CN102863744A - High-power packaging epoxy resin composition with good forming performances - Google Patents

High-power packaging epoxy resin composition with good forming performances Download PDF

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Publication number
CN102863744A
CN102863744A CN2012103688739A CN201210368873A CN102863744A CN 102863744 A CN102863744 A CN 102863744A CN 2012103688739 A CN2012103688739 A CN 2012103688739A CN 201210368873 A CN201210368873 A CN 201210368873A CN 102863744 A CN102863744 A CN 102863744A
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China
Prior art keywords
epoxy resin
resin composition
grams
epoxy
resol
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CN2012103688739A
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Chinese (zh)
Inventor
张德伟
单玉来
孙波
周佃香
王松松
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JIANGSU ZHONGPENG NEW MATERIAL CO Ltd
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JIANGSU ZHONGPENG NEW MATERIAL CO Ltd
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Abstract

A high-power packaging epoxy resin composition with good forming performances contains epoxy resin (A), phenolic resin (B), inorganic filler (C), high thermal conductive filler (D), solidification accelerator (E), silane coupling agent (F), silicone (G), releasing agent (H), colorant (I) and flame retardant (J). The high thermal conductive filler selects silicon carbide which has a thermal conductive coefficient of 83.6W/m-K. The epoxy resin composition is treated by adding the silicone with epoxy group, and the melt viscosity of the obtained composition is 50-80Pa s. The high-power packaging epoxy resin composition with the good forming performances has the advantages that the epoxy resin composition has good mobility and operating performance, so that problems of incomplete filling, poor operability and the like can be solved, and requirements of packaging clients on product packaging processes and high-power packaging heat radiation can be met.

Description

High-power encapsulating epoxy resin composition with good processability
Technical field
The present invention relates to a kind of composition epoxy resin, particularly a kind of high-power encapsulating epoxy resin composition with good processability.
Background technology
At present, the high power device encapsulation is had relatively high expectations to the heat dispersion of material, existing technology mainly be by the mineral filler that adds high heat conduction (such as silicon carbide, aluminum oxide etc.) in the middle of composition epoxy resin, can give the good heat conductivility of composition (for example, with reference to Unexamined Patent 6-200124 communique).The problems such as but the Material Filling amount of high heat conduction is too high, will cause the variety of issues such as mobile reduction, can cause occurring filling in the follow-up encapsulated moulding process incomplete, and operability is bad.
In the middle of disclosed technology, adopt silane coupling agent that surface treatment is carried out in mineral filler and increase the content (for example, with reference to Unexamined Patent 8-20673 communique) of mineral filler, the low viscosity in the time of can keeping moulding and high workability.Yet the conventional silanes coupling agent molecule amount of using in the method is less, and the bonding force between the mineral filler is relatively poor, does not have certain toughening effect, thereby so that the composition epoxy resin melt viscosity is not enough little, therefore requires further improvement technology.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, has proposed a kind ofly to satisfy the filling that occurs in the encapsulated moulding process fully and the high-power encapsulating epoxy resin composition with good processability of the requirement of operability.
The technical problem to be solved in the present invention is achieved through the following technical solutions, a kind of high-power encapsulating epoxy resin composition with good processability, and be characterized in: it comprises the component of following weight part:
5~15 parts of Resins, epoxy (A)
5~10 parts in resol (B)
60~85 parts of mineral fillers (C)
5~15 parts of high heat conductive fillers (D)
0.5~2.5 part of curing catalyst (E)
0.5~4.5 part of silane coupling agent (F)
0.1 ~ 1 part of silicone (G)
0.1 ~ 1 part of releasing agent (H)
0.5~4.5 part of tinting material (I)
0.1 ~ 1 part of fire retardant (J)
Described silicone contains epoxide group in molecular structure, pH value is 4 ~ 7, and molecular weight is 5000 ~ 10000, and has following general formula (1)
Figure 44700DEST_PATH_IMAGE001
Wherein in general formula (1),
R 1And R 2Expression has the alkyl of 1 to 5 carbon atom separately;
R 3Expression has alkyl, vinyl, phenyl or epoxy group(ing);
R 4Expression has ether, ethylene glycol or propylene glycol;
X, Y and Z are respectively 1 to 20,1 to 15 and 1 to 20 integer.
The technical problem to be solved in the present invention can also be come further to realize by the following technical programs, described Resins, epoxy (A) is divided into a part and the partially mixed use of b, a partly selects ortho-cresol type Resins, epoxy, viscosity is 1.0 ~ 2.0P, fugitive constituent<0.08%, epoxy equivalent (weight) is 200g/eq, and wherein a part weight accounts for 75 ~ 85%; B partly selects a kind of in dicyclopentadiene type Resins, epoxy, the biphenyl type epoxy resin.Remainder is the b part.
The technical problem to be solved in the present invention can also be come further to realize by the following technical programs, described solidifying agent resol (B), be divided into c part and the partially mixed use of d, select lacquer resins, viscosity is 3.0 ~ 4.0P, fugitive constituent<0.1%, hydroxyl equivalent are 107g/eq, and wherein c partly accounts for 80%; D partly selects a kind of in the resol of resol, biphenyl structural of p-Xylol modification.
The technical problem to be solved in the present invention can also be come further realization by the following technical programs, and described mineral filler (C) is divided into e part and the partially mixed use of f, and two kinds of mineral fillers all are crystalline silicon powder, wherein e part mineral filler meta particle diameter d 50Be 20~30um, f part mineral filler meta particle diameter d 50Be 2~8um, e part weight accounts for 75~85%, f part weight and accounts for 10~25%.
The technical problem to be solved in the present invention can also be come further realization by the following technical programs, and described high heat conductive filler (D) is silicon carbide.
High heat conductive filler is selected silicon carbide among the present invention, and its thermal conductivity is 83.6W/m-K.By adding a kind of silicone that contains epoxide group, because its higher molecular weight so that molecular chain has certain kindliness and ductility, plays certain toughening effect; Contained epoxide group can combine with resin combination well effectively simultaneously, thereby obtains to be fit to the melt viscosity of encapsulation and the composition epoxy resin of high workability.Compared with prior art, composition epoxy resin of the present invention has low melt viscosity, good fluidity and operability, can not only reach the high heat dispersion requirement of high-power encapsulation usefulness, also satisfies plasticity good in the encapsulation process and operability.
Embodiment
A kind of high-power encapsulating epoxy resin composition with good processability, it comprises the component of following weight part:
5~15 parts of Resins, epoxy (A)
5~10 parts in resol (B)
60~85 parts of mineral fillers (C)
5~15 parts of high heat conductive fillers (D)
0.5~2.5 part of curing catalyst (E)
0.5~4.5 part of silane coupling agent (F)
0.1 ~ 1 part of silicone (G)
0.1 ~ 1 part of releasing agent (H)
0.5~4.5 part of tinting material (I)
0.1 ~ 1 part of fire retardant (J)
Described silicone contains epoxide group in molecular structure, pH value is 4 ~ 7, and molecular weight is 5000 ~ 10000, and has following general formula (1)
Figure 699804DEST_PATH_IMAGE001
Wherein in general formula (1),
R 1And R 2Expression has the alkyl of 1 to 5 carbon atom separately;
R 3Expression has alkyl, vinyl, phenyl or epoxy group(ing);
R 4Expression has ether, ethylene glycol or propylene glycol;
X, Y and Z are respectively 1 to 20,1 to 15 and 1 to 20 integer.
Described Resins, epoxy (A) is divided into a part and the partially mixed use of b, and a partly selects ortho-cresol type Resins, epoxy, and viscosity is 1.0 ~ 2.0P, and fugitive constituent<0.08%, epoxy equivalent (weight) are 200g/eq, and wherein a part weight accounts for 75 ~ 85%; B partly selects a kind of in dicyclopentadiene type Resins, epoxy, the biphenyl type epoxy resin.Remainder is the b part.
Described solidifying agent resol (B) is divided into c part and the partially mixed use of d, selects lacquer resins, and viscosity is 3.0 ~ 4.0P, and fugitive constituent<0.1%, hydroxyl equivalent are 107g/eq, and wherein c partly accounts for 80%; D partly selects a kind of in the resol of resol, biphenyl structural of p-Xylol modification.
Described mineral filler (C) is divided into e part and the partially mixed use of f, and two kinds of mineral fillers all are crystalline silicon powder, wherein e part mineral filler meta particle diameter d 50Be 20~30um, f part mineral filler meta particle diameter d 50Be 2~8um, e part weight accounts for 75~85%, f part weight and accounts for 10~25%.
Described high heat conductive filler (D) is silicon carbide.
Composition epoxy resin of the present invention can adopt following methods preparation: in will filling a prescription after the accurate weighing of each component, carry out melting mixing at double roll mill, melting temperature is 90~110 ℃, mixing time is 2 ~ 20 minutes, mixing material is pressed into the thick thin slice of 1.5mm, through to be mixed evenly after, cooling crush carries out performance test.
Below further describe concrete technical scheme of the present invention, so that those skilled in the art further understands the present invention, but do not consist of Copyright law of the present invention.
Experimental example 1.Embodiment 1 described Resins, epoxy (a+b) 90 grams; Resol (c+d) 47 grams; Silicon carbide 100 grams; Mineral filler: e part 560 grams, f part 80 grams; Promotor 1.5 grams; Fire retardant 6 grams; Coupling agent KH-560 4.5 grams; Tinting material carbon black 3 grams; Releasing agent carnauba wax 3 grams; Silicone 3 grams.After the accurate weighing of each component of starting material, silicon powder was processed in mixing machine 5 minutes with coupling agent in the above-mentioned prescription, then added other component, carry out melting mixing at double roll mill, melting temperature is 90 oC, mixing time are 10 minutes, and mixing material is pressed into the thick thin slice of 1.5mm, to be mixed evenly after, cooling crush is pressed into the material cake, carries out performance test.
Experimental example 2.Embodiment 2 described Resins, epoxy (a+b) 90 grams; Resol (c+d) 47 grams; Mineral filler: e part 560 grams, f part 80 grams; Silicon carbide 100 grams; Promotor 1.5 grams; Fire retardant 6 grams; Coupling agent KH-560 4.5 grams; Tinting material carbon black 3 grams; Releasing agent carnauba wax 3 grams; Silicone 6 grams.After the accurate weighing of each component of starting material, silicon powder was processed in mixing machine 5 minutes with coupling agent in the above-mentioned prescription, then added other component, carry out melting mixing at double roll mill, melting temperature is 90 oC, mixing time are 10 minutes, and mixing material is pressed into the thick thin slice of 1.5mm, to be mixed evenly after, cooling crush is pressed into the material cake, carries out performance test.
Experimental example 3.Embodiment 3 described Resins, epoxy (a+b) 92 grams; Resol (c+d) 49 grams; Mineral filler: e part 550 grams, f part 100 grams; Silicon carbide 50 grams; Promotor 1.5 grams; Fire retardant 6 grams; Coupling agent KH-560 4.5 grams; Tinting material carbon black 3 grams; Releasing agent carnauba wax 3 grams; Silicone 6 grams.After the accurate weighing of each component of starting material, silicon powder was processed in mixing machine 5 minutes with coupling agent in the above-mentioned prescription, then added other component, carry out melting mixing at double roll mill, melting temperature is 90 oC, mixing time are 10 minutes, and mixing material is pressed into the thick thin slice of 1.5mm, to be mixed evenly after, cooling crush is pressed into the material cake, carries out performance test.
Experimental example 4.Embodiment 4 described Resins, epoxy (a+b) 92 grams; Resol (c+d) 49 grams; Mineral filler: e part 530 grams, f part 90 grams; Silicon carbide 100 grams; Promotor 1.5 grams; Fire retardant 6 grams; Coupling agent KH-560 4.5 grams; Tinting material carbon black 3 grams; Releasing agent carnauba wax 3 grams; Silicone 6 grams.After the accurate weighing of each component of starting material, silicon powder was processed in mixing machine 5 minutes with coupling agent in the above-mentioned prescription, then added other component, carry out melting mixing at double roll mill, melting temperature is 90 oC, mixing time are 10 minutes, and mixing material is pressed into the thick thin slice of 1.5mm, to be mixed evenly after, cooling crush is pressed into the material cake, carries out performance test.
Comparative Examples 1.Described Resins, epoxy (a+b) 90 grams; Resol (c+d) 47 grams; Mineral filler: e part 560 grams, f part 80 grams; Promotor 1.5 grams; Fire retardant 6 grams; Silicon carbide 100 grams; Coupling agent KH-560 4.5 grams; Tinting material carbon black 3 grams; Releasing agent carnauba wax 3 grams.After the accurate weighing of each component of starting material, silicon powder was processed in mixing machine 5 minutes with coupling agent in the above-mentioned prescription, then added other component, carry out melting mixing at double roll mill, melting temperature is 90 oC, mixing time are 10 minutes, and mixing material is pressed into the thick thin slice of 1.5mm, to be mixed evenly after, cooling crush is pressed into the material cake, carries out performance test.
Comparative Examples 2.Described Resins, epoxy (a+b) 92 grams; Resol (c+d) 49 grams; Mineral filler: e part 580 grams, f part 120 grams; Promotor 1.5 grams; Fire retardant 6 grams; Coupling agent KH-560 4.5 grams; Tinting material carbon black 3 grams; Releasing agent carnauba wax 3 grams; Silicone 6 grams.After the accurate weighing of each component of starting material, silicon powder was processed in mixing machine 5 minutes with coupling agent in the above-mentioned prescription, then added other component, carry out melting mixing at double roll mill, melting temperature is 90 oC, mixing time are 10 minutes, and mixing material is pressed into the thick thin slice of 1.5mm, to be mixed evenly after, cooling crush is pressed into the material cake, carries out performance test.
Main performance index uses following method to test among the contrast experiment:
1, gel time: hot plate method is heated to 175 ± 1 with hot plate oC gets 2-3g sample powder and is placed on the hot plate, and powder is terminal point when becoming colloidal state by fluid gradually, reads required time.
2, flowability: measure by EMMI-1-66 helicoidal flow metal die on the transfer mould press, forming pressure is 70Kgf/cm 2Die temperature is 175 ± 2 oC, sample thief 15g tests.
3, melt viscosity: the melt viscosity that utilizes the described epoxy composite of capillary rheometer determining of Japanese Shimadzu company.Test condition: a mouthful mould is 0.5 * 1.0mm, and load is 20kg, and temperature is 175 oC.
4, thermal conductivity: utilize conductometer to measure the thermal conductivity of described epoxy composite.
Experimental result sees the following form:
Figure 95013DEST_PATH_IMAGE002

Claims (5)

1. high-power encapsulating epoxy resin composition with good processability, it is characterized in that: it comprises the component of following weight part:
5~15 parts of Resins, epoxy (A)
5~10 parts in resol (B)
60~85 parts of mineral fillers (C)
5~15 parts of high heat conductive fillers (D)
0.5~2.5 part of curing catalyst (E)
0.5~4.5 part of silane coupling agent (F)
0.1 ~ 1 part of silicone (G)
0.1 ~ 1 part of releasing agent (H)
0.5~4.5 part of tinting material (I)
0.1 ~ 1 part of fire retardant (J)
Described silicone contains epoxide group in molecular structure, pH value is 4 ~ 7, and molecular weight is 5000 ~ 10000, and has following general formula (1)
Figure 2012103688739100001DEST_PATH_IMAGE002
Wherein in general formula (1),
R 1And R 2Expression has the alkyl of 1 to 5 carbon atom separately;
R 3Expression has alkyl, vinyl, phenyl or epoxy group(ing);
R 4Expression has ether, ethylene glycol or propylene glycol;
X, Y and Z are respectively 1 to 20,1 to 15 and 1 to 20 integer.
2. the high-power encapsulating epoxy resin composition with good processability according to claim 1, it is characterized in that: described Resins, epoxy (A) is divided into a part and the partially mixed use of b, a partly selects ortho-cresol type Resins, epoxy, viscosity is 1.0 ~ 2.0P, fugitive constituent<0.08%, epoxy equivalent (weight) is 200g/eq, and wherein a part weight accounts for 75 ~ 85%; B partly selects a kind of in dicyclopentadiene type Resins, epoxy, the biphenyl type epoxy resin, and remainder is the b part.
3. the high-power encapsulating epoxy resin composition with good processability according to claim 1, it is characterized in that: described solidifying agent resol (B), be divided into c part and the partially mixed use of d, select lacquer resins, viscosity is 3.0 ~ 4.0P, fugitive constituent<0.1%, hydroxyl equivalent are 107g/eq, and wherein c partly accounts for 80%; D partly selects a kind of in the resol of resol, biphenyl structural of p-Xylol modification.
4. the high-power encapsulating epoxy resin composition with good processability according to claim 1, it is characterized in that: described mineral filler (C) is divided into e part and the partially mixed use of f, two kinds of mineral fillers all are crystalline silicon powder, wherein e part mineral filler meta particle diameter d 50Be 20~30um, f part mineral filler meta particle diameter d 50Be 2~8um, e part weight accounts for 75~85%, f part weight and accounts for 10~25%.
5. the high-power encapsulating epoxy resin composition with good processability according to claim 1, it is characterized in that: described high heat conductive filler (D) is silicon carbide.
CN2012103688739A 2012-09-27 2012-09-27 High-power packaging epoxy resin composition with good forming performances Pending CN102863744A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107353597A (en) * 2017-08-21 2017-11-17 江苏中鹏新材料股份有限公司 Capsulation material and IGBT packagings
CN109467881A (en) * 2018-10-31 2019-03-15 科化新材料泰州有限公司 A kind of super heat-resisting, high thermal conductivity epoxy-plastic packaging material of semiconductor-sealing-purpose

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101068846A (en) * 2004-11-30 2007-11-07 住友电木株式会社 Epoxy resin composition and semiconductor device

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101068846A (en) * 2004-11-30 2007-11-07 住友电木株式会社 Epoxy resin composition and semiconductor device

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107353597A (en) * 2017-08-21 2017-11-17 江苏中鹏新材料股份有限公司 Capsulation material and IGBT packagings
CN109467881A (en) * 2018-10-31 2019-03-15 科化新材料泰州有限公司 A kind of super heat-resisting, high thermal conductivity epoxy-plastic packaging material of semiconductor-sealing-purpose
CN109467881B (en) * 2018-10-31 2021-10-26 江苏科化新材料科技有限公司 Super-heat-resistant high-thermal-conductivity epoxy plastic packaging material for semiconductor packaging

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Application publication date: 20130109