003822 epoxy resin Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 238000009775 high-speed stirring Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229930185605 Bisphenol Natural products 0.000 claims description 10
- 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 description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 8
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000012756 surface treatment agent Substances 0.000 claims description 6
- 150000008065 acid anhydrides Chemical class 0.000 claims description 5
- UIDDPPKZYZTEGS-UHFFFAOYSA-N 3-(2-ethyl-4-methylimidazol-1-yl)propanenitrile Chemical compound CCC1=NC(C)=CN1CCC#N UIDDPPKZYZTEGS-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 229960001866 silicon dioxide Drugs 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 4
- WTYYGFLRBWMFRY-UHFFFAOYSA-N 2-[6-(oxiran-2-ylmethoxy)hexoxymethyl]oxirane Chemical compound C1OC1COCCCCCCOCC1CO1 WTYYGFLRBWMFRY-UHFFFAOYSA-N 0.000 claims description 3
- XDKUKGIJDNUFGK-UHFFFAOYSA-N 4-methylimidazole Chemical compound CC1=CN=C[N]1 XDKUKGIJDNUFGK-UHFFFAOYSA-N 0.000 claims description 3
- OXQXGKNECHBVMO-UHFFFAOYSA-N 7-oxabicyclo[4.1.0]heptane-4-carboxylic acid Chemical compound C1C(C(=O)O)CCC2OC21 OXQXGKNECHBVMO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- BFHIGGJUBGXSIG-UHFFFAOYSA-N C(C1CO1)OC(C1C(C(=O)O)C=CCC1)=O Chemical compound C(C1CO1)OC(C1C(C(=O)O)C=CCC1)=O BFHIGGJUBGXSIG-UHFFFAOYSA-N 0.000 claims description 3
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 3
- 150000002118 epoxides Chemical group 0.000 claims description 3
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims description 3
- KILURZWTCGSYRE-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]alumanyloxypent-3-en-2-one Chemical compound CC(=O)\C=C(\C)O[Al](O\C(C)=C/C(C)=O)O\C(C)=C/C(C)=O KILURZWTCGSYRE-LNTINUHCSA-K 0.000 claims description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 2-phenyl-1h-imidazole Chemical compound C1=CNC(C=2C=CC=CC=2)=N1 ZCUJYXPAKHMBAZ-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- LSZVXYBAQNQHCW-UHFFFAOYSA-N 3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione;2-benzofuran-1,3-dione Chemical compound C1CCCC2C(=O)OC(=O)C21.C1=CC=C2C(=O)OC(=O)C2=C1 LSZVXYBAQNQHCW-UHFFFAOYSA-N 0.000 claims description 2
- TYOXIFXYEIILLY-UHFFFAOYSA-N 5-methyl-2-phenyl-1h-imidazole Chemical compound N1C(C)=CN=C1C1=CC=CC=C1 TYOXIFXYEIILLY-UHFFFAOYSA-N 0.000 claims description 2
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 2
- LCKKYSBLGICEAB-UHFFFAOYSA-N N(C1=CC=CC=C1)C[SiH2]OCC Chemical compound N(C1=CC=CC=C1)C[SiH2]OCC LCKKYSBLGICEAB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- SSQIOAPXYBWOKP-UHFFFAOYSA-N [Nd].C(C)C(=O)C(=O)C Chemical compound [Nd].C(C)C(=O)C(=O)C SSQIOAPXYBWOKP-UHFFFAOYSA-N 0.000 claims description 2
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 2
- SZKXDURZBIICCF-UHFFFAOYSA-N cobalt;pentane-2,4-dione Chemical compound [Co].CC(=O)CC(C)=O SZKXDURZBIICCF-UHFFFAOYSA-N 0.000 claims description 2
- 229940015043 glyoxal Drugs 0.000 claims description 2
- 150000002460 imidazoles Chemical class 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 239000008393 encapsulating agent Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 10
- 238000005538 encapsulation Methods 0.000 abstract description 8
- 238000011049 filling Methods 0.000 abstract description 4
- 230000009477 glass transition Effects 0.000 abstract description 4
- 150000008064 anhydrides Chemical class 0.000 abstract description 2
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 abstract description 2
- 239000011256 inorganic filler Substances 0.000 abstract 2
- 229910003475 inorganic filler Inorganic materials 0.000 abstract 2
- 239000006087 Silane Coupling Agent Substances 0.000 abstract 1
- 238000005452 bending Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 16
- 230000004927 fusion Effects 0.000 description 12
- 239000011863 silicon-based powder Substances 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 239000000758 substrate Substances 0.000 description 6
- CSHJJWDAZSZQBT-UHFFFAOYSA-N 7a-methyl-4,5-dihydro-3ah-2-benzofuran-1,3-dione Chemical class C1=CCCC2C(=O)OC(=O)C21C CSHJJWDAZSZQBT-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- AJHFBIPDUISYDU-UHFFFAOYSA-N 2-(2-ethyl-5-methyl-1h-imidazol-4-yl)propanenitrile Chemical class CCC1=NC(C(C)C#N)=C(C)N1 AJHFBIPDUISYDU-UHFFFAOYSA-N 0.000 description 1
- 150000008614 2-methylimidazoles Chemical class 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910021488 crystalline silicon dioxide Inorganic materials 0.000 description 1
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- MUTGBJKUEZFXGO-UHFFFAOYSA-N hexahydrophthalic anhydride Chemical class C1CCCC2C(=O)OC(=O)C21 MUTGBJKUEZFXGO-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000012536 packaging technology Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
本发明公开了一种适用于FC－BGA/CSP等高密度微电子封装用的高纯度、高填充量、低粘度、高流动性、高耐热液体环氧封装料，该封装料包括重量份数100份的两种类型的液体环氧树脂；50－150份的酸酐固化剂；0.5－5.0份的固化促进剂；0.5－5.0份的硅烷偶联剂；300－600份的两种不同粒径的无机填料。本发明所述的液体环氧封装料，其特征在于所述的液体环氧封装料在无机填料添加量达到65－75％时仍然具有较低的粘度(25℃时绝对粘度可低达3000－4000mPas)；树脂经适当工艺固化后形成的树脂固化物具有较低热膨胀系数(低达25ppm/℃)、高玻璃化温度(可高达240℃)以及优良的力学性能(弯曲强度可达92MPa)等，可以满足FC－BGA/CSP等高密度微电子封装的需要。The invention discloses a high-purity, high-filling, low-viscosity, high-fluidity, high-heat-resistant liquid epoxy encapsulation material suitable for high-density microelectronic packaging such as FC-BGA/CSP. The encapsulation material includes parts by weight 100 parts of two types of liquid epoxy resin; 50-150 parts of anhydride curing agent; 0.5-5.0 parts of curing accelerator; 0.5-5.0 parts of silane coupling agent; 300-600 parts of two different particles diameter inorganic fillers. The liquid epoxy encapsulant of the present invention is characterized in that the liquid epoxy encapsulant still has a relatively low viscosity when the amount of inorganic filler added reaches 65-75% (the absolute viscosity can be as low as 3000-3000-25°C). 4000mPas); the cured resin formed after the resin is cured by an appropriate process has a low thermal expansion coefficient (as low as 25ppm/°C), a high glass transition temperature (up to 240°C) and excellent mechanical properties (bending strength up to 92MPa), etc. , can meet the needs of high-density microelectronic packaging such as FC-BGA/CSP.
Description
Technical field
The present invention relates to a kind of high purity, high filler loading capacity, low viscosity, high workability, high heat-resisting liquid epoxy encapsulating compound.
The invention still further relates to the preparation method of above-mentioned encapsulating compound.
Encapsulating compound of the present invention is applicable to the high-density microelectronics Packaging.
Background technology
In recent years, microelectronic packaging technology develops to little, light, thin direction, the various packing forms of suitable SMT, go between (TQFP), ball type array (BGA), the development of wafer-level package packing forms such as (CSP) rapidly as flat four limits lead-in wires (QFP), slim flat four limits, and especially upside-down mounting welding core (FC)-BGA/CSP has become the technology focus that recent people pay close attention to.FC-BGA/CSP is the highest a kind of packing forms of present packaging density, and the number of pins of every chip block can reach 1681, is particularly suitable for cableless communication, notebook computer etc. and requires little, light, the thin Application Areas of chip.
Material filling at the bottom of the liquid epoxy (Underfill) is the key material of FC-BGA/CSP; it is filled in the slit that is formed by miniature soldered ball between upside-down mounting welding core and the organic substrate; its main purpose is the strength of joint that strengthens chip and substrate; protect miniature soldered ball to avoid external pollution; reduce the stress of packaging, improve the work-ing life of device.Therefore, require that material filling (Underfill) is the good liquid of flowing property at normal temperatures at the bottom of the liquid epoxy; Because the slit between chip and the substrate is very narrow (general＜as 0.05mm), need low viscosity, high capillary liquid epoxy encapsulating compound to be filled into the slit between chip and the substrate fast by capillary osmosis.Except low viscosity, also require epoxy encapsulant to have high heat-resisting, high glass-transition temperature, low thermal coefficient of expansion, good mechanical property and characteristics such as anti-cracking performance and low water absorption.In addition, because FC-BGA/CSP is the encapsulation that is close to bare chip, therefore require encapsulating compound to have very high purity requirement.In order to reduce the internal stress that causes greatly owing to difference of thermal expansion coefficients between chip, soldered ball and the substrate, need in epoxy encapsulant, add the mineral filler of 65-75%, to reduce its thermal expansivity to greatest extent.But after mineral filler was increased to a certain degree, the viscosity of liquid encapsulation material can sharply increase, its mobile can decline significantly.Therefore solve the flowability of liquid encapsulation material and the contradiction of thermal expansivity becomes a guardian technique.
US Patent 6,117,953 disclose the preparation method of a kind of semi-conductor with the liquid epoxy encapsulating compound, and this liquid epoxy encapsulating compound is by bisphenol type epoxy and alicyclic epoxy and Resins, epoxy thereof, compositions such as anhydride curing agent, the second-order transition temperature of resin cured matter is 150-160 ℃ scope; US Patent6,365,649 disclose a kind of liquid epoxy encapsulating compound; Because the substrate ring epoxy resin system viscosity of selecting for use is big, causes the viscosity of encapsulating compound higher, the viscosity of liquid encapsulation material surpasses 4500mPas in the time of 50 ℃; US Patent 5,439,977 discloses a kind of epoxy encapsulant, and this encapsulating compound has shelf lives and flowability preferably, but the resistance toheat of resin cured matter is low, and second-order transition temperature has only 100-110 ℃.
Summary of the invention
The object of the present invention is to provide a kind of high purity, high filler loading capacity, low viscosity, high workability, high heat-resisting liquid epoxy encapsulating compound, this liquid epoxy encapsulating compound have very high purity (＞98%), the foreign metal ion comprises that sodium, potassium, iron, zinc, aluminium, copper, chlorine, bromine, iodine plasma content all are lower than 3-5ppm; When the loading level of mineral filler surpassed 65-70%, liquid encapsulation material still had good mobile filling properties.
Another object of the present invention is to provide the preparation method of above-mentioned encapsulating compound.
Liquid epoxy encapsulating compound of the present invention is characterized in that described liquid epoxy encapsulating compound comprises following component:
The component weight percentage
Resins, epoxy A 0-100
Resins, epoxy B 100-0
Solidifying agent 50-150
Curing catalyst 0.5-5.0
Surface treatment agent 0.5-5.0
Mineral filler 300-600
The preparation method of liquid epoxy encapsulating compound of the present invention is characterized in that described liquid epoxies preparation process is:
After Resins, epoxy A and Resins, epoxy B evenly be 100 parts by the arbitrary proportion thorough mixing,, under mechanical stirring, mix, obtain the liquid of homogeneous phase transparent with 50-100 part epoxy curing agent, 0.5-5.0 part curing catalyst, 0.5-5.0 part surface treatment agent.Under high-speed stirring, 300-600 part mineral filler gradation is added in the aforesaid liquid, continue then to stir 30 minutes, obtain finely dispersed liquid epoxy encapsulating compound.
Liquid epoxy encapsulating compound of the present invention is characterized in that described Resins, epoxy A means and is the cycloaliphatic epoxy resin of liquid under the normal temperature, comprises 3,4-epoxy cyclohexane carboxylic acid 3, and 4-epoxycyclohexyl methyl ester (shown in structure I),
Or two-(2, the 3-epoxycyclohexyl) ethers (shown in structure I I);
R=-O-wherein ,-O-(CH
2)
m-O-, m=1-3; When R=-O-, be two-(2, the 3-epoxycyclohexyl) ether.
Above-mentioned Resins, epoxy can use separately, also can mix use by arbitrary proportion.
Liquid epoxy encapsulating compound of the present invention is characterized in that described Resins, epoxy B means under the normal temperature and comprises 1 for the Resins, epoxy of liquid) the bisphenol A-type diglycidyl ether epoxy resin; 2) Bisphenol F type diglycidyl ether epoxy resin; 3) other glycidyl ethers (fat) type Resins, epoxy: tetrahydrophthalic acid 2-glycidyl ester, 1,6 hexanediol diglycidyl ether, trihydroxymethylpropanyltri diglycidyl ether.Above-mentioned Resins, epoxy can use separately, and mixture that also can two or more many arbitrary proportions uses.
Liquid epoxy encapsulating compound of the present invention is characterized in that described solidifying agent comprises that methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, hexahydrophthalic anhydride phthalic anhydride, methyl are received and repeatedly restrains acid anhydrides or the siliceous organic dianhydride shown in structure III.These solidifying agent can use separately or use with two or more mixture.The equivalence ratio of acid anhydrides and epoxide group is 0.6-1.0, is preferably 0.7-0.9.
N=1-100 wherein; When n=1, be 5,5 '-(1,1,3,3-tetramethyl--1, two replacements of 3-sily oxide)-two-norbornylene-2, the 3-dianhydride.
Liquid epoxy encapsulating compound of the present invention, it is characterized in that described curing catalyst comprises imidazoles, glyoxal ethyline, 2,4-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 1,3,5-triethyl-six hydrogen-S-triazine, 1,3,5-trimethylammonium-six hydrogen-S-triazine, triethylamine, triphenylphosphine, triethyl phosphine, acetylacetone cobalt, ferric acetyl acetonade, acetylacetonate nickel, methyl ethyl diketone neodymium or aluminium acetylacetonate.These promotor can be used separately, also can use by the mixture of arbitrary proportion more than 2 kinds or 2 kinds.
Liquid epoxy encapsulating compound of the present invention, it is characterized in that the interfacial interaction that described surface treatment agent means can be increased between mineral filler and the Resins, epoxy, improve the organic compound and composition thereof of both consistencies, comprise Racemic glycidol oxygen propyl trimethoxy silicane, γ-An Jibingjisanyiyangjiguiwan, γ-mercaptan aminopropyl trimethoxysilane, anilinomethyl Ethoxysilane or 3,4-epoxy cyclohexane propyl trimethoxy silicane.
Liquid epoxy resin composition of the present invention also further comprises the carbon black of parts by weight 0.1-5.0 part, can be used as dyestuff and uses.
Liquid epoxy encapsulating compound of the present invention is characterized in that described mineral filler maximum particle diameter is above 20 microns.Preferably form by fused preparing spherical SiO 2, fused dihedral silicon-dioxide, crystalline silicon-dioxide, synthetic silicon-dioxide, aluminum oxide, silicon nitride or the boron nitride of two kinds of different-grain diameters.Wherein the median size of mineral filler 1 is in the scope of 0.10-5.0 micron, and its weight content accounts for the 5-80% of mineral filler total amount, and in the scope of the median size 3-10 micron of another kind of mineral filler 2, its weight content accounts for 95-20%.
Liquid epoxy encapsulating compound of the present invention is characterized in that described liquid epoxy encapsulating compound still has lower viscosity (25 ℃ time absolute viscosity can hang down reach 3000-4000mPas) when the mineral filler addition reaches 65-75%; Resin solidifies resin cured matter that the back forms through suitable technology and has relatively low thermel expansion coefficient (hang down and reach 25ppm/ ℃), high glass transition temperature (can up to 240 ℃) and excellent mechanical property (flexural strength can reach 92MPa) etc., can satisfy the needs of high-density microelectronics Packaging such as FC-BGA/CSP.Table 1 is listed the physicals of representative formula resin and cured article.
The performance of table 1 typical liquid epoxy encapsulation material and resin cured matter thereof
| Viscosity cp, 25 ℃ | Body resistivity 10 16Ωcm | ????Tg ????℃ | ????CTE ????ppm/℃ | Flexural strength Mpa | Modulus in flexure Gpa | Water-intake rate % | |
| Prescription 1 | ????4300 | ????2.9 | ????214 | ????31 | ??76.9 | ??6.2 | ??0.41 |
| Prescription 2 | ????3500 | ????3.0 | ????216 | ????30 | ??88.3 | ??6.2 | ??0.40 |
| Prescription 3 | ????3300 | ????3.1 | ????205 | ????31 | ??82.5 | ??6.3 | ??0.42 |
| Prescription 4 | ????5900 | ????2.9 | ????208 | ????30 | ??68.0 | ??6.4 | ??0.48 |
| Prescription 5 | ????14000 | ????3.0 | ????240 | ????29 | ??80.5 | ??6.2 | ??0.51 |
| Prescription 6 | ????17000 | ????2.9 | ????235 | ????30 | ??82 | ??6.1 | ??0.48 |
| Prescription 7 | ????8800 | ????3.1 | ????204 | ????25 | ??75.7 | ??7.5 | ??0.38 |
| Prescription 8 | ????9200 | ????3.6 | ????198 | ????28 | ??92.3 | ??6.6 | ??0.43 |
| Prescription 9 | ????6600 | ????2.8 | ????178 | ????30 | ??75.5 | ??6.1 | ??0.40 |
| Prescription 10 | ????4150 | ????3.0 | ????204 | ????31 | ??78.2 | ??6.2 | ??0.42 |
The resin cured matter of encapsulating compound provided by the invention after suitably technology is solidified has characteristics such as height is heat-resisting, high glass-transition temperature, low thermal coefficient of expansion, low moisture absorption ratio, high electric insulation, low-k, low-dielectric loss, is suitable for high-density microelectronics Packaging such as FC-BGA/CSP.
Embodiment
Embodiment 1: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 90 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 10 weight part bisphenol A-type diglycidyl ether epoxy resin, 107 weight part methylhexahydrophthalic anhydrides, 1 weight part 2-methyl-imidazoles, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes, at room temperature stir, obtain homogeneous phase transparent liquid.Then, add 0.5 micron fusion ball-type of 80 weight part median sizes silicon powder, 4.2 microns fusion ball-shaped silicon micro powders of 310 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 2: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 80 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 10 parts two-(2, the 3-epoxycyclohexyl) ether, 10 weight part Bisphenol F type diglycidyl ether epoxy resin, 22 weight parts two-(2, the 3-epoxycyclohexyl) ether, 111 weight part methyl tetrahydrophthalic anhydrides, 1 weight part 2,4-methylimidazole, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes at room temperature stir, and obtain homogeneous phase transparent liquid.Then, add 0.5 micron of 20 weight part median size, 5.6 microns fused dihedrals of 378 weight part median sizes silicon powder successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 3: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 70 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 10 parts two-(2, the 3-epoxycyclohexyl) ether, 20 weight part bisphenol A-type diglycidyl ether epoxy resin, 60 weight part methyl tetrahydrophthalic anhydrides, 50 weight part methyl tetrahydrophthalic anhydrides, 2 weight part 2-ethyl-4-methylimidazoles, 2 weight part γ-An Jibingjisanyiyangjiguiwans, at room temperature stir, obtain homogeneous phase transparent liquid.Then, add 0.4 micron boron nitride of 80 weight part median sizes, 6.5 microns silicon powders of 318 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 4: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 45 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 40 parts two-(2, the 3-epoxycyclohexyl) ether, 5 weight part bisphenol A-type diglycidyl ether epoxy resin, 93 weight part hexahydrophthalic anhydrides, 18 weight parts 5,5 '-(1,1,3,3-tetramethyl--1,3-sily oxide two replaces)-two-norbornylene-2,3-dianhydride, 1 weight part 1-cyanoethyl-2-ethyl-4-methylimidazole, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes at room temperature stir, and obtain homogeneous phase transparent liquid.Then, add 1.2 microns fusion ball-types of 100 weight part median sizes silicon powder, 6.5 microns molten silicon micro mists of 298 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 5: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 80 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 10 parts two-(2, the 3-epoxycyclohexyl) ether, 10 weight part bisphenol A-type diglycidyl ether epoxy resin, 80 weight part methylhexahydrophthalic anhydrides, 37 weight parts 5,5 '-(1,1,3,3-tetramethyl--1,3-sily oxide two replaces)-two-norbornylene-2,3-dianhydride, 1 weight part 2-ethyl-4-methylimidazole, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes at room temperature stir, and obtain homogeneous phase transparent liquid.Then, add 1.2 microns fusion ball-types of 51 weight part median sizes silicon powder, 3.5 microns fusion ball-shaped silicon micro powders of 358 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 6: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 80 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 5 parts two-(2, the 3-epoxycyclohexyl) ether, 15 weight part bisphenol A-type diglycidyl ether epoxy resin, 79 weight part methylhexahydrophthalic anhydrides, 37 weight parts 5,5 '-(1,1,3,3-tetramethyl--1,3-sily oxide two replaces)-two-norbornylene-2,3-dianhydride, 1 weight part 1-cyanoethyl-2-ethyl-4-methylimidazole, 2 weight part γ-An Jibingjisanyiyangjiguiwans at room temperature stir, and obtain homogeneous phase transparent liquid.Then, add 164 weight part median sizes, 0.7 micrometer alumina, 6.5 microns silicon powders of 245 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 7: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 20 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 20 parts two-(2, the 3-epoxycyclohexyl) ether, 20 weight parts two-(2, the 3-epoxycyclohexyl) ether, 60 weight part bisphenol A-type diglycidyl ether epoxy resin, 111 weight part methylhexahydrophthalic anhydrides, 3 weight part 2-ethyl-4-methylimidazoles, 3 weight part Racemic glycidol oxygen propyl trimethoxy silicanes, at room temperature stir, obtain homogeneous phase transparent liquid.Then, add 0.4 micron fusion ball-type of 112 weight part median sizes silicon powder, 6.5 microns fusion ball-shaped silicon micro powders of 394 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 8: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 100 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 20 weight parts 1,6 hexanediol diglycidyl ether, 107 weight part methylhexahydrophthalic anhydrides, 1 weight part ferric acetyl acetonade, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes, at room temperature stir, obtain homogeneous phase transparent liquid.Then, add 1.2 microns fusion ball-types of 218 weight part median sizes silicon powder, 4.2 microns fusion ball-shaped silicon micro powders of 218 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 9: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 70 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 30 weight part bisphenol A-type diglycidyl ether epoxy resin, 105 weight part methyl tetrahydrophthalic anhydrides, 1 weight part 2-ethyl-4-methylimidazole, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes, at room temperature stir, obtain homogeneous phase transparent liquid.Then, add 2.5 microns fusion ball-types of 273 weight part median sizes silicon powder, 6.5 microns fusion ball-shaped silicon micro powders of 159 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Embodiment 10: in three mouthfuls of round-bottomed flasks of 1000ml, mechanical stirrer and feed hopper are installed.Add 70 weight parts 3,4-epoxy cyclohexane carboxylic acid 3,4-epoxycyclohexyl methyl ester, 30 weight part tetrahydrophthalic acid 2-glycidyl esters, 40 weight part methylhexahydrophthalic anhydrides, 40 weight part methyl tetrahydrophthalic anhydrides, 37 weight parts 5,5 '-(1,1,3,3-tetramethyl--1,3-sily oxide two replaces)-two-norbornylene-2,3-dianhydride, 2 weight part 1-cyanoethyl-2-ethyl-4-methylimidazoles, 2 weight part Racemic glycidol oxygen propyl trimethoxy silicanes, at room temperature stir, obtain homogeneous phase transparent liquid.Then, add 0.7 micron fusion ball-type of 164 weight part median sizes silicon powder, 6.5 microns silicon nitrides of 245 weight part median sizes successively, at room temperature high-speed stirring is 30 minutes, obtains finely dispersed thick liquid epoxy encapsulant.
Claims (11)
1, a kind of liquid epoxy encapsulating compound, percentage ratio meter by weight, described liquid epoxy encapsulating compound component ratio is: Resins, epoxy A, 0-100; Resins, epoxy B, 100-0; Solidifying agent, 50-150; Curing catalyst, 0.5-5.0; Surface treatment agent, 0.5-5.0; Mineral filler, 300-600;
Described Resins, epoxy A is 3,4-epoxy cyclohexane carboxylic acid 3, the mixture of 4-epoxycyclohexyl methyl ester, two-(2, the 3-epoxycyclohexyl) ether or both arbitrary proportions;
Wherein 3,4-epoxy cyclohexane carboxylic acid 3, the structure of 4-epoxycyclohexyl methyl ester is suc as formula shown in the I;
Wherein the structural formula of two-(2, the 3-epoxycyclohexyl) ether is suc as formula shown in the II;
Wherein R=-O-,-O-(CH
2)
m-O-, m=1-3;
Described Resins, epoxy B is: the mixture of bisphenol A-type diglycidyl ether epoxy resin, Bisphenol F type diglycidyl ether epoxy resin, other glycidyl ethers (fat) type Resins, epoxy or above-mentioned two or more arbitrary proportions;
Mineral filler is that 20 microns fused preparing spherical SiO 2 or dihedral silicon-dioxide, crystallization or synthetic silicon-dioxide, aluminum oxide, silicon nitride or boron nitride formed by maximum particle diameter;
2, liquid epoxy encapsulating compound as claimed in claim 1 is characterized in that, when R=-O-, is two-(2, the 3-epoxycyclohexyl) ether.
3, liquid epoxy encapsulating compound as claimed in claim 1, it is characterized in that, other glycidyl ethers (fat) type Resins, epoxy is among the described Resins, epoxy B: tetrahydrophthalic acid 2-glycidyl ester, 1,6 hexanediol diglycidyl ether or trihydroxymethylpropanyltri diglycidyl ether.
4, liquid epoxy encapsulating compound as claimed in claim 1 is characterized in that, described mineral filler is two kinds of different-grain diameters, and wherein the median size of mineral filler 1 is the 0.10-5.0 micron, and weight content accounts for the 5-80% of mineral filler total amount; The median size of mineral filler 2 is the 3-10 micron, and weight accounts for the 95-20% of mineral filler total amount.
5, a kind of method for preparing the described liquid epoxy encapsulating compound of claim 1, its preparation process is: with Resins, epoxy A with after Resins, epoxy B evenly becomes 100 parts by the arbitrary proportion thorough mixing, with 50-100 part epoxy curing agent, 0.5-5.0 part curing catalyst, 0.5-5.0 part surface treatment agent, under mechanical stirring, mix, obtain the liquid of homogeneous phase transparent; Under high-speed stirring, 300-600 part mineral filler gradation is added in the aforesaid liquid, continue then to stir 30 minutes, obtain finely dispersed liquid epoxy encapsulating compound.
6, preparation method as claimed in claim 5, it is characterized in that described solidifying agent is that methylhexahydrophthalic anhydride, methyl tetrahydrophthalic anhydride, hexahydrophthalic anhydride phthalic anhydride, methyl are received and repeatedly restrained acid anhydrides or the siliceous organic dianhydride shown in formula III;
N=1-100 wherein;
Above-mentioned solidifying agent can use separately or use with two or more mixture; The equivalence ratio of acid anhydrides and epoxide group is 0.6-1.0.
7, preparation method as claimed in claim 6 is characterized in that, the equivalence ratio of described acid anhydrides and epoxide group is 0.7-0.9.
8, preparation method as claimed in claim 6 is characterized in that, when the n=1 among the structural formula II I, is 5,5 '-(1,1,3,3-tetramethyl--1, two replacements of 3-sily oxide)-two-norbornylene-2, the 3-dianhydride.
9, preparation method as claimed in claim 5, it is characterized in that, described curing catalyst is: imidazoles, glyoxal ethyline, 2,4-methylimidazole, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2-phenyl-4-methylimidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole, 1,3,5-triethyl-six hydrogen-S-triazine, 1,3, the said mixture of 5-trimethylammonium-six hydrogen-S-triazine, triethylamine, triphenylphosphine, triethyl phosphine, acetylacetone cobalt, ferric acetyl acetonade, acetylacetonate nickel, methyl ethyl diketone neodymium or aluminium acetylacetonate and arbitrary proportion thereof.
10, preparation method as claimed in claim 5, it is characterized in that, described surface treatment agent is: Racemic glycidol oxygen propyl trimethoxy silicane, γ-An Jibingjisanyiyangjiguiwan, γ-mercaptan aminopropyl trimethoxysilane, anilinomethyl Ethoxysilane or 3,4-epoxy cyclohexane propyl trimethoxy silicane.
11, liquid epoxy encapsulating compound as claimed in claim 1 is in the application in microelectronics Packaging field.
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