Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, proposes a kind of composition epoxy resin of Flip-Chip Using.Meet and meet the high workability of Flip-Chip Using, and can meet the filling that occurs in encapsulated moulding process completely, the requirement of operability.
The technical problem to be solved in the present invention is achieved through the following technical solutions, and a kind of composition epoxy resin of Flip-Chip Using, is characterized in:
It comprises epoxy resin 5 ~ 30 mass parts, resol 5 ~ 20 mass parts, mineral filler 70 ~ 90 mass parts, fire retardant 1 ~ 10 mass parts, curing catalyst 0.5 ~ 2.5 mass parts, silane coupling agent 0.5 ~ 4.5 mass parts; After each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, and mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, pulverizes and make after cooling;
Wherein: epoxy resin adopts has low viscosity, high workability, the naphthalane-contained type of high glass transition temperature or biphenyl structural type epoxy resin;
Resol adopts the resol containing biphenyl structures or multiple hydroxyl structure with good mobility;
Mineral filler used is ball-shaped silicon micro powder, and its size-grade distribution D50 is 4 ~ 6 μm, and 60 ~ 75%, 6 ~ 12 μm of part silicon powders that 1 ~ 6 μm of part silicon powder accounts for total amount account for 20 ~ 25% of total amount.12 ~ 48 μm of part silicon powders account for 5 ~ 20% of total amount.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, and silane coupling agent used is epoxy radicals silicone hydride.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, when the Ratio control of the epoxy equivalent (weight) of epoxy resin and the hydroxyl equivalent of resol is in 0.8-1.3 scopes, composition epoxy resin, when shaping, shows good curing characteristics.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, releasing agent used be bar wax, polyethylene wax, stearic acid or montanin wax any one.
The technical problem to be solved in the present invention can also be come to realize further by the following technical programs, and described curing catalyst is: imidazoles or phosphorus species, comprises 2-methyl 4-phenyl imidazoles; Or be tertiary amine compound, comprise benzyldimethylamine, triethylamine benzyldimethylamine, 1,8-diazabicyclo (5,4,0) undecylene-7; Or be organic phosphine compound, comprise triphenylphosphine, tetraphenyl phosphine, three (p-methylphenyl) phosphine.
The present invention compared with prior art, well can fill 80 μm of gaps between flip chip integrated circuit chips and circuit card and coated ball salient point.The present invention is by selecting suitable silicon powder size-grade distribution, its size-grade distribution D50 is 4 ~ 6um, 1 ~ 6um part silicon powder accounts for 60 ~ 75% of total amount, 6 ~ 12um part silicon powder accounts for 20 ~ 25% of total amount, 12 ~ 48um part silicon powder accounts for 5 ~ 20% of total amount, can prepare the composition epoxy resin of the Flip-Chip Using of high workability and good fillibility.
Embodiment
A composition epoxy resin for Flip-Chip Using, it comprises epoxy resin 5 ~ 30 mass parts, resol 5 ~ 20 mass parts, mineral filler 70 ~ 90 mass parts, fire retardant 1 ~ 10 mass parts, curing catalyst 0.5 ~ 2.5 mass parts, silane coupling agent 0.5 ~ 4.5 mass parts; After each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, and mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, pulverizes and make after cooling;
Wherein: epoxy resin adopts has low viscosity, high workability, the naphthalane-contained type of high glass transition temperature or biphenyl structural type epoxy resin;
Resol adopts the resol containing biphenyl structures or multiple hydroxyl structure with good mobility;
The upper limit of the resol used is in 3%-10% scope, and when super going beyond the scope, material has good mobility, when lower than this scope, occurs the problem of mobility and poor reliability.
When the Ratio control of the epoxy equivalent (weight) of epoxy resin and the hydroxyl equivalent of resol is in 0.8-1.3 scopes, composition epoxy resin, when shaping, shows good curing characteristics.
Mineral filler used is ball-shaped silicon micro powder, and its size-grade distribution D50 is 4 ~ 6 μm, and 60 ~ 75%, 6 ~ 12 μm of part silicon powders that 1 ~ 6 μm of part silicon powder accounts for total amount account for 20 ~ 25% of total amount.12 ~ 48 μm of part silicon powders account for 5 ~ 20% of total amount.
Silane coupling agent used is epoxy radicals silicone hydride.
Silane coupling agent used is the mixture of several coupling agent of epoxy radicals silicone hydride, adopts wherein two kinds or several used in combination.It and inorganic materials, organism has good cohesive force.
Described curing catalyst is: imidazoles or phosphorus species, comprises 2-methyl 4-phenyl imidazoles; Or be tertiary amine compound, comprise benzyldimethylamine, triethylamine benzyldimethylamine, 1,8-diazabicyclo (5,4,0) undecylene-7; Or be organic phosphine compound, comprise triphenylphosphine, tetraphenyl phosphine, three (p-methylphenyl) phosphine.Imidazoles or phosphorus species, comprise 2MZ-A or can be used alone or as a mixture, and preferentially selecting can catalyzed reaction under the high temperature conditions, and material can be made to have better mobility.
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Experimental example 1.Fill a prescription described in embodiment 1 in A after each component precise, double roll mill carries out melting mixing, and melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
Experimental example 2.In formula B described in embodiment 2 after each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
Experimental example 3.In formula described in embodiment 3 after each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
Experimental example 4.In formula described in embodiment 4 after each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
Comparative example 1.In described formula after each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
Comparative example 2.In described formula after each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
Comparative example 3.In described formula after each component precise, double roll mill carries out melting mixing, melting temperature is 90 ~ 110 DEG C, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thin slice that 1.5mm is thick, through to be mixed evenly after, cooling crush, carries out performance test.
In contrast experiment, main performance index uses following method to carry out testing:
A) gel time: hot plate method, is heated to 175 ± 1 DEG C by hot plate, get 2-3g sample powder and be placed on hot plate, is terminal when powder becomes colloidal state by fluid gradually, reads required time.
B) mobility: measure by EMMI-1-66 helicoidal flow metal die on transfer mould press, forming pressure is 70Kgf/cm
2die temperature is at 175 ± 2 DEG C, and sample thief 15g tests.
C) melt viscosity: the melt viscosity of epoxy composite described in the capillary rheometer determining utilizing Japanese Shimadzu Corporation.Test condition: mouth mould is 0.5 × 1.0mm, pressure is 25 kilograms, and temperature is 175 DEG C.
Experimental result is as follows:
As can be seen from the above table, the mobility of embodiment and fillibility are all fine, and the mobility of comparative example, formability and fillibility are all very poor, can find out in Flip-Chip Using, in composition, its size-grade distribution D50 of silicon powder controls at 4 ~ 6um, 1 ~ 6um part silicon powder accounts for 60 ~ 75% of total amount, 6 ~ 12um part silicon powder accounts for 20 ~ 25% of total amount, 12 ~ 48um part silicon powder accounts for 5 ~ 20% of total amount, can prepare the composition epoxy resin of the Flip-Chip Using of high workability and good fillibility.