CN102627929B - Underfill flowable at room temperature and rapidly solidified at low temperature, and preparation method thereof - Google Patents
Underfill flowable at room temperature and rapidly solidified at low temperature, and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an underfill which is flowable at room temperature and is rapidly solidified at a low temperature. The underfill is prepared from the following raw materials, by weight, 20-50 parts of a liquid epoxy resin, 5-20 parts of an active epoxy diluent, 0-60 parts of spherical silicon powder, 5-20 parts of a polyester or polyester polyol, 0.1-5 parts of a catalyst, 0.2-2 parts of a coupling agent, 0.1-2 parts of a pigment, and proper amounts of a defoaming agent and a flow assistant. The invention also discloses a preparation method of the underfill. The underfill flowable at room temperature and rapidly solidified at a low temperature, which is prepared according to the method of the invention, has the advantages of reasonable composition ratio, fast flow speed, low solidification temperature, short solidification time, easy reparation, and effective improvement of the technological efficiency of a production lien of electronic products.
Description
Technical field
The present invention relates to a kind of semiconductor components and devices and be assembled into a kind of underfill used on the electronic circuit board, but a kind of room temperature quick-setting bottom of low temperature weighting agent that flows particularly; The invention still further relates to a kind of preparation method of this bottom weighting agent.
Background technology
Along with the develop rapidly of auto electroincs and other consumer electronics products with popularize, microelectronic packaging technology is faced with challenge and the opportunity that electronic product " high performance-price ratio, high reliability, multi-functional, miniaturization and low cost " development trend is brought.Flip-chip (FC), wafer-level package (CSP), ball grid array (BGA) and microballoon grid array (μ BGA) etc. arise at the historic moment under these challenges and opportunity.Usually FC/CSP/BGA/ μ BGA welds together by salient point solder joint and substrate with the form of upside-down mounting, and it provides higher packaging density, shorter connection distance and better electrical property., under the conditions such as the electronic product that is comprised of FC/CSP/BGA/ μ BGA is exposed to cold cycling, shakes and falls, the salient point solder joint between FC/CSP/BGA/ μ BGA and the substrate often can disconnect, thereby electronic product lost efficacy.In order to address this problem; Electronic Assemblies factory can adopt the underfill technology usually; namely in the space between FC/CSP/BGA/ μ BGA and substrate; fill that a kind of thermosetting epoxy resin is used for absorbing between FC/CSP/BGA/ μ BGA and the substrate waits the internal stress that produces because cold cycling and mechanical shock fall, to reach the purpose of raising reliability.According to the specific requirement of different sorts electronic product, bottom weighting agent technology can adopt whole fillings or partially filled.For whole filling modes, can be categorized as again the Capillary Flow bottom and fill and the non-current filling of soldering flux.Every class filling mode has its advantage and limitation, but at present the most widely used be the Capillary Flow underfill.
Existing Capillary Flow underfill adopts liquid-state epoxy resin and epoxide diluent, modified amine curing agent, modified imidazole class promotor usually in the market.Solidification value is generally 150 ℃ of 120 ℃ –, and be 15 minutes to 30 minutes set time.
For the Capillary Flow underfill, because the requirement of the high-level efficiency of electronic product production technique, low cost, good reliability, need that underfill fills that velocity of flow is fast, solidification value is low, set time is short, room temperature storage good stability, cold-hot circulation, anti-mechanical shock and easily reprocess.Present existing technology can't satisfy above requirement.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, but the mobile quick-setting bottom of low temperature of room temperature that a kind of prescription proportioning is more reasonable, velocity of flow is fast, solidification value is low, set time is short, easily reprocess weighting agent is provided.
But another technical problem to be solved by this invention has provided a kind of preparation method of the mobile quick-setting bottom of low temperature of aforesaid room temperature weighting agent.
Technical problem to be solved by this invention is to realize by following technical scheme.But the present invention is the mobile quick-setting bottom of low temperature of a kind of room temperature weighting agent, is characterized in, it is to be made by the raw material of following weight proportion:
Liquid epoxies 20 – 50; Active epoxy thinner 5 – 20;
Ball-shaped silicon micro powder 0 – 60; Polyester type or polyether polyol 5 – 20;
Catalyzer 0.1 – 5; Coupling agent 0.2 – 2;
Colorant 0.1 – 2; And an amount of go out infusion and flow promotor;
Wherein:
Liquid epoxies is selected from one or more the mixing in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the cycloaliphatic epoxy resin;
The active epoxy thinner is that viscosity is that 10-1000mpas is for aliphatics or the aromatic epoxies thinner of epoxide group;
The ball-shaped silicon micro powder median size is the 0.1-1.0 micron, and maximum particle diameter is 5 microns;
Polyester type or polyether polyol are that molecular weight is polyester type or the polyether polyol performed polymer with oh group of 200-50000;
Colorant is the color that carbon black and Resins, epoxy mix, and the shared weight percent of carbon black is not higher than 50% in the colorant;
Catalyzer is the hexafluoro antimonate cationic catalyst;
Coupling agent is selected from least a among propyl trimethoxy silicane HK-560, γ-methacryloxy Trimethoxy silane HK-570.
Technical problem to be solved by this invention can also further realize by following technical scheme.But the invention also discloses preparation method a kind of as the mobile quick-setting bottom of low temperature of the described room temperature of above technical scheme weighting agent, be characterized in, its step is as follows: take by weighing raw material by described weight proportion,
(1) colorant preparation: carbon black and Resins, epoxy are mixed in the mode that three rollers grind, be prefabricated into color;
(2) catalyzer is dissolved in advance makes catalyst intermediate in the Resins, epoxy;
(3) with liquid epoxies, active epoxy thinner, polyester type or polyether polyol, color, go out infusion and flow promotor and add in the reactor and mix, perhaps add as required again ball-shaped silicon micro powder, mixing temperature is 20-30 ℃, mixing time 20-40 minute; Regulate temperature and be down to 10-18 ℃, add coupling agent and catalyst intermediate, under temperature 10-18 ℃, mix 20-40 minute, full vacuum restir mixing 10-20 minute is filtered can, and be get final product.
But room temperature of the present invention flows in low temperature quick-setting bottom weighting agent and the method for making, the Resins, epoxy of Kaolinite Preparation of Catalyst intermediate, colorant can be disclosed any applicable to Resins, epoxy of the present invention in the prior art, and its consumption can be selected on demand.And its consumption is not counted in the liquid epoxies of the present invention.Among the present invention, ball-shaped silicon micro powder is the alternative raw material that adds.
Liquid epoxies of the present invention can be bisphenol A-type or bisphenol f type epoxy resin, or cycloaliphatic epoxy resin, also can be one or more resin blends.For example, the bisphenol A type epoxy resin EXA-850CRP that the large Japanese ink company (DIC) of Japan produces, bisphenol f type epoxy resin EXA-830LVP.Tg point bisphenol A-type or bisphenol f type epoxy resin and cycloaliphatic epoxy resin can improve material cured in underfill of the present invention after, high adhesion and the thermotolerance problem of solution material.
Epoxide diluent of the present invention selects low viscosity for aliphatics or the aromatic epoxies thinner of epoxide group, and it not only can reduce the viscosity of material, solves the velocity of flow problem of underfill, can improve the toughness of material.For example, the HELOXY 61 of U.S. Mai Tu company, HELOXY 68, the DER732 of Dow Chemical.
Polyester type of the present invention or polyether polyol not only can improve the toughness of material, and improve chemical reaction velocity with the Resins, epoxy reaction under the effect of cationic catalyst.
Catalyzer of the present invention is the hexafluoro antimonate cationic catalyst, and it has the characteristics that speed of response is fast, temperature of reaction is low, room temperature stability is good when catalysis Resins, epoxy reacts.
The present invention is that semiconductor components and devices is assembled into a kind of underfill used on the electronic circuit board, described semiconductor components and devices can be flip-chip (FC), wafer-level package (CSP), ball grid array (BGA) and microballoon grid array (μ BGA) etc., it is a kind of thermosetting epoxy resin tackiness agent, have the advantages that viscosity is low, the room temperature current downflow is fast, fast setting under can room temperature, stability in storage is good, reacted product has excellent shock resistance and high and low temperature resistance, and easily reprocesses.
Performance test: the viscosity test under 25 ℃ need be controlled between 300 cps to 500 cps.Flow the required time of 1 cm distance between the sheet glass in 50 microns gaps should be less than 1 minute.Room temperature stability is changed to test by 25 ℃ of lower viscosity of monitoring, curing speed and time by DSC respectively 100 ℃, 110 ℃, and 120 ℃ of lower signs.Tg and CTE are tested by TMA.
Through the ordinary method by prior art the present invention bottom weighting agent is tested detection, the viscosity of the present invention bottom weighting agent is generally between 200 cps –, 1000 cps, its solidification value is 150 ℃ of 100 –, be 2 to 5 minutes set time, storing temp is 2-10 ℃, and room temperature duration of service is more than 7 days.The present invention well balance cold-hot circulation, anti-mechanical shock, easily to reprocess these several respects are mutual conflicting performances.
Compared with prior art, but the present invention and more reasonable by the mobile quick-setting underfill prescription of the low temperature proportioning of the room temperature of the inventive method preparation, and velocity of flow is fast, solidification value is low, set time is short, easily reprocesses, process efficiency that can the Effective Raise electronic product assembly line.The preparation method of the present invention bottom weighting agent is reasonable, and it is simple to operate, can effectively guarantee the quality product of bottom weighting agent.
Embodiment
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 consist of its Copyright law.
Embodiment 1, the quick-setting bottom of the low temperature weighting agent but a kind of room temperature flows, and it is to be made by the raw material of following weight proportion:
Liquid epoxies 20; Active epoxy thinner 5;
Polyester type or polyether polyol 5;
Catalyzer 0.1; Coupling agent 0.2;
Colorant 0.1; And an amount of go out infusion and flow promotor;
Wherein:
Liquid epoxies is selected from one or more the mixing in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the cycloaliphatic epoxy resin;
The active epoxy thinner is that viscosity is that 10-1000mpas is for aliphatics or the aromatic epoxies thinner of epoxide group;
The ball-shaped silicon micro powder median size is the 0.1-1.0 micron, and maximum particle diameter is 5 microns;
Polyester type or polyether polyol are that molecular weight is polyester type or the polyether polyol performed polymer with oh group of 200-50000;
Colorant is the color that carbon black and Resins, epoxy mix, and the shared weight percent of carbon black is not higher than 50% in the colorant;
Catalyzer is the hexafluoro antimonate cationic catalyst;
Coupling agent is selected from least a among propyl trimethoxy silicane HK-560, γ-methacryloxy Trimethoxy silane HK-570.
Ordinary method preparation by prior art.
Embodiment 2, the quick-setting bottom of the low temperature weighting agent but a kind of room temperature flows, and it is to be made by the raw material of following weight proportion:
Liquid epoxies 50; Active epoxy thinner 20;
Ball-shaped silicon micro powder 60; Polyester type or polyether polyol 20;
Catalyzer 5; Coupling agent 2;
Colorant 2; And an amount of go out infusion and flow promotor;
Wherein:
Liquid epoxies is selected from one or more the mixing in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the cycloaliphatic epoxy resin;
The active epoxy thinner is that viscosity is that 10-1000mpas is for aliphatics or the aromatic epoxies thinner of epoxide group;
The ball-shaped silicon micro powder median size is the 0.1-1.0 micron, and maximum particle diameter is 5 microns;
Polyester type or polyether polyol are that molecular weight is polyester type or the polyether polyol performed polymer with oh group of 200-50000;
Colorant is the color that carbon black and Resins, epoxy mix, and the shared weight percent of carbon black is not higher than 50% in the colorant;
Catalyzer is the hexafluoro antimonate cationic catalyst;
Coupling agent is selected from least a among propyl trimethoxy silicane HK-560, γ-methacryloxy Trimethoxy silane HK-570.
Its step of its preparation method is as follows: take by weighing raw material by described weight proportion,
(1) colorant preparation: carbon black and Resins, epoxy are mixed in the mode that three rollers grind, be prefabricated into color;
(2) catalyzer is dissolved in advance makes catalyst intermediate in the Resins, epoxy;
(3) with liquid epoxies, active epoxy thinner, polyester type or polyether polyol, color, go out infusion and flow promotor and add in the reactor and mix, add again ball-shaped silicon micro powder, mixing temperature is 20 ℃, mixing time 20 minutes; Regulate temperature and be down to 10 ℃, add coupling agent and catalyst intermediate, under 10 ℃ of temperature, mix 20 minutes, full vacuum restir mixed 10 minutes, filtered can, and get final product.
Embodiment 3, the quick-setting bottom of the low temperature weighting agent but a kind of room temperature flows, and it is to be made by the raw material of following weight proportion:
Liquid epoxies 35; Active epoxy thinner 12;
Ball-shaped silicon micro powder 20; Polyester type or polyether polyol 12;
Catalyzer 2.5; Coupling agent 1.2;
Colorant 1.0; And an amount of go out infusion and flow promotor;
Wherein:
Liquid epoxies is selected from one or more the mixing in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the cycloaliphatic epoxy resin;
The active epoxy thinner is that viscosity is that 10-1000mpas is for aliphatics or the aromatic epoxies thinner of epoxide group;
The ball-shaped silicon micro powder median size is the 0.1-1.0 micron, and maximum particle diameter is 5 microns;
Polyester type or polyether polyol are that molecular weight is polyester type or the polyether polyol performed polymer with oh group of 200-50000;
Colorant is the color that carbon black and Resins, epoxy mix, and the shared weight percent of carbon black is not higher than 50% in the colorant;
Catalyzer is the hexafluoro antimonate cationic catalyst;
Coupling agent is selected from least a among propyl trimethoxy silicane HK-560, γ-methacryloxy Trimethoxy silane HK-570.
Its preparation methods steps is as follows: take by weighing raw material by described weight proportion,
(1) colorant preparation: carbon black and Resins, epoxy are mixed in the mode that three rollers grind, be prefabricated into color;
(2) catalyzer is dissolved in advance makes catalyst intermediate in the Resins, epoxy;
(3) with liquid epoxies, active epoxy thinner, polyester type or polyether polyol, color, go out infusion and flow promotor and add in the reactor and mix, add again ball-shaped silicon micro powder, mixing temperature is 30 ℃, mixing time 40 minutes; Regulate temperature and be down to 18 ℃, add coupling agent and catalyst intermediate, under 18 ℃ of temperature, mix 40 minutes, full vacuum restir mixed 20 minutes, filtered can, and get final product.
Embodiment 4, the quick-setting bottom of the low temperature weighting agent but a kind of room temperature flows, and it is to be made by the raw material of following weight proportion:
Liquid epoxies 40; Active epoxy thinner 15;
Polyester type or polyether polyol 15;
Catalyzer 3; Coupling agent 1;
Colorant 1.5; And an amount of go out infusion and flow promotor;
Wherein:
Liquid epoxies is selected from one or more the mixing in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the cycloaliphatic epoxy resin;
The active epoxy thinner is that viscosity is that 10-1000mpas is for aliphatics or the aromatic epoxies thinner of epoxide group;
The ball-shaped silicon micro powder median size is the 0.1-1.0 micron, and maximum particle diameter is 5 microns;
Polyester type or polyether polyol are that molecular weight is polyester type or the polyether polyol performed polymer with oh group of 200-50000;
Colorant is the color that carbon black and Resins, epoxy mix, and the shared weight percent of carbon black is not higher than 50% in the colorant;
Catalyzer is the hexafluoro antimonate cationic catalyst;
Coupling agent is selected from least a among propyl trimethoxy silicane HK-560, γ-methacryloxy Trimethoxy silane HK-570.
Its preparation methods steps is as follows: take by weighing raw material by described weight proportion,
(1) colorant preparation: carbon black and Resins, epoxy are mixed in the mode that three rollers grind, be prefabricated into color;
(2) catalyzer is dissolved in advance makes catalyst intermediate in the Resins, epoxy;
(3) with liquid epoxies, active epoxy thinner, polyester type or polyether polyol, color, go out infusion and flow promotor and add in the reactor and mix, mixing temperature is 25 ℃, mixing time 30 minutes; Regulate temperature and be down to 15 ℃, add coupling agent and catalyst intermediate, under 15 ℃ of temperature, mix 30 minutes, full vacuum restir mixed 15 minutes, filtered can, and get final product.
Embodiment 5, the quick-setting bottom of the low temperature weighting agent preparation experiment one but room temperature flows: take by weighing the EXA-850CRP20 gram, EXA-830LVP20 gram, cycloaliphatic epoxy resin 40.1 grams, polyether polyol 7 grams, 10 gram HELOXY-68, black cream 1 gram goes out infusion 0.2 gram, flow promotor 0.2 gram, add in the reactor and mix 20 ℃-30 ℃ of temperature, mixing time 30 minutes.Regulate temperature and be down to 15 ℃, add 1 gram coupling agent KH560 and hexafluoro antimonate cationic catalyst intermediate 0.5 gram, under 15 ℃ of temperature, mix 30 minutes, full vacuum restir mixed 15 minutes.Filter at last can, but obtain the mobile quick-setting underfill of low temperature of room temperature.
Embodiment 6, the quick-setting bottom of the low temperature weighting agent preparation experiment two but room temperature flows: take by weighing the EXA-850CRP15 gram, the EXA-830LVP15 gram, cycloaliphatic epoxy resin 30.1 grams, polyether polyol 7 grams, 20 gram silicon powders, 10 gram HELOXY-68, black cream 1 gram, go out infusion 0.2 gram, flow promotor 0.2 gram mixes in the adding reactor, 20 ℃-30 ℃ of temperature, mixing time 30 minutes.Regulate temperature and be down to 15 ℃, add 1 gram coupling agent KH560 and hexafluoro antimonate cationic catalyst intermediate 0.5 gram, under 15 ℃ of temperature, mix 30 minutes, full vacuum restir mixed 15 minutes.Filter at last can, but obtain the mobile quick-setting underfill of low temperature of room temperature.
Embodiment 7, the quick-setting bottom of the low temperature weighting agent preparation experiment three but room temperature flows: take by weighing the EXA-850CRP20 gram, EXA-830LVP20 gram, cycloaliphatic epoxy resin 39.6 grams, polyether polyol 7 grams, 10 gram HELOXY-68, black cream 1 gram goes out infusion 0.2 gram, flow promotor 0.2 gram, add in the reactor and mix 20 ℃-30 ℃ of temperature, mixing time 30 minutes.Regulate temperature and be down to 15 ℃, add 1 gram coupling agent KH560 and hexafluoro antimonate cationic catalyst intermediate 1 gram, under 15 ℃ of temperature, mix 30 minutes, full vacuum restir mixed 15 minutes.Filter at last can, but obtain the mobile quick-setting underfill of low temperature of room temperature.
Embodiment 8, the quick-setting bottom of the low temperature weighting agent preparation experiment four but room temperature flows: take by weighing the EXA-850CRP20 gram, EXA-830LVP20 gram, cycloaliphatic epoxy resin 39.6 grams, polyether polyol 7 grams, 10 gram HELOXY-61, black cream 1 gram goes out infusion 0.2 gram, flow promotor 0.2 gram, add in the reactor and mix 20 ℃-30 ℃ of temperature, mixing time 30 minutes.Regulate temperature and be down to 15 ℃, add 1 gram coupling agent KH560 and hexafluoro antimonate cationic catalyst intermediate 1 gram, under 15 ℃ of temperature, mix 30 minutes, full vacuum restir mixed 15 minutes.Filter at last can, but obtain the mobile quick-setting underfill of low temperature of room temperature.
Claims (1)
1. but the mobile quick-setting bottom of low temperature of a room temperature weighting agent is characterized in that, it is to be made by the raw material of following weight proportion:
Liquid epoxies 40; Active epoxy thinner 15;
Polyester type or polyether polyol 15;
Catalyzer 3; Coupling agent 1;
Colorant 1.5; And an amount of defrother and flow promotor;
Wherein:
Liquid epoxies is selected from one or more the mixing in bisphenol A type epoxy resin, bisphenol f type epoxy resin, the cycloaliphatic epoxy resin;
The active epoxy thinner is that viscosity is that 10-1000mpas is with aliphatics or the aromatic epoxies thinner of epoxide group;
Polyester type or polyether polyol are that molecular weight is polyester type or the polyether polyol performed polymer with oh group of 200-50000;
Colorant is the color that carbon black and Resins, epoxy mix, and the shared weight percent of carbon black is not higher than 50% in the colorant;
Catalyzer is the hexafluoro antimonate cationic catalyst;
Coupling agent is selected from least a among propyl trimethoxy silicane KH-560, γ-methacryloxy Trimethoxy silane KH-570;
Its preparation methods steps is as follows: take by weighing raw material by described weight proportion,
(1) colorant preparation: carbon black and Resins, epoxy are mixed in the mode that three rollers grind, be prefabricated into color;
(2) catalyzer is dissolved in advance makes catalyst intermediate in the Resins, epoxy;
(3) will mix in liquid epoxies, active epoxy thinner, polyester type or polyether polyol, color, defrother and the flow promotor adding reactor, mixing temperature is 25 ℃, mixing time 30 minutes; Regulate temperature and be down to 15 ℃, add coupling agent and catalyst intermediate, under 15 ℃ of temperature, mix 30 minutes, full vacuum restir mixed 15 minutes, filtered can, and get final product.
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| CN103756612B (en) * | 2013-12-23 | 2015-12-30 | 东莞市亚聚电子材料有限公司 | A kind of low-temperature curing underfill and preparation method thereof |
| CN104979225A (en) * | 2015-05-19 | 2015-10-14 | 深圳创维－Rgb电子有限公司 | Bottom filling method for preventing cold solder joint of BGA IC |
| CN106675477A (en) * | 2016-10-26 | 2017-05-17 | 惠州市杜科新材料有限公司 | Epoxy adhesive with characteristics of single component, low viscosity, medium-temperature rapid curing and high heat conduction |
| CN107641490A (en) * | 2017-09-22 | 2018-01-30 | 北京天山新材料技术有限公司 | A kind of epoxy adhesive |
| CN107868643A (en) * | 2017-11-28 | 2018-04-03 | 长春永固科技有限公司 | Smart card temperature curing epoxy low adhesive and smart card low-temperature setting method for packing |
| CN108219726A (en) * | 2017-12-29 | 2018-06-29 | 汕头市骏码凯撒有限公司 | A kind of one pack system rapid curing cofferdam glue and preparation method thereof |
| CN115141588A (en) * | 2022-06-29 | 2022-10-04 | 上海回天新材料有限公司 | Epoxy resin adhesive for Type C sealing and preparation method thereof |
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| EP0721477B1 (en) * | 1993-07-20 | 1999-06-02 | DELO Industrieklebstoffe GmbH & Co. KG | Flexibilised light-curing epoxy resin compounds, their production and use |
| US6420450B1 (en) * | 1999-06-18 | 2002-07-16 | Delo Industrieklebstoffe Gmbh & Co. Kg | Cationically hardening mass, the use thereof and process for preparing hardened polymer masses |
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| CN102061060A (en) * | 2010-11-26 | 2011-05-18 | 烟台德邦电子材料有限公司 | High-reliability intelligent-card encapsulating glue and preparation method thereof |
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| EP0721477B1 (en) * | 1993-07-20 | 1999-06-02 | DELO Industrieklebstoffe GmbH & Co. KG | Flexibilised light-curing epoxy resin compounds, their production and use |
| US6420450B1 (en) * | 1999-06-18 | 2002-07-16 | Delo Industrieklebstoffe Gmbh & Co. Kg | Cationically hardening mass, the use thereof and process for preparing hardened polymer masses |
| CN101085856A (en) * | 2006-06-09 | 2007-12-12 | 国家淀粉及化学投资控股公司 | Low viscosity curable compositions |
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Denomination of invention: Underfill flowable at room temperature and rapidly solidified at low temperature, and preparation method thereof Effective date of registration: 20170710 Granted publication date: 20131023 Pledgee: China Merchants Bank Limited by Share Ltd Lianyungang branch Pledgor: Lianyungang Huahai Chengke Electronic Material Co., Ltd. Registration number: 2017990000619 |
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