CN101508878B - Bonder and method of preparing the same - Google Patents
Bonder and method of preparing the same Download PDFInfo
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- CN101508878B CN101508878B CN2009101197995A CN200910119799A CN101508878B CN 101508878 B CN101508878 B CN 101508878B CN 2009101197995 A CN2009101197995 A CN 2009101197995A CN 200910119799 A CN200910119799 A CN 200910119799A CN 101508878 B CN101508878 B CN 101508878B
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Abstract
A bonding glue is characterized by containing the components proportioning by weight: 100 parts of bisphenol A type epoxide resin, 0.1-2 parts of alkyl glycidyl ether, 5-8 parts of triazine group imidazolium compound, 3-5 parts of imidazoles accelerant, 0.5-2 parts of gas phase silicon dioxide, 0.5-1 part of carbon powder, 20-40 parts of calcium carbonate, 40-80 parts of aluminium hydroxide and 0.1-0.5 part of organosilane defoaming agent. The bonding glue can be solidified under the condition of 120-150 DEG C and stored for a longer time; generally, the bonding glue can be stored for one month at normal temperature and stored for half a year in a freezer at the temperature below 5 DEG C; furthermore, as the triazine group imidazolium compound is matched with the imidazoles accelerant for use, curing process can be accelerated, and the products have higher thermal stability after being solidified. When in use, the bonding glue has moderate fluidity and is convenient for operation; furthermore, the solidified bonding glue has stronger hardness and thixotropy.
Description
Technical field
The present invention relates to the packaged material of semiconductor electronic product, specifically, relate to a kind of bonder that is used for the encapsulation of semiconductor electronic product, and the preparation method of this bonder.
Background technology
Existing bonder generally is made up of epoxy resin, solidifying agent, promotor, weighting agent and various auxiliary agent, can be used for the encapsulation of semiconductor electronic product (like the wiring board of Die elektrische Zeituhr, the wiring board of counter).But there are many shortcomings in bonder in the market, and for example: condition of storage is harsh, and set time is longer, and thermostability is not good, and is poor with the wiring board viscosifying power, or the like.
Summary of the invention
Technical problem to be solved by this invention provide a kind of shelf lives long, curing speed is fast, thermostability is strong and mobile moderate bonder, and the preparation method of this bonder.The technical scheme that adopts is following:
A kind of bonder is characterized in that containing following components in weight percentage: 100 parts of bisphenol A type epoxy resins; 0.1～2 part of alkyl glycidyl ether; 5～8 parts of the imidazolium compoundss of triazines group; 3～5 parts of imidazoles promotor, said imidazoles promotor are one or more the combinations in glyoxal ethyline, 2-phenylimidazole, 2-undecyl imidazole, 2-heptadecyl imidazoles, 2-phenyl-4-methylimidazole and the 2-ethyl-4-methylimidazole; 0.5～2 part of aerosil; 0.5～1 part of carbon dust; 20～40 parts in lime carbonate; 40～80 parts in white lake; 0.1～0.5 part of organosilane skimmer.
Preferred above-mentioned bisphenol A type epoxy resin is that viscosity is that 10000-20000cps (centipoise), epoxy equivalent (weight) are the bisphenol A type epoxy resin of 180-200.The general bisphenol A type epoxy resin that adopts simple function group, the Tg (second-order transition temperature) after bonder solidifies is 130-140 ℃; When adopting multi-functional bisphenol A type epoxy resin, the Tg after bonder solidifies is higher, can be used for the very high product of reliability requirement, but the too high certain difficulty of having reprocessed for the semiconductor electronic product of Tg.
Preferred abovementioned alkyl glycidyl ether is C
10-C
15Alkyl glycidyl ether.Alkyl glycidyl ether is low viscous reactive thinner; Its effect has the following aspects: the viscosity that 1, reduces the bisphenol A type epoxy resin system; Help the wetting of weighting agent and other auxiliary agent (being the imidazolium compounds, imidazoles promotor, aerosil, carbon dust, organosilane skimmer, dispersion agent etc. of triazines group) and disperse; Reduce the production difficulty of bonder, also helped the application of terminal client; 2, improve toughness after bonder solidifies, remedy the defective of bisphenol A type epoxy resin, the carbochain of the general alkyl glycidyl ether of selecting is long more, and the toughness after bonder solidifies is high more; 3, the Tg after the adjustment bonder solidifies, the addition of general alkyl glycidyl ether is high more, and the Tg after bonder solidifies is low more; 4, reduce the curing exothermic peak of bisphenol A type epoxy resin system, improve product working life.
The imidazolium compounds of above-mentioned triazines group is as solidifying agent, and it has following advantage than general Dyhard RU 100 (DICY) curing system: 1, resistance toheat is better, and thermostability is strong; 2, be used with imidazoles promotor, make the bonder solidification value less demanding, can solidify rapidly down at medium temperature condition (120 ℃-150 ℃); 3, make the bonder stable performance, the shelf lives is longer.The imidazolium compounds of triazines group is with the imidazolium compounds salify, has quite high stability.
It is temperature required that imidazoles promotor is played reduction curing, the effect that improves curing speed.
Preferred above-mentioned aerosil is the nano level aerosil.Aerosil belongs to lyophobic dust as thixotropic agent, is difficult for suction, helps the stability requirement of bonder; Simultaneously, aerosil makes bonder have good thixotroping ability and moderate flowability, through regulating the addition of aerosil, can make bonder adapt to different package thickness requirements.
Preferred above-mentioned carbon dust is non-conductive nanometer level carbon dust, and carbon dust mainly plays pigmentation, promptly gives bonder black apparent colour.
Above-mentioned lime carbonate is as weighting agent.Preferred above-mentioned lime carbonate is 800 orders～1500 purpose lime carbonate.Lime carbonate makes bonder have good hardness, intensity and thixotropic property, and cost is lower, and cost performance is high.The nonactive carbonic acid calcium of the general employing of lime carbonate, nonactive carbonic acid calcium is difficult for suction, can avoid causing the bonder quality deterioration because of suction.Lime carbonate order number is high more, and particle is more little, and product viscosity is high more, and thixotropy is also high more; In addition, the addition of lime carbonate is many more, and the product thixotropy is also strong along with more.
Above-mentioned white lake is used with lime carbonate as weighting agent.Preferred above-mentioned white lake is 800 orders～1500 purpose white lakes.White lake also possesses the ability of control bonder levelling except can giving the good hardness of bonder, intensity and thixotropic property.After adding an amount of white lake, bonder has better leveling characteristics, and mobile steadily and indiffusion more helps the use of terminal client.In addition, use white lake as weighting agent after, bonder is difficult for bubbling under hot conditions, has largely improved the quality of bonder.
Above-mentioned organosilane skimmer has stronger surfactivity effect, can when minimum addition, show higher effect of impregnation may, and reduces the surface tension of bisphenol A type epoxy resin, suppresses the generation of bubble in the course of processing, and eliminates bubble.
Owing to contain more weighting agent (being lime carbonate and white lake) and other powder auxiliary agents (like carbon dust) in the bonder composition; For these weighting agents and auxiliary agent are dispersed in the bisphenol A type epoxy resin better, preferred above-mentioned bonder also contains 0.05～0.5 part of dispersion agent.Dispersion agent can be selected a non-hydrophilic class I liquid I auxiliary agent; Lipid (like glyceryl monostearate (GMS), Tristearoylglycerol (HTG) etc.) like unsaturated fatty acids; It impels material particles (like carbon dust, lime carbonate, white lake etc.) to be dispersed in the bisphenol A type epoxy resin; Form stable suspensoid, prevent to assemble each other between the material particles.Above-mentioned dispersion agent must have stronger consistency with bisphenol A type epoxy resin, to avoid occurring defectives such as apparent layering of bonder or oil stripping.
The present invention also provides a kind of preparation method of above-mentioned bonder, and this preparation method comprises the steps: successively
(1) respectively lime carbonate and white lake are carried out drying, remove the moisture in lime carbonate and the white lake; Drying temperature is preferably 110-120 ℃;
(2) take by weighing imidazolium compounds, imidazoles promotor, aerosil, carbon dust and the organosilane skimmer of bisphenol A type epoxy resin, alkyl glycidyl ether, triazines group in proportion;
(3) materials such as imidazolium compounds, imidazoles promotor, aerosil, carbon dust and organosilane skimmer of bisphenol A type epoxy resin, alkyl glycidyl ether, triazines group are joined cleaning, dry and have in the reaction vessel of watercooling jacket; Move watercooling jacket then, the material temperature in the reaction vessel is controlled at 20-50 ℃, and the material in the reaction vessel is stirred (preferred mixing speed be 1500～3000rpm (rev/min), churning time is 15～30min (minute)), obtains sizing material;
(4) sizing material that obtains after using three-roll grinder that step (3) is stirred carries out 1～2 time and grinds; Through grinding, but the refinement material particles, and it is dispersed in the bisphenol A type epoxy resin;
(5) sizing material that obtains after step (4) grinding is weighed, and join in cleaning, dried reaction vessel; And then take by weighing in proportion, and it is joined in the reaction vessel through dried lime carbonate of step (1) and white lake;
(6) operation watercooling jacket; Material temperature in the reaction vessel is controlled at 20-50 ℃; And stir that (preferred mixing speed is 2000～3500rpm; Churning time is the material in 25～40min) reaction vessels, and lime carbonate and white lake are distributed in the bisphenol A type epoxy resin, obtains whole sizing material;
(7) the whole sizing material that obtains after using three-roll grinder that step (6) is stirred carries out 1～2 time and grinds, and under vacuum condition, carries out deaeration 2～4 hours then, obtains bonder.
When production contains the bonder of dispersion agent; In above-mentioned steps (2), take by weighing dispersion agent in proportion, and in above-mentioned steps (2), the materials such as imidazolium compounds, imidazoles promotor, aerosil, carbon dust and organosilane skimmer of dispersion agent and bisphenol A type epoxy resin, alkyl glycidyl ether, triazines group are together joined cleaning, dry and have in the reaction vessel of watercooling jacket.
Bonder provided by the invention uses the glyoxaline compound of suitable deal as solidifying agent, can under 120～150 ℃ condition, solidify, and can make the shelf lives longer, generally can store 1 month at normal temperatures, places the refrigerator below 5 ℃ can store half a year; And the imidazolium compounds of triazines group and the collocation of imidazoles promotor are used, and can accelerate the curing process, and solidify the back product and have higher thermostability.Two kinds of filler collocation of lime carbonate and white lake are used, and add the aerosil thixotropic agent, can make bonder mobile in use moderate, handled easily.Solidify the back bonder and have stronger hardness and thixotropy, firmly the chip on the protection circuit plate.
Embodiment
Embodiment 1
The preparation method of this bonder comprises the steps: successively
(1) under 110 ℃ condition, respectively lime carbonate (its fineness is 1500 orders) and white lake (its fineness is 1250 orders) are carried out drying, drying process continues 3 hours;
(2) take by weighing bisphenol A type epoxy resin (its viscosity is that 10000cps, epoxy equivalent (weight) are 180) 100Kg (kilogram), C
10-C
15The imidazolium compounds 5Kg of alkyl glycidyl ether 0.2Kg, triazines group, glyoxal ethyline 4Kg, nano level aerosil 1.8Kg, non-conductive nano level carbon dust 0.5Kg, organosilane skimmer 0.5Kg;
(3) materials such as the imidazolium compounds of bisphenol A type epoxy resin, C10-C15 alkyl glycidyl ether, triazines group, glyoxal ethyline, nano level aerosil, non-conductive nano level carbon dust, organosilane skimmer are joined cleaning, dry and have in the reaction vessel of watercooling jacket; Move watercooling jacket then, the material temperature in the reaction vessel is controlled at 20-50 ℃, and the material in the reaction vessel is stirred (mixing speed is 1800rpm, and churning time is 20min), each material is disperseed rapidly, obtain sizing material;
(4) sizing material that obtains after using three-roll grinder that step (3) is stirred carries out 2 times and grinds; The various material particles of refinement, and it is dispersed in the bisphenol A type epoxy resin;
(5) sizing material that obtains after step (4) grinding is weighed, and join in cleaning, dried reaction vessel; And then take by weighing in proportion, and it is joined in the reaction vessel through dried 30Kg lime carbonate of step (1) and 65Kg white lake;
(6) operation watercooling jacket; Material temperature in the reaction vessel is controlled at 20-50 ℃, and stirs the material in (mixing speed is 3000rpm, and churning time is 30min) reaction vessel; Lime carbonate and white lake are distributed to rapidly in the bisphenol A type epoxy resin, obtain whole sizing material;
(7) the whole sizing material that obtains after using three-roll grinder that step (6) is stirred carries out 1 time and grinds, and under vacuum condition, carries out deaeration 3 hours then, obtains bonder.
The bonder that obtains contains bisphenol A type epoxy resin 100Kg, C
10-C
15The imidazolium compounds 5Kg of alkyl glycidyl ether 0.2Kg, triazines group, glyoxal ethyline 4Kg, nano level aerosil 1.8Kg, non-conductive nano level carbon dust 0.5Kg, lime carbonate 30Kg, white lake 65Kg and organosilane skimmer 0.5Kg.
Embodiment 2
The preparation method of this bonder comprises the steps: successively
(1) under 120 ℃ condition, respectively lime carbonate (its fineness is 800 orders) and white lake (its fineness is 1000 orders) are carried out drying, drying process continues 3 hours;
(2) take by weighing bisphenol A type epoxy resin (its viscosity is that 20000cps, epoxy equivalent (weight) are 190) 100Kg, C
10-C
15The imidazolium compounds 8Kg of alkyl glycidyl ether 2Kg, triazines group, 2-phenylimidazole 2Kg, 2-heptadecyl imidazoles 3Kg, nano level aerosil 0.5Kg, non-conductive nano level carbon dust 0.7Kg, organosilane skimmer 0.12Kg, dispersion agent 0.06Kg (being glyceryl monostearate);
(3) materials such as the imidazolium compounds of bisphenol A type epoxy resin, C10-C15 alkyl glycidyl ether, triazines group, 2-phenylimidazole, 2-heptadecyl imidazoles, nano level aerosil, non-conductive nano level carbon dust, organosilane skimmer, dispersion agent are joined cleaning, dry and have in the reaction vessel of watercooling jacket; Move watercooling jacket then, the material temperature in the reaction vessel is controlled at 20-50 ℃, and the material in the reaction vessel is stirred (mixing speed is 3000rpm, and churning time is 15min), each material is disperseed rapidly, obtain sizing material;
(4) sizing material that obtains after using three-roll grinder that step (3) is stirred carries out 1 time and grinds; The various material particles of refinement, and it is dispersed in the bisphenol A type epoxy resin;
(5) sizing material that obtains after step (4) grinding is weighed, and join in cleaning, dried reaction vessel; And then take by weighing in proportion, and it is joined in the reaction vessel through dried 40Kg lime carbonate of step (1) and 50Kg white lake;
(6) operation watercooling jacket; Material temperature in the reaction vessel is controlled at 20-50 ℃, and stirs the material in (mixing speed is 2000rpm, and churning time is 40min) reaction vessel; Lime carbonate and white lake are distributed to rapidly in the bisphenol A type epoxy resin, obtain whole sizing material;
(7) the whole sizing material that obtains after using three-roll grinder that step (6) is stirred carries out 2 times and grinds, and under vacuum condition, carries out deaeration 2 hours then, obtains bonder.
The bonder that obtains contains bisphenol A type epoxy resin 100Kg, C
10-C
15The imidazolium compounds 8Kg of alkyl glycidyl ether 2Kg, triazines group, 2-phenylimidazole 2Kg, 2-heptadecyl imidazoles 3Kg, nano level aerosil 0.5Kg, non-conductive nano level carbon dust 0.7Kg, lime carbonate 40Kg, white lake 50Kg, organosilane skimmer 0.12Kg and dispersion agent 0.06
Kg (being glyceryl monostearate).
Embodiment 3
The preparation method of this bonder comprises the steps: successively
(1) under 114 ℃ condition, respectively lime carbonate (its fineness is 1250 orders) and white lake (its fineness is 1500 orders) are carried out drying, drying process continues 3 hours;
(2) take by weighing bisphenol A type epoxy resin 100Kg (viscosity is that 15000cps, epoxy equivalent (weight) are 200), C10-C15 alkyl glycidyl ether 1.2Kg, the imidazolium compounds 6Kg of triazines group, 2-phenyl-4-methylimidazole 3Kg, nano level aerosil 1Kg, non-conductive nano level carbon dust 0.9Kg, organosilane skimmer 0.3Kg, dispersion agent 0.5Kg (being Tristearoylglycerol);
(3) materials such as the imidazolium compounds of bisphenol A type epoxy resin, C10-C15 alkyl glycidyl ether, triazines group, 2-phenylimidazole, 2-heptadecyl imidazoles, nano level aerosil, non-conductive nano level carbon dust, organosilane skimmer, dispersion agent are joined cleaning, dry and have in the reaction vessel of watercooling jacket; Move watercooling jacket then, the material temperature in the reaction vessel is controlled at 20-50 ℃, and the material in the reaction vessel is stirred (mixing speed is 2000rpm, and churning time is 25min), each material is disperseed rapidly, obtain sizing material;
(4) sizing material that obtains after using three-roll grinder that step (3) is stirred carries out 2 times and grinds; The various material particles of refinement, and it is dispersed in the bisphenol A type epoxy resin;
(5) sizing material that obtains after step (4) grinding is weighed, and join in cleaning, dried reaction vessel; And then take by weighing in proportion, and it is joined in the reaction vessel through dried 20Kg lime carbonate of step (1) and 80Kg white lake;
(6) operation watercooling jacket; Material temperature in the reaction vessel is controlled at 20-50 ℃, and stirs the material in (mixing speed is 2500rpm, and churning time is 25min) reaction vessel; Lime carbonate and white lake are distributed to rapidly in the bisphenol A type epoxy resin, obtain whole sizing material;
(7) the whole sizing material that obtains after using three-roll grinder that step (6) is stirred carries out 1 time and grinds, and under vacuum condition, carries out deaeration 4 hours then, obtains bonder.
The bonder that obtains contains imidazolium compounds 6Kg, 2-phenyl-4-methylimidazole 3Kg, nano level aerosil 1Kg, non-conductive nano level carbon dust 0.9Kg, lime carbonate 20Kg, white lake 80Kg, organosilane skimmer 0.3Kg, the dispersion agent 0.5Kg (being Tristearoylglycerol) of bisphenol A type epoxy resin 100Kg, C10-C15 alkyl glycidyl ether 1.2Kg, triazines group.
In the foregoing description 1,2 and 3, suppose that in stirring and process of lapping, sizing material is loss not.But in the actual production, in the process of lapping of the stirring of step (3) and step (4), sizing material is lossy; Therefore in step (5) when weighing; Should correspondingly reduce the consumption of lime carbonate and white lake according to the rate of loss of sizing material, to obtain the bonder of predetermined ingredients proportioning.
Claims (9)
1. a bonder is characterized in that containing following components in weight percentage: 100 parts of bisphenol A type epoxy resins; 0.1～2 part of alkyl glycidyl ether; 5～8 parts of the imidazolium compoundss of triazines group; 3～5 parts of imidazoles promotor, said imidazoles promotor are one or more the combinations in glyoxal ethyline, 2-phenylimidazole, 2-undecyl imidazole, 2-heptadecyl imidazoles, 2-phenyl-4-methylimidazole and the 2-ethyl-4-methylimidazole; 0.5～2 part of aerosil; 0.5～1 part of carbon dust; 20～40 parts in lime carbonate; 40～80 parts in white lake; 0.1～0.5 part of organosilane skimmer.
2. bonder according to claim 1 is characterized in that: said bisphenol A type epoxy resin is that viscosity is that 10000-20000cps, epoxy equivalent (weight) are the bisphenol A type epoxy resin of 180-200.
3. bonder according to claim 1 is characterized in that: said alkyl glycidyl ether is C
10-C
15Alkyl glycidyl ether.
4. bonder according to claim 1 is characterized in that: said aerosil is the nano level aerosil.
5. bonder according to claim 1 is characterized in that: said carbon dust is non-conductive nanometer level carbon dust.
6. bonder according to claim 1 is characterized in that: said lime carbonate is 800 orders～1500 purpose lime carbonate.
7. bonder according to claim 1 is characterized in that: said white lake is 800 orders～1500 purpose white lakes.
8. according to each described bonder of claim 1-8, it is characterized in that: said bonder also contains 0.05～0.5 part of dispersion agent.
9. the preparation method of the described bonder of claim 1 is characterized in that comprising the steps: successively
(1) respectively lime carbonate and white lake are carried out drying, remove the moisture in lime carbonate and the white lake;
(2) take by weighing imidazolium compounds, imidazoles promotor, aerosil, carbon dust and the organosilane skimmer of bisphenol A type epoxy resin, alkyl glycidyl ether, triazines group in proportion;
(3) materials such as imidazolium compounds, imidazoles promotor, aerosil, carbon dust and organosilane skimmer of bisphenol A type epoxy resin, alkyl glycidyl ether, triazines group are joined cleaning, dry and have in the reaction vessel of watercooling jacket; Move watercooling jacket then, the material temperature in the reaction vessel is controlled at 20-50 ℃, and the material in the reaction vessel is stirred, obtain sizing material;
(4) sizing material that obtains after using three-roll grinder that step (3) is stirred carries out 1～2 time and grinds;
(5) sizing material that obtains after step (4) grinding is weighed, and join in cleaning, dried reaction vessel; And then take by weighing in proportion, and it is joined in the reaction vessel through dried lime carbonate of step (1) and white lake;
(6) the operation watercooling jacket is controlled at 20-50 ℃ with the material temperature in the reaction vessel, and the material in the stirring reaction container, and lime carbonate and white lake are distributed in the bisphenol A type epoxy resin, obtains whole sizing material;
(7) the whole sizing material that obtains after using three-roll grinder that step (6) is stirred carries out 1～2 time and grinds, and under vacuum condition, carries out deaeration 2～4 hours then, obtains bonder.
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| CN2009101197995A CN101508878B (en) | 2009-03-30 | 2009-03-30 | Bonder and method of preparing the same |
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| CN101508878B true CN101508878B (en) | 2012-08-15 |
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| CN102010576A (en) * | 2010-09-11 | 2011-04-13 | 汕头市骏码凯撒有限公司 | Repairable type epoxy resin encapsulating glue and preparation method thereof |
| CN101948609A (en) * | 2010-09-11 | 2011-01-19 | 汕头市骏码凯撒有限公司 | Black rubber and preparation method thereof |
| CN104312509A (en) * | 2014-10-31 | 2015-01-28 | 合肥鼎雅家具有限责任公司 | Wear-resisting epoxy resin composite material for chip bonding agent and manufacture method thereof |
| CN109296617A (en) * | 2018-10-31 | 2019-02-01 | 中国船舶重工集团公司第七0七研究所 | A kind of anti-loosening method of gyro machine locking nut |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872938A (en) * | 2006-03-21 | 2006-12-06 | 上海市合成树脂研究所 | Epoxy binder in monocomponent in use for insulation of electrical motor |
| CN101313045A (en) * | 2005-11-23 | 2008-11-26 | 3M创新有限公司 | Anisotropic conductive adhesive compositions |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101313045A (en) * | 2005-11-23 | 2008-11-26 | 3M创新有限公司 | Anisotropic conductive adhesive compositions |
| CN1872938A (en) * | 2006-03-21 | 2006-12-06 | 上海市合成树脂研究所 | Epoxy binder in monocomponent in use for insulation of electrical motor |
Non-Patent Citations (1)
| Title |
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| JP特开2002-201448A 2002.07.19 |
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