CN103881310A - Halogen-free environment-friendly epoxy resin envelope material for thermistors and application thereof - Google Patents
Halogen-free environment-friendly epoxy resin envelope material for thermistors and application thereof Download PDFInfo
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- CN103881310A CN103881310A CN201410145782.8A CN201410145782A CN103881310A CN 103881310 A CN103881310 A CN 103881310A CN 201410145782 A CN201410145782 A CN 201410145782A CN 103881310 A CN103881310 A CN 103881310A
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Abstract
The invention provides a halogen-free environment-friendly epoxy resin envelope material for thermistors, which is prepared from the following components in parts by weight: 80-100 parts of epoxy resin additive, 40-60 parts of ammonia curing agent, 40-80 parts of epoxy resin additive and 1-10 parts of filler. The envelope material has the characteristics of long service life, excellent operability, shorter curing time and the like. The cured product has the advantages of favorable gloss, excellent moisture resistance and excellent weather resistance.
Description
Technical field
The present invention relates to the epoxy resin enclosed material of a kind of halogen-free environmental, specifically, relate to a kind of epoxy resin enclosed material and application for halogen-free environmental thermistor.
Background technology
In recent years, along with mobile intelligent, lighting, the development of battery request high capacity, the speed that mobile phone updates is very fast.Because European Union has proposed the restriction to content of halogen in electronic product components and parts to the protection of environment.Market not only proposes product can not be halogen-containing, and in RoHS report, forbid that six grand duke's harmful substances occur.Also more and more higher to the desired performance index of thermistor epoxy resin used like this, require the electrical property of electronic devices and components not change simultaneously.
Therefore, need to research and develop further a kind of novel epoxy resin enclosed material of halogen-free environmental thermistor, not only meet market demands, also there is good bonding strength and good heatproof weather resisteant energy simultaneously.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide the epoxy resin enclosed material of a kind of halogen-free environmental thermistor.
Another object of the present invention is to provide the preparation method of the epoxy resin enclosed material of this halogen-free environmental thermistor.
A further object of the present invention is to provide the application of the epoxy resin enclosed material of this halogen-free environmental thermistor.
In order to realize the object of the invention, the invention provides the epoxy resin enclosed material of a kind of halogen-free environmental thermistor: the component by following weight part forms:
Wherein, described epoxy resin host is bisphenol A type epoxy resin, and epoxy equivalent (weight) is 185-195g/mol, and 25 DEG C of viscosity are 20000 ± 5000cps, and cl content is less than 500ppm.
Preferably, described bisphenol A type epoxy resin is 128K, YD127 or KDS8128, and epoxy equivalent (weight) is at 185-195g/mol, and 25 DEG C of viscosity are 20000 ± 5000cps, cl content 350ppm.
Described Ammonia solidifying agent is one or more in mphenylenediamine, diaminodiphenylmethane or diamino diphenyl sulfone, and 25 DEG C of viscosity are 750 ± 250cps.
Preferably, described Ammonia solidifying agent is mphenylenediamine or diaminodiphenylmethane, and 25 DEG C of viscosity are 750 ± 250cps.
Described epoxy resin additive is one or more in vinylbenzene, dimethyl phthalate, diethyl phthalate, dioctyl phthalate (DOP), diamyl phthalate, and 25 DEG C of viscosity are 5-15pcs.
Preferably, described epoxy resin additive is vinylbenzene, diethyl phthalate or diamyl phthalate, and 25 DEG C of viscosity are 5-10pcs.
Described filler is one or more of aluminum oxide, calcium carbonate, talcum powder, aerosil or silica powder, and particle diameter is 5-10um.
Preferably, described filler is aluminum oxide or calcium carbonate, and particle diameter is 5-8.5um.
Ammonia solidifying agent of the present invention is compared with existing conventional acid anhydride type curing agent, Ammonia solidifying agent shows better resistance to medium and moisture resistance properties, Ammonia solidifying agent reacts and has larger cross-linking density with epoxy resin in addition, therefore show better oxygen-barrier property.
Filler of the present invention can improve hardness and the bonding force of material, and different filler hardness is different with bonding force; And the size of filler also can affect the oxygen-barrier property of material.
Epoxy resin additive of the present invention can regulate the viscosity of resin, can improve the perviousness of resin.
The described epoxy resin enclosed material of halogen-free environmental thermistor, epoxy resin mixes viscosity at 500 ± 250cps according at 25 DEG C of corresponding proportionings, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth more than 3.5.
The preparation method of epoxy resin enclosed material for halogen-free environmental thermistor of the present invention, comprises the steps:
First in proportion epoxy resin host, epoxy resin additive and filler are carried out to mix and blend 30-60 minute, after froth breaking, add Ammonia solidifying agent to stir 30-60 minute, then carry out defoaming treatment.
Need in use the epoxy resin enclosed material of halogen-free environmental thermistor to dry 1.5-2 hour at 90-120 DEG C, become cured epoxy resin encapsulating material.
Described defoaming treatment employing-76mmHg vacuum defoamation 30 minutes.
Wherein, preferred preparation process is as follows:
First by epoxy resin host, epoxy resin additive and filler according to proportioning mix and blend 30 minutes, in-76mmHg vacuum defoamation after 30 minutes; Add Ammonia solidifying agent to stir 30 minutes according to proportioning again, in-76mmHg vacuum defoamation must mixture of epoxy resins after 30 minutes.
Then, will be stirred epoxy resin pours a glue groove into (the wide * height of long * is: 15cm*15cm*3cm); Finally, glue groove is placed in to baking oven 90-120 DEG C and dries 1.5-2 hour, obtain cured epoxy resin encapsulating material.
Halogen-free environmental thermistor of the present invention is the application at the encapsulating material for as thermistor chip and other electronic devices and components with epoxy resin enclosed material.
Halogen-free environmental thermistor of the present invention has the following advantages with epoxy resin enclosed material tool:
1) halogen-free environmental thermistor of the present invention is not halogen-containing with epoxy resin enclosed material, six grand duke's harmful substances of not forbidding containing current RoHS, and it is long that it has the serviceable time, operability excellence, the feature such as set time is relatively short, and solidification value is suitable.And the good luster of cured article, wet fastness and air barrier excellent performance.
2) halogen-free environmental thermistor of the present invention is mainly used in sealing of thermistor chip and other electronic devices and components with epoxy resin enclosed material, and the bonding strength between itself and thermistor is good, and heatproof weather resisteant can be good.
3) the epoxy resin enclosed material that the present invention makes, after hot setting, strong with the interface binding power of metal in electronic devices and components, the water rate of permeation of epoxy resin is low, and oxygen barrier property is good.
Embodiment
Further describe the present invention with embodiment below, be conducive to the understanding to the present invention and advantage thereof, better effects if, but described embodiment is only for illustrating the present invention instead of restriction the present invention.
Embodiment 1
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
100 weight part bisphenol A epoxide resin host 128K, epoxy equivalent (weight) is at 190g/mol, and 25 DEG C of viscosity are 20000cps, and cl content is 350ppm.
40 weight part mphenylenediamine solidifying agent, 25 DEG C of viscosity are 750cps;
60 parts by weight of styrene additives, 25 DEG C of viscosity are 1cps;
10 weight part pearl fillers, particle diameter is 5um.
Its preparation process is as follows: first by epoxy resin host, epoxy resin additive and filler according to proportioning mix and blend 30 minutes, in-76mmHg vacuum defoamation after 30 minutes; Add Ammonia solidifying agent to stir 30 minutes according to mixing match again, in-76mmHg vacuum defoamation must mixture of epoxy resins after 30 minutes.Then, will be stirred epoxy resin and pour a glue groove into, the wide * height of long * is: 15cm*15cm*3cm; Finally, glue groove is placed in to 120 DEG C, baking oven and dries 1.5 hours, obtain cured epoxy resin encapsulating material, through sanding and polishing, cutting into thickness is 1.5mm, and the sample that area is 100cm2, shown in moisture-proof and weather resisteant test performance table 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 600cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.7.
Embodiment 2
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
80 weight part bisphenol A epoxide resin host 128K, epoxy equivalent (weight) is at 190g/mol, and 25 DEG C of viscosity are 20000cps, and cl content is 350ppm.
60 weight part mphenylenediamine solidifying agent, 25 DEG C of viscosity are 750cps;
40 parts by weight of styrene additives, 25 DEG C of viscosity are 1cps;
5 weight part pearl fillers, particle diameter is 5um;
Other processes and parameter are with embodiment 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 650cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.5.
Embodiment 3
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
100 weight part bisphenol A epoxide resin hosts, 128K, epoxy equivalent (weight) is at 190g/mol, and 25 DEG C of viscosity are 20000cps, and cl content is 350ppm.
50 weight part mphenylenediamine solidifying agent, 25 DEG C of viscosity are 750cps;
80 weight part diethyl phthalate additives, 25 DEG C of viscosity are 1cps;
1 weight part pearl filler, particle diameter is 5um;
Other processes and parameter are with embodiment 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 540cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.64.
Embodiment 4
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
95 weight part bisphenol A epoxide resin host KDS8128, epoxy equivalent (weight) is at 195g/mol, and 25 DEG C of viscosity are 25000cps, and cl content is 350ppm.
45 weight part diaminodiphenyl-methane solidifying agent, 25 DEG C of viscosity are 750cps;
40 weight part dimethyl phthalate additives, 25 DEG C of viscosity are 1cps;
5 weight part pearl fillers, particle diameter is 5um;
Other processes and parameter are with embodiment 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 500cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.6.
Embodiment 5
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
95 weight part bisphenol A epoxide resin host KDS8128, epoxy equivalent (weight) is at 195g/mol, and 25 DEG C of viscosity are 25000cps, and cl content is 350ppm.
45 weight part diamino diphenyl sulfone solidifying agent, 25 DEG C of viscosity are 750cps;
80 weight part diamyl phthalate additives, 25 DEG C of viscosity are 1cps;
10 weight part alumina packings, particle diameter is 5um;
Other processes and parameter are with embodiment 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 750cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.8.
Embodiment 6
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
95 weight part bisphenol A epoxide resin host KDS8128, epoxy equivalent (weight) is at 195g/mol, and 25 DEG C of viscosity are 25000cps, and cl content is 350ppm.
45 weight part meta phenylene diamine solidifying agent, 25 DEG C of viscosity are 750cps;
60 parts by weight of styrene additives, 25 DEG C of viscosity are 1cps;
10 weight part pearl fillers, particle diameter is 10um;
Other processes and parameter are with embodiment 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 450cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.5.
Embodiment 7
The epoxy resin enclosed material of halogen-free environmental thermistor of the present embodiment, it comprises:
100 weight part bisphenol A epoxide resin host YD127, epoxy equivalent (weight) is at 185g/mol, and 25 DEG C of viscosity are 18000cps, and cl content is 350ppm.
40 weight part meta phenylene diamine solidifying agent, 25 DEG C of viscosity are 750cps;
75 parts by weight of styrene additives, 25 DEG C of viscosity are 1cps;
9.5 weight part pearl fillers, particle diameter is 8um;
Other processes and parameter are with embodiment 1.
The epoxy resin enclosed material of the present embodiment halogen-free environmental thermistor, mixed mixing viscosity is at 450cps at 25 DEG C, and the 25 DEG C of thixotropy indexs (Ti) after cooperation are worth 3.7.
Comparative example
The epoxy resin enclosed material of a kind of halogen-free environmental thermistor, it comprises:
100 weight part bisphenol A epoxide resin host 128K, epoxy equivalent (weight) is at 190g/mol, and 25 DEG C of viscosity are 20000cps, and cl content is 1200ppm;
40 weight part phthalic acid anhydride curing agents, 25 DEG C of viscosity are 750cps;
60 parts by weight of styrene additives, 25 DEG C of viscosity are 1cps;
5 weight part pearl fillers, particle diameter is 5um;
First by epoxy resin host, epoxy resin additive and filler according to proportioning mix and blend 30 minutes, in-76mmHg vacuum defoamation after 30 minutes; Add Ammonia solidifying agent to stir 30 minutes according to mixing match again, in-76mmHg vacuum defoamation must mixture of epoxy resins after 30 minutes.Then, will be stirred mixture of epoxy resins and pour a glue groove into, the wide * height of long * is: 15cm*15cm*3cm; Finally, glue groove is placed in to 120 DEG C, baking oven and dries 1.5 hours, obtain cured epoxy resin encapsulating material, through sanding and polishing, cutting into thickness is 1.5mm, the sample that area is 100cm2.
Shown in the moisture-proof of embodiment and comparative example and weather resisteant test performance table 1.
Table 1
Table 1 is the performance characteristic of embodiment 1-7 and the epoxy resin enclosed material of comparative example.
Water vapor transmittance: sample area 50cm
2, thickness is 1.5mm, adopts moisture vapor transmission cup weighting method, the parameters such as the water vapor transmission rate (WVTR) of sample are obtained in test, judge the performance of material steam penetrating capacity with this.
Gas permeation rate: sample area 100cm
2, thickness is 2mm, by pressing subtraction to measure gas by the amount of material.
As can be seen from Table 1, embodiment 1,2,3 compares with comparative example, and in identical epoxy resin host situation, in the time that solidifying agent is Ammonia epoxy resin, the water vapor transmittance of material and gas permeation rate are all little than acid anhydride type curing agent; Under epoxy resin host and solidifying agent same case, the proportioning difference between them, the cross-linking density difference of epoxy resin, therefore the ventilation property of material and water-permeable are also different, by comparing embodiment 1,2,3, embodiment 2 performance the bests; In the time that epoxy resin host is identical, the kind of solidifying agent also affects the water-permeable of material, finds by comparing embodiment 1,4,5, and embodiment 1 is better than embodiment 4 and 5 performances; On the other hand, the particle diameter of filler also affects material permeability, finds by comparing embodiment 1,6,7, and embodiment 1 over-all properties is better.
The above; it is only preferred embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; do not departing under the prerequisite of the inventive method, also can make some improvement and supplement, these improvement and the supplementary protection scope of the present invention that also should be considered as.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change of making when utilizing disclosed above technology contents, the equivalent variations of modifying and developing, be equivalent embodiment of the present invention; Meanwhile, the change of any equivalent variations that all foundations essence technology of the present invention is done above-described embodiment, modification and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (10)
1. the epoxy resin enclosed material of halogen-free environmental thermistor, is characterized in that, its component by following weight part forms:
2. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 1, is characterized in that, its component by following weight part forms:
3. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 1 and 2, it is characterized in that, described epoxy resin host is bisphenol A type epoxy resin host, and epoxy equivalent (weight) is 185-195g/mol, 25 DEG C of viscosity are 20000 ± 5000cps, and cl content is for being less than 500ppm.
4. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 1 and 2, it is characterized in that, described Ammonia solidifying agent is one or more of mphenylenediamine, diaminodiphenylmethane, diamino diphenyl sulfone, and 25 DEG C of viscosity are 750 ± 250cps.
5. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 4, is characterized in that, described Ammonia solidifying agent is mphenylenediamine or diaminodiphenylmethane, and 25 DEG C of viscosity are 750 ± 250cps.
6. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 1 and 2, it is characterized in that, described epoxy resin additive is one or more of vinylbenzene, dimethyl phthalate, diethyl phthalate, dioctyl phthalate (DOP), diamyl phthalate, and 25 DEG C of viscosity are 5-15pcs.
7. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 1 and 2, is characterized in that, described epoxy resin additive is vinylbenzene, diethyl phthalate or diamyl phthalate, and 25 DEG C of viscosity are 5-10pcs.
8. the epoxy resin enclosed material of halogen-free environmental thermistor according to claim 1 and 2, is characterized in that, described filler is one or more of aluminum oxide, calcium carbonate, talcum powder, aerosil, silica powder, and particle diameter is 5-10um; Be preferably aluminum oxide or talcum powder, particle diameter is 5-8.5um.
9. prepare the method for the epoxy resin enclosed material of halogen-free environmental thermistor described in claim 1-8 any one, it is characterized in that, first in proportion epoxy resin host, epoxy resin additive and filler are carried out to mix and blend 30-60 minute, after froth breaking, add Ammonia solidifying agent to stir 30-60 minute, then carry out defoaming treatment.
10. halogen-free environmental thermistor application at the encapsulating material for as thermistor chip and other electronic devices and components with epoxy resin enclosed material described in claim 1-8 any one.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410145782.8A CN103881310A (en) | 2014-04-11 | 2014-04-11 | Halogen-free environment-friendly epoxy resin envelope material for thermistors and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410145782.8A CN103881310A (en) | 2014-04-11 | 2014-04-11 | Halogen-free environment-friendly epoxy resin envelope material for thermistors and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105648267A (en) * | 2016-03-30 | 2016-06-08 | 广东合科泰实业有限公司 | Low-temperature-coefficient resistor body, preparation method of low-temperature-coefficient resistor body and low-temperature-coefficient resistor with low-temperature-coefficient resistor body |
| CN108342147A (en) * | 2018-02-26 | 2018-07-31 | 上海闰龙电子材料有限公司 | A kind of formula and preparation method thereof of thermistor isolation protective material |
| CN108570213A (en) * | 2017-03-10 | 2018-09-25 | 味之素株式会社 | Resin composition layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1908108A (en) * | 2005-08-05 | 2007-02-07 | 比亚迪股份有限公司 | Encapsulating material and method for making same |
| CN101173159A (en) * | 2006-11-02 | 2008-05-07 | 比亚迪股份有限公司 | Epoxy resin encapsulating material composition |
| CN101817969A (en) * | 2010-04-08 | 2010-09-01 | 长兴华强电子有限公司 | Dipping material for capacitor of energy-saving lamp |
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2014
- 2014-04-11 CN CN201410145782.8A patent/CN103881310A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1908108A (en) * | 2005-08-05 | 2007-02-07 | 比亚迪股份有限公司 | Encapsulating material and method for making same |
| CN101173159A (en) * | 2006-11-02 | 2008-05-07 | 比亚迪股份有限公司 | Epoxy resin encapsulating material composition |
| CN101817969A (en) * | 2010-04-08 | 2010-09-01 | 长兴华强电子有限公司 | Dipping material for capacitor of energy-saving lamp |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105648267A (en) * | 2016-03-30 | 2016-06-08 | 广东合科泰实业有限公司 | Low-temperature-coefficient resistor body, preparation method of low-temperature-coefficient resistor body and low-temperature-coefficient resistor with low-temperature-coefficient resistor body |
| CN108570213A (en) * | 2017-03-10 | 2018-09-25 | 味之素株式会社 | Resin composition layer |
| CN108342147A (en) * | 2018-02-26 | 2018-07-31 | 上海闰龙电子材料有限公司 | A kind of formula and preparation method thereof of thermistor isolation protective material |
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Application publication date: 20140625 |