CN102079957A - Low-temperature rapidly-curable surface mounting adhesive - Google Patents
Low-temperature rapidly-curable surface mounting adhesive Download PDFInfo
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- CN102079957A CN102079957A CN201010580322XA CN201010580322A CN102079957A CN 102079957 A CN102079957 A CN 102079957A CN 201010580322X A CN201010580322X A CN 201010580322XA CN 201010580322 A CN201010580322 A CN 201010580322A CN 102079957 A CN102079957 A CN 102079957A
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Abstract
The invention discloses a low-temperature rapidly-curable surface mounting adhesive, which is prepared from the following raw materials in percent by weight: 5.8 to 59 percent of bisphenol epoxy resin, 5.8 to 59 percent of modified epoxy resin, 2 to 10 percent of toughening agent, 0.5 to 14.5 percent of latent curing agent, 1.5 to 10.5 percent of accelerator, 20 to 59 percent of thixotropic agent, 1.1 to 10.8 percent of coupling agent, 0.5 to 14.8 percent of inorganic filler and 0 to 6 percent of dye. Due to the adoption of the component proportions, the low-temperature rapidly-curable surface mounting adhesive overcomes the shortcomings of the conventional surface mounting adhesive, and has the advantages of (1) stable storage period, (2) low viscosity and high dispensing performance, (3) low linear expansion coefficient of 40 to 60ppm/DEG C, (4) short curing time of 5 minutes at 80 DEG C, (5) shearing strength of 16MPa and the like.
Description
Technical field
The present invention relates to surface mount and stick with glue agent, but relate in particular to a kind of high surface dress tackiness agent of the quick-setting adhesiveproperties of low temperature that can be used for thermal sensing element.
Background technology
Surface mounting technology (SMT) has been penetrated into every field as electronics package technique of new generation, and SMT develops rapidly, is widely used, and has replaced traditional electronics package technique in a lot of fields fully.SMT makes the electronics package technique produce basic, revolutionary change, and constantly develops perfect in application process with self characteristics and advantage.Surface mounting technology (SMT) is a kind of brand new technical of current electronic package, and it is with hypomegetic nothing lead-in wire components and parts or the extremely short components and parts of lead-in wire, directly is welded on the printed circuit board.Adopt this technology, machine volume can reduce 40%, weight saving 75 %, and improved the function and the reliability of complete machine.Adopt the circuit of surface mounting technology to have characteristics such as volume is little, in light weight, function is strong, and this technology easily is automated production, can improve the high speed performance and the reliability of products of circuit, and can reduce cost, using on electronic industry has remarkable advantages.
The needs of electronic product of new generation have been satisfied in the widespread use of SMT, have also proposed new requirement for the new electronic chemical product of exploitation.But surface mounting adhesive is the quick-setting single-component surface pasting adhesive of a kind of low temperature, is called for short Heraeus.Heraeus is one of material crucial in the surface installation technique, mainly is in wave soldering and solder reflow process, is used for components and parts are fixed on the printed circuit board, guarantees that components and parts do not take place to be shifted or to come off after mounting.The performance of Heraeus is that influence mounts the reliability of components and parts and the key factor of qualification rate.Usually, Heraeus should have that viscosity is low, thixotropy good, and cohesive strength height, high temperature resistant, good insulation preformance, set time is short and the storage time is long and good characteristics such as the colloidality put.
The surface mounting adhesive of one of main raw of using as SMT, its performance is to improve the key factor of assembling reliability and qualification rate.Have only and improve its stability and operability, could satisfy high-quality, a large amount of SMT, at a high speed, microminiaturized and unleaded requirement.The single-component surface pasting adhesive that on supermatic SMT production line, uses, except possessing characteristics such as strength of joint height, high temperature resistant, good insulation preformance, low temperature fast setting and storage time be long, also must have good operability, adapt to various attachment process.The specific performance of high-end Heraeus product requires as follows:
1), strength of joint: the SMT Heraeus must possess stronger strength of joint, after being cured, both having made under the temperature of solder fusing and has not also peeled off;
2), spot printing: Heraeus adopts the spot printing mode to the distribution means of printed board more at present, therefore requires Heraeus will adapt to various attachment process, and is easy to the feed rate of every kind of components and parts;
3), do not have hangover, slump: Heraeus is in case quilt is sticked on the pad, and components and parts just can't be realized being connected with the electric property of printed board, so Heraeus must not have hangover, the coating no slump in back when coating, in order to avoid pollute pad;
4), low temperature rapidly-curable: during curing, heat labile components and parts (LED, alminium electrolytic condenser etc.) also will pass through the reflow welding stove, so require condition of cure must satisfy low temperature, short period of time;
5), self aligning: in reflow welding, the pre-coat process, Heraeus solidifies earlier before solder fusing, fixing components and parts, so can hinder components and parts welding and oneself to adjust (dependence solder surface tension force carries out the self position correction);
6), satisfying envrionment test requires: the Heraeus cured article must satisfy high temperature resistant, the requirement of envrionment tests such as high humidity and acid and alkali-resistance.
Along with the SMT industry develops rapidly, the Heraeus demand constantly increases, and market potential is huge.The Heraeus that existing market is released, both can not accomplish fast setting, bonding strength height again the shelf lives stable, and remain to be improved at product stability and operability.Present performance requriements and market requirement situation, but be necessary to develop the quick-setting single-component surface pasting adhesive of a kind of low temperature, can accomplish the low temperature fast setting, cohesive strength height and shelf lives are stable, can satisfy the automatization requirement of using technology again.
Summary of the invention
The present invention for the existing surface mounting adhesive that solves can not low-temperature curing, unsettled technical problem of rudimentary shelf lives of cohesive strength, but a kind of low temperature fast setting, the shelf lives is stable, bonding force is high surface mounting adhesive are provided.
For solving the problems of the technologies described above, but the quick-setting surface mounting adhesive of low temperature that the present invention proposes is formed by the raw material configuration of following weight percentage:
Bisphenol-type epoxy resin-5.8～59 %,
Modified epoxy-5.8～59 %,
Toughner-2～10 %,
Latent curing agent-0.5～14.5%,
Promotor-1.5～10.5 %,
Thixotropic agent-20～59 %,
Coupling agent-1.1～10.8 %,
Mineral filler-0.5～14.8 %,
Pigment-0～6 %.
Surface mounting adhesive provided by the invention mainly is in wave soldering and solder reflow process, be used for components and parts are fixed in the printed board, generally distribute with some glue or steel mesh method of printing, to keep the position of components and parts on printed circuit board (PCB), guarantee that on fabrication line components and parts can not lost in the transport process, put into baking oven or Re-current welder heat hardening after sticking components and parts.It and so-called soldering paste are inequality, and after heat hardening, reheat can not dissolve yet, and that is to say, the heat embrittlement process of Heraeus is irreversible.The result of use of surface mounting adhesive can because of the thermofixation condition, be connected thing, employed equipment, operating environment difference variant.
Owing to adopted the said components proportioning, the present invention compared with prior art has the following advantages: 1. the shelf lives stablizes, and stores after 1 month in the time of 40 ℃, and the viscosity velocity of variation is 10%, and be 4 months the storage period under the room temperature, and be 8 months the storage period under 2-10 ℃; 2. viscosity is low, and thixotropy is good, and viscosity is the 5000-6000 centipoise, and thixotropy index is 7.5; 3. linear expansivity is low, 40-60ppm/ ℃; 4. curing speed is fast, 80 ℃ of curing in following 5 minutes; 5. shearing resistance is 16MPa.
Embodiment
The low viscosity that the present invention proposes, the underfill of low linear expansion coefficient can be formed by the raw material configuration of following weight percentage:
Bisphenol-type epoxy resin-5.8～59 %,
Modified epoxy-5.8～59 %,
Toughner-2～10 %,
Latent curing agent-0.5～14.5%,
Promotor-1.5～10.5 %,
Thixotropic agent-20～59 %,
Coupling agent-1.1～10.8 %,
Mineral filler-0.5～14.8 %,
Pigment-0～6 %.
Wherein, bisphenol-type epoxy resin can be selected bisphenol A type epoxy resin for use, as 828 Resins, epoxy of Shell Co. Ltd, and 331 Resins, epoxy of the Dow Chemical Company; Also can select bisphenol f type epoxy resin for use, as 862 Resins, epoxy of Shell Co. Ltd.Can also select Resins, epoxy such as dihydroxyphenyl propane D type, resol, organic carboxyl acid class glycidyl ether for use.Oxirane value is 0.45～0.8, and its molecular weight is 1000 to 5000.
Modified epoxy can obtain the dipentadiene Resins, epoxy of four-functional group type by dipentadiene modified bisphenol type Resins, epoxy, can improve the reactive behavior of resin like this, reduces temperature of reaction, improves thermotolerance simultaneously.
Toughner can be selected elastomer materials such as acrylic rubber, divinyl rubber, styrene butadiene ribber for use.The material of promptly can therefrom choosing any one kind of them also can select for use two or more material mixing to use.Toughner is used for reducing the linear expansivity of product, improves cementability.
Latent curing agent can select for use modified amine to add and thing or modified imidazole affixture, and wherein modified amine adds and the thing best results, and the PN-40 such as Japanese aginomoto company can effectively reduce curing reaction temperature.
Promotor can be selected trialkyl phosphates, mercaptobenzothiazole, a-mercaptobenzothiazole etc. for use.As trialkyl phosphates, the alkyl thing of C5-C10 is arranged, trioctylphosphine phosphoric acid salt also is to select preferably.In order to improve operation and security, addition between 0.1-40 or 1-30 weight for well.Can prevent pliability and reactive the reduction, will reduce, surpass 40 weight and then can reduce reactivity less than 0.1 weight additive effect.Particularly curing speed being required very highly under cryogenic situation, need to add curing catalyst, generally is to use the mercaptobenzothiazole that C7H5NS2 represents and dielectric substance or mixture low-temp reaction effect thereof can be better separately.
Thixotropic agent can be selected wilkinite for use, nanometer anhydride silica, at least a in the polyamide wax.If thixotropic effect of improving of binding agent is not very abundant, the components and parts confining force is low, and the components and parts before being heating and curing can produce problems such as displacement, and the caking agent angle of collapsing increases when solidifying simultaneously, and it is first-class that scolder just is difficult to stick to electrode of substrate.Add thixotropic agent and can improve a colloidality energy, can prevent the collapse expansion at angle of components and parts displacement and heating.
Coupling agent can be selected for use and select 3-Racemic glycidol propyl trimethoxy silicane, 3-Racemic glycidol propyl group methyl dimethoxysilane, propyl trimethoxy silicane, METHYL TRICHLORO SILANE, dimethyldichlorosilane(DMCS) etc.But wherein most effective is 3-Racemic glycidol propyl group methyl dimethoxysilane.When carrying out surface-treated, be in order to improve the affinity of thixotropic agent and Resins, epoxy, the dispersiveness and the moisture-proof thermotolerance of raising thixotropic agent, and resin flow with silane coupling agent.
Mineral filler can be selected the linear expansivity materials with smaller for use, such as, quartzy, synthetic silicon, silicon metal, aluminum oxide, boron nitride, magnesium oxide etc.Its median size is 2～10um, requires maximum particle diameter below 25um.Pigment can be selected the organic preferably red of thermotolerance for use.
Above-mentioned materials can buy in Chemicals manufacturer.
Further specify the present invention below by specific embodiment:
Embodiment 1
The raw material configuration of the following weight percentage of present embodiment forms:
862 Resins, epoxy 5.8%
Four-functional group type dipentadiene Resins, epoxy 29.6%
Acrylic rubber 2%
PN-40 solidifying agent 0.5%
Mercaptobenzothiazole 1.5%
Wilkinite 59%
3-glycidoxypropyltrimewasxysilane 1.1%
Aluminum oxide 0.5%
Embodiment 2
The weight percent of the underfill of the described low viscosity of present embodiment, low linear expansion coefficient is:
862 Resins, epoxy 16.1%
Four-functional group type dipentadiene Resins, epoxy 5.8%
Acrylic rubber 6%
PN-40 solidifying agent 14.5%
Mercaptobenzothiazole 6%
Nanometer anhydride silica 20%
3-glycidoxypropyltrimewasxysilane 10.8%
Aluminum oxide 14.8%
Red 6%
Embodiment 3
The weight percent of the underfill of the described low viscosity of present embodiment, low linear expansion coefficient is:
862 Resins, epoxy 32.4%
Four-functional group type dipentadiene Resins, epoxy 5.9%
Acrylic rubber 10%
PN-40 solidifying agent 7.5%
Trioctylphosphine phosphoric acid salt 10.5%
Nanometer anhydride silica 20%
3-glycidoxypropyltrimewasxysilane 6 %
Aluminum oxide 7.7 %
Embodiment 4
The weight percent of the underfill of the described low viscosity of present embodiment, low linear expansion coefficient is:
862 Resins, epoxy 59%
Four-functional group type dipentadiene Resins, epoxy 5.8%
Acrylic rubber 2%
PN-40 solidifying agent 0.5%
Mercaptobenzothiazole 1.5%
Polyamide wax powder 20%
3-glycidoxypropyltrimewasxysilane 1.1%
Aluminum oxide 7.1%
Red 3%
Embodiment 5
828 Resins, epoxy 5.8%
Four-functional group type dipentadiene Resins, epoxy 59%
Acrylic rubber 5%
PN-40 solidifying agent 0.5%
Trioctylphosphine phosphoric acid salt 3%
Nanometer anhydride silica 23.2%
3-glycidoxypropyltrimewasxysilane 3%
Aluminum oxide 0.5%
Embodiment 6
862 Resins, epoxy 5.8%
Four-functional group type dipentadiene Resins, epoxy 32.4%
Acrylic rubber 2%
PN-40 solidifying agent 1.3%
Mercaptobenzothiazole 1.5%
Polyamide wax powder 40%
3-glycidoxypropyltrimewasxysilane 6%
Aluminum oxide 8%
Red 3%
Prepare the surface mounting adhesive of low-temperature curable by the weight percent prescription of the foregoing description, earlier Resins, epoxy and mineral filler are carried out heat treated, and stir, dissolve, mix, disperse with planetary mixer simultaneously, thereby obtain this surface mounting adhesive, after with high speed dispersor compound being uniformly dispersed again, after the screening more than 100 orders is filtered, carry out vacuum defoamation and handle, at last by the filling machine can.Can and provide other material to prepare the surface mounting adhesive of low-temperature curable according to proportioning provided by the invention in addition.
The present invention is carried out performance test by the following method:
The wire drawing incidence: connect at 10000 and be coated with caking agents with the 0.12 second/speed of any with point gum machine on printed base plate, measure the wire drawing shape and count, (a point/10000 point)/100% is the wire drawing incidence.
The part offset distance: the IC assembly is installed on the printed base plate that has been coated with caking agent, and is installed additional the shake device, IC assembly miles of relative movement 1mm is the parts offset distance after 5 minutes.
Curing reaction temperature: (DSC) measures the solidified optimal reaction temperature with thermomechanical analyzer.
Curing reaction speed: measure 80 ℃ curing reaction time with thermomechanical analyzer (DSC).
Linear expansivity: with thermo-mechanical analysis (TMA) be determined at 80 degrees centigrade solidified in following 10 minutes and cured article come the testing wire coefficient of expansion.
Shearing force: make the 15mm*30mm shearing force and close the strong test piece of bonding force, the shearing force of testing its test piece with puller system.
The performance index gluing according to the surface mount of above testing method gained are as follows:
Wire drawing incidence (%): 0
Set time (80 ℃): 5 minutes
Linear expansivity (ppm/ ℃): 46
Component deviation distance (mm): 0.05
Solidification value (℃): 75
Shearing force: 17MPA
Thixotropy index: 7.5
Owing to adopted the said components proportioning, the present invention has the following advantages: 1. the shelf lives stablizes, and stores after 1 month in the time of 40 ℃, and the viscosity velocity of variation is 10%, and be 4 months the storage period under the room temperature, and be 8 months the storage period under 2-10 ℃; 2. thixotropy is good, no wire drawing; 3. linear expansivity is low, 40-60ppm/ ℃; 4. curing speed is fast, and 5. 80 ℃ solidified in following 5 minutes that shearing resistance is 17MPa.
Claims (9)
1. but the quick-setting surface mounting adhesive of low temperature is characterized in that, is formed by the configuration of the raw material of following weight percentage:
Bisphenol-type epoxy resin-5.8～59 %,
Modified epoxy-5.8～59 %,
Toughner-2～10 %,
Latent curing agent-0.5～14.5%,
Promotor-1.5～10.5 %,
Thixotropic agent-20～59 %,
Coupling agent-1.1～10.8 %,
Mineral filler-0.5～14.8 %,
Pigment-0～6 %.
2. surface mounting adhesive according to claim 1, it is characterized in that, described bisphenol-type epoxy resin is a kind of in bisphenol A-type, dihydroxyphenyl propane D type, Bisphenol F type, resol, the organic carboxyl acid class glycidyl ether, oxirane value is 0.45～0.8, and its molecular weight ranges is 1000～5000.
3. surface mounting adhesive according to claim 1 is characterized in that, described modified epoxy is a four-functional group type dipentadiene Resins, epoxy.
4. surface mounting adhesive according to claim 1 is characterized in that, described toughner is a kind of of acrylonitrile butadiene rubber, divinyl rubber, acrylic rubber.
5. surface mounting adhesive according to claim 1 is characterized in that, described latent curing agent is that modified amine adds and thing or modified imidazole affixture.
6. surface mounting adhesive according to claim 1 is characterized in that, described promotor is a kind of in trialkyl phosphates, mercaptobenzothiazole, a-mercaptobenzothiazole.
7. surface mounting adhesive according to claim 1 is characterized in that, described thixotropic agent is a kind of in wilkinite, nanometer anhydride silica, the polyamide wax.
8. surface mounting adhesive according to claim 1, it is characterized in that described coupling agent is any in 3-Racemic glycidol propyl trimethoxy silicane, 3-Racemic glycidol propyl group methyl dimethoxysilane, propyl trimethoxy silicane, METHYL TRICHLORO SILANE, the dimethyldichlorosilane(DMCS).
9. surface mounting adhesive according to claim 1 is characterized in that the median size of described mineral filler is 2～10um, and maximum particle diameter is below 25um.
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| CN103059749A (en) * | 2013-02-03 | 2013-04-24 | 张延� | Preparation method of modified silicate inorganic adhesive |
| CN103059748A (en) * | 2013-02-03 | 2013-04-24 | 梁建波 | Modified silicate inorganic adhesive |
| CN103073999A (en) * | 2013-02-03 | 2013-05-01 | 韩敏杰 | Water-resistant inorganic bonding agent |
| CN103073998A (en) * | 2013-02-03 | 2013-05-01 | 王康 | Preparation method of water-resistant inorganic bonding agent |
| CN103409095A (en) * | 2013-07-30 | 2013-11-27 | 烟台德邦科技有限公司 | Flexible one-component epoxy adhesive and preparation method thereof |
| CN103773297A (en) * | 2014-01-10 | 2014-05-07 | 江苏德威涂料有限公司 | Epoxy adhesive |
| CN103952109A (en) * | 2014-04-21 | 2014-07-30 | 苏州之诺新材料科技有限公司 | Carbon nano modified vehicle one-component structure adhesive and preparation method thereof |
| CN104073193A (en) * | 2013-03-27 | 2014-10-01 | 南京喜力特胶粘剂有限公司 | Thermal conductive adhesive and preparing method thereof |
| CN105201132A (en) * | 2015-08-06 | 2015-12-30 | 安徽铭源新型建材科技有限公司 | Wallboard with excellent mechanical property, good bonding effect and low peeling possibility |
| CN108219728A (en) * | 2018-01-10 | 2018-06-29 | 深圳市邦大科技有限公司 | A kind of Halogen is without sulphur patch red glue and preparation method thereof |
| CN108641645A (en) * | 2018-03-29 | 2018-10-12 | 江苏矽时代材料科技有限公司 | A kind of encapsulating semiconductor packaging plastic and preparation method thereof |
| CN109082253A (en) * | 2018-06-25 | 2018-12-25 | 南亚新材料科技股份有限公司 | A kind of halogen-free adhesive of polymolecularity and preparation method thereof |
| CN110248496A (en) * | 2019-05-31 | 2019-09-17 | 深圳市英创立电子有限公司 | A kind of pcb board attachment process and the Heraeus for applying to the attachment process |
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| CN111019578A (en) * | 2019-12-26 | 2020-04-17 | 深圳德邦界面材料有限公司 | Epoxy resin heat-conducting adhesive sheet and preparation method thereof |
| CN112646523A (en) * | 2020-12-23 | 2021-04-13 | 重庆德天汽车新材料研究院有限公司 | High-performance medium-temperature curing single-component epoxy structural adhesive and preparation method thereof |
| CN115651579A (en) * | 2022-11-02 | 2023-01-31 | 杭州之江有机硅化工有限公司 | Epoxy adhesive capable of being rapidly cured and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103059748A (en) * | 2013-02-03 | 2013-04-24 | 梁建波 | Modified silicate inorganic adhesive |
| CN103073999A (en) * | 2013-02-03 | 2013-05-01 | 韩敏杰 | Water-resistant inorganic bonding agent |
| CN103073998A (en) * | 2013-02-03 | 2013-05-01 | 王康 | Preparation method of water-resistant inorganic bonding agent |
| CN103059749A (en) * | 2013-02-03 | 2013-04-24 | 张延� | Preparation method of modified silicate inorganic adhesive |
| CN104073193A (en) * | 2013-03-27 | 2014-10-01 | 南京喜力特胶粘剂有限公司 | Thermal conductive adhesive and preparing method thereof |
| CN103409095A (en) * | 2013-07-30 | 2013-11-27 | 烟台德邦科技有限公司 | Flexible one-component epoxy adhesive and preparation method thereof |
| CN103409095B (en) * | 2013-07-30 | 2015-04-15 | 烟台德邦科技有限公司 | Flexible one-component epoxy adhesive and preparation method thereof |
| CN103773297B (en) * | 2014-01-10 | 2016-05-18 | 江苏德威涂料有限公司 | Epoxy adhesive |
| CN103773297A (en) * | 2014-01-10 | 2014-05-07 | 江苏德威涂料有限公司 | Epoxy adhesive |
| CN103952109A (en) * | 2014-04-21 | 2014-07-30 | 苏州之诺新材料科技有限公司 | Carbon nano modified vehicle one-component structure adhesive and preparation method thereof |
| CN105201132A (en) * | 2015-08-06 | 2015-12-30 | 安徽铭源新型建材科技有限公司 | Wallboard with excellent mechanical property, good bonding effect and low peeling possibility |
| CN108219728A (en) * | 2018-01-10 | 2018-06-29 | 深圳市邦大科技有限公司 | A kind of Halogen is without sulphur patch red glue and preparation method thereof |
| CN108641645A (en) * | 2018-03-29 | 2018-10-12 | 江苏矽时代材料科技有限公司 | A kind of encapsulating semiconductor packaging plastic and preparation method thereof |
| CN109082253A (en) * | 2018-06-25 | 2018-12-25 | 南亚新材料科技股份有限公司 | A kind of halogen-free adhesive of polymolecularity and preparation method thereof |
| CN110248496A (en) * | 2019-05-31 | 2019-09-17 | 深圳市英创立电子有限公司 | A kind of pcb board attachment process and the Heraeus for applying to the attachment process |
| CN110499120A (en) * | 2019-09-02 | 2019-11-26 | 中国科学院深圳先进技术研究院 | A kind of delustering agent and preparation method thereof, the underfill comprising it and application |
| CN111019578A (en) * | 2019-12-26 | 2020-04-17 | 深圳德邦界面材料有限公司 | Epoxy resin heat-conducting adhesive sheet and preparation method thereof |
| CN112646523A (en) * | 2020-12-23 | 2021-04-13 | 重庆德天汽车新材料研究院有限公司 | High-performance medium-temperature curing single-component epoxy structural adhesive and preparation method thereof |
| CN115651579A (en) * | 2022-11-02 | 2023-01-31 | 杭州之江有机硅化工有限公司 | Epoxy adhesive capable of being rapidly cured and preparation method thereof |
| CN115651579B (en) * | 2022-11-02 | 2024-01-26 | 杭州之江有机硅化工有限公司 | Epoxy adhesive capable of being rapidly cured and preparation method thereof |
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