CN104804192A - Preparation method of MQ branched-chain modified silicon resin polymer for large-scale integrated circuit package - Google Patents
Preparation method of MQ branched-chain modified silicon resin polymer for large-scale integrated circuit package Download PDFInfo
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- CN104804192A CN104804192A CN201510143900.6A CN201510143900A CN104804192A CN 104804192 A CN104804192 A CN 104804192A CN 201510143900 A CN201510143900 A CN 201510143900A CN 104804192 A CN104804192 A CN 104804192A
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Abstract
The invention discloses a preparation method of an MQ branched-chain modified silicon resin polymer for large-scale integrated circuit package. Alpha, omega-dyhydroxyl polydimethylsiloxane or alpha, omega-hydroxyl poly(dimethyl-methyl vinyl) silicon dioxide is taken as a main raw material, methyl vinyl MQ silicon resin with the value of M/Q value being 0.6-0.9 or methyl MQ silicon resin is taken as an auxiliary raw material, the mixture is stirred to have a reaction for 45 minutes at the rotation speed of 70 revolutions per minute, the temperature is raised to 50-130 DEG C, and the temperature rising rate is 2 DEG C per minute; sodium trimethylsilanol or potassium trimethylsilanol accounting for 0.01%-0.1% of the main raw material by mass is added to serve as a catalyst, the mixture is stirred for 1-4 hours at the constant temperature, and a target product is obtained. The tensile strength, the impact strength and the adhesive property of the polymer prepared with the method are excellent, the resistance is higher than 1,013 omega, the heat conductivity is lower than 1.40 W/mK, the silicon resin polymer can resist radiation not lower than 109 rad, and the elasticity is good.
Description
Technical field
The invention belongs to lsi package field of material technology, particularly a kind of preparation method for lsi package MQ side chain modified silicone resin polymkeric substance.
Background technology
Packaged material is on performance, the stability of unicircuit and have great impact work-ing life.Particularly for large-scale integrated circuit, because of its at a high speed, the feature such as multi-functional and microminiaturized, under long-term big current working conditions, packaged material very easily carbonization, forms conductive channel at device surface, causes component failure.At present for the epoxide resin material of lsi package, after solidification, cross-linking density is high, internal stress is large, fragility is large, poor impact resistance, and transparency raises with temperature and declines, and during more than 150 DEG C, carburizing reagent occurs.
MQ silicone resin is made up of simple function chain link (R3SiO1/2 and M) and four sense chain links (SiO4/2 and Q), the hybrid organopolysiloxane that structure comparison is special.It is generally acknowledged, MQ resin is the tight spherule of double-deck three-dimensional structure, centre of sphere part be link with Si-O chain, higher, the polymerization degree of density is the caged SiO2 of 15 ~ 50; A spherical shell part surround by the less R3SiO1/2 layer of density.MQ silicone resin has half special inorganic half organic structure, and the R on simple function chain link is except for except methyl, can also be vinyl, hydrogen base, epoxy group(ing), gives the different reactive behavior of MQ resin and other performance.MQ silicone resin is mainly used as organic pressure-sensitive gel, liquid silastic, personal care articles and other auxiliary agent etc.
Silicone resin material is except having the advantages such as excellent wear resistance, scale resistance, resistant of high or low temperature, radiation resistance, weathering resistance, insulativity, hydrophobic nature and low surperficial potential energy, also have superior electric property, as low in dielectric loss, proof voltage, resistance to electric arc, Inverter fed motor, volume resistivity is high and surface resistivity is high.The main deficiency existed is that tensile strength, shock strength and adhesive property are poor.
Therefore, necessary on the basis of prior art a kind of preparation method that can significantly improve the polymer organic silicium encapsulating material of tensile strength, shock strength and cohesive strength of R & D design.
Summary of the invention
Goal of the invention: the object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method being applicable to the silicone resin material of lsi package is provided, the method is with α, alpha, omega-dihydroxy polydimethyl siloxane or α, poly-(dimethyl-methyl vinyl) siloxanes of ω-hydroxyl is main raw material, with methyl vinyl MQ silicon resin or methyl MQ silicone resin for auxiliary material, by controlling reaction raw materials proportioning, reaction times, temperature and catalyst levels regulate and control the structure of product, thus ensure that material property reaches lsi package processing requirement.
Technical scheme: for realizing above object, the technical scheme that the present invention takes is:
For a preparation method for lsi package MQ side chain modified silicone resin polymkeric substance, the method comprises the following steps,
The first step, by main raw material 65 ~ 95 parts of α, alpha, omega-dihydroxy polydimethyl siloxane or poly-(dimethyl-methyl vinyl) siloxanes of α, ω-hydroxyl join in reactor;
Second step, according to mass parts, gets 5-35 part methyl vinyl MQ silicon resin or reactor put into by methyl MQ silicone resin, and open stirring 45 ~ 60 minutes, rotating speed is 70 ~ 100 revs/min, is warming up to 50-130 DEG C, and temperature rise rate is 2 ~ 3 DEG C/min;
3rd step, after all even temperature-stable of above-mentioned material mixing, according to main raw material α, alpha, omega-dihydroxy polydimethyl siloxane or α, the 0.01-0.1% of poly-(dimethyl-methyl vinyl) the siloxanes mass parts of ω-hydroxyl adds catalyzer, and constant temperature stirs 1-4 hour, and question response thing stops heating after becoming transparent colloid, continue to be stirred to cooling room temperature, namely obtain the encapsulation polymkeric substance of target product.
Preferably, the above-described preparation method for lsi package MQ side chain modified silicone resin polymkeric substance, described α, it is 5-30 that alpha, omega-dihydroxy polydimethyl siloxane or α, ω-hydroxyl gather polymerization degree scope in (dimethyl-methyl vinyl) siloxanes; Consumption is 70 ~ 100 mass parts.
Preferably, the above-described preparation method for lsi package MQ side chain modified silicone resin polymkeric substance, describedly state M/Q in methyl vinyl MQ silicon resin or methyl MQ silicone resin (M is single functionality siloxane chain joint number, Q is four functionality siloxane polycondensation chain numbers) ratio range is 0.6-0.9, is 2.0-4.0% at methyl vinyl MQ silicon resin medium vinyl percentage composition.MQ resin structure following (linear polymer A, or cyclic polymer B, or cross-linked polymer C):
Linear polymer A:
Cyclic polymer B:
Cross-linked polymer C:
Preferably, the above-described preparation method for lsi package MQ side chain modified silicone resin polymkeric substance, described catalyzer is trimethyl silicane sodium alkoxide or trimethyl silicane potassium alcoholate.The present invention filters out best catalyzer by great many of experiments, can improve reaction efficiency, ensures stable reaction.
Beneficial effect: compared to the prior art the preparation method for lsi package MQ side chain modified silicone resin polymkeric substance provided by the invention has the following advantages:
1. the present invention is screened by great many of experiments, select α, alpha, omega-dihydroxy polydimethyl siloxane or α, alpha, omega-dihydroxy polydimethyl siloxane is raw material, can ensure that product has excellent weathering resistance and electric property, by adding preferred auxiliary material methyl vinyl MQ silicon resin or methyl MQ silicone resin, effectively can improve the tensile strength of product, shock strength and adhesive property, thus polymer organic silicone resin can be strengthened as vibrations buffering during packaged material, impact damping and cohesive strength, and it is high to have resistance, thermal conductivity is low, the advantages such as radiation-resistant property is strong.
2. the preferred whole preparation technology of the present invention, step is few, simple to operate, reaction conditions is gentle, production cost is low, is applicable to large-scale industrial production.
Embodiment
The present invention relates to the method preparing polymer organic silicone material.The method is with α, alpha, omega-dihydroxy polydimethyl siloxane or α, poly-(dimethyl-methyl vinyl) siloxanes of ω-hydroxyl is main raw material, with methyl vinyl MQ silicon resin or methyl MQ silicone resin for auxiliary material, add a small amount of trimethyl silicane sodium alkoxide or trimethyl silicane potassium alcoholate as catalyzer, regulate and control the structure of product by controlling reaction raw materials proportioning, reaction times, temperature and catalyst levels, thus ensure that material property reaches lsi package processing requirement.
Below in conjunction with embodiment, the present invention is described in further detail, but working of an invention mode is not limited thereto.
Embodiment 1
According to mass fraction, getting 70 parts of polymerization degree is the α of 10, the methyl vinyl MQ silicon resin (linear polymer A) that alpha, omega-dihydroxy polydimethyl siloxane and 30 parts of M/Q values are 0.7, contents of ethylene is 3.0% puts into reactor, open stirring 25 minutes, rotating speed is 75 revs/min, be warming up to 90 DEG C, temperature rise rate is 2 DEG C/min; Until system mix with temperature-stable after, according to α, 0.03% of alpha, omega-dihydroxy polydimethyl siloxane mass parts adds trimethyl silicane potassium alcoholate as catalyzer, constant temperature stirs 2.5 hours, question response thing stops heating after becoming transparent colloid, continues to be stirred to cooling room temperature, namely obtains product 1, and properties detection is carried out to product, detected result is as shown in table 1:
The main performance index of table 1 product 1
| Performance title | Performance perameter |
| Body resistance | 3.21×10 13Ω |
| Thermal conductivity | 1.31W/mK |
| Irradiation can be tolerated | 5.23×10 9rad |
| Tensile strength | 161kg/cm 2 |
| Shock strength | 5.35kJ/m 2 |
| Cohesive strength | 21MPa |
Embodiment 2
According to mass fraction, getting 80 parts of polymerization degree is the α of 15, poly-(dimethyl-methyl vinyl) siloxanes of ω-hydroxyl and 20 parts of methyl MQ silicone resin (cyclic polymer B) put into reactor, open stirring 35 minutes, rotating speed is 80 revs/min, be warming up to 85 DEG C, temperature rise rate is 2 DEG C/min; Until system mix with temperature-stable after, according to α, 0.02% of poly-(dimethyl-methyl vinyl) siloxanes mass parts of ω-hydroxyl adds trimethyl silicane potassium alcoholate as catalyzer, constant temperature stirs 1.5 hours, question response thing stops heating after becoming transparent colloid, continue to be stirred to cooling room temperature, namely obtain product 2.And properties detection is carried out to product, detected result is as shown in table 2:
The main performance index of table 2 product 2
| Performance title | Performance perameter |
| Body resistance | 4.31×10 13Ω |
| Thermal conductivity | 1.09W/mK |
| Irradiation can be tolerated | 7.32×10 9rad |
| Tensile strength | 171kg/cm 2 |
| Shock strength | 5.72kJ/m 2 |
| Cohesive strength | 36MPa |
Embodiment 3
According to mass fraction, getting 85 parts of polymerization degree is the α of 20, alpha, omega-dihydroxy polydimethyl siloxane and 15 parts of M/Q values be 0.7 methyl vinyl MQ silicon resin (cross-linked polymer C) put into reactor, open stirring 35 minutes, rotating speed is 60 revs/min, be warming up to 95 DEG C, temperature rise rate is 2 DEG C/min; Until system mix with temperature-stable after, according to α, 0.04% of alpha, omega-dihydroxy polydimethyl siloxane mass parts adds trimethyl silicane sodium alkoxide as catalyzer, constant temperature stirs 3 hours, question response thing stops heating after becoming transparent colloid, continues to be stirred to cooling room temperature, namely obtains product 3.And properties detection is carried out to product, detected result is as shown in table 3:
The main performance index of table 3 product 3
| Performance title | Performance perameter |
| Body resistance | 4.61×10 13Ω |
| Thermal conductivity | 1.19W/mK |
| Irradiation can be tolerated | 4.73×10 9rad |
| Tensile strength | 173kg/cm 2 |
| Shock strength | 5.82kJ/m 2 |
| Cohesive strength | 29MPa |
Embodiment 4
According to mass fraction, getting 90 parts of polymerization degree is the α of 20, alpha, omega-dihydroxy polydimethyl siloxane and 10 parts of M/Q values be 0.7 methyl vinyl MQ silicon resin (cyclic polymer B) put into reactor, open stirring 40 minutes, rotating speed is 75 revs/min, be warming up to 95 DEG C, temperature rise rate is 2 DEG C/min; Until system mix with temperature-stable after, according to α, 0.05% of poly-(dimethyl-methyl vinyl) siloxanes mass parts of ω-hydroxyl adds trimethyl silicane potassium alcoholate as catalyzer, constant temperature stirs 3 hours, question response thing stops heating after becoming transparent colloid, continue to be stirred to cooling room temperature, namely obtain product 4.And properties detection is carried out to product, detected result is as shown in table 4:
The main performance index of table 4 product 4
| Performance title | Performance perameter |
| Body resistance | 7.13×10 13Ω |
| Thermal conductivity | 0.98W/mK |
| Irradiation can be tolerated | 7.12×10 9rad |
| Tensile strength | 181kg/cm 2 |
| Shock strength | 7.35kJ/m 2 |
| Cohesive strength | 36MPa |
The present invention filters out best material component by great many of experiments, catalyzer, with the amount ratio of each component, and optimize best reaction conditions, the polymer organic silicone resin of the lsi package prepared, there is good tensile strength, shock strength and adhesive property, polymer organic silicone resin can be strengthened as vibrations buffering during packaged material, impact damping and cohesive strength, and there is the advantages such as resistance is high, thermal conductivity is low, radiation-resistant property is strong, achieve extraordinary technique effect.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1., for a preparation method for lsi package MQ side chain modified silicone resin polymkeric substance, it is characterized in that, comprise the following steps:
The first step, gets 65 ~ 95 parts of α, and alpha, omega-dihydroxy polydimethyl siloxane or poly-(dimethyl-methyl vinyl) siloxanes of α, ω-hydroxyl join in reactor;
Second step, according to mass parts, gets 5 ~ 35 parts of methyl vinyl MQ silicon resin or reactor put into by methyl MQ silicone resin, and open stirring 45 ~ 60 minutes, rotating speed is 70 ~ 100 revs/min, is warming up to 50-130 ° of C, and temperature rise rate is 2 ~ 3 ° of C/ minute;
3rd step, after all even temperature-stable of above-mentioned material mixing, according to α, alpha, omega-dihydroxy polydimethyl siloxane or α, the 0.01-0.1% of poly-(dimethyl-methyl vinyl) the siloxanes mass parts of ω-hydroxyl adds catalyzer, and constant temperature stirs 1-4 hour, and question response thing stops heating after becoming transparent colloid, continue to be stirred to cooling room temperature, namely obtain the encapsulation polymkeric substance of target product.
2. the preparation method for lsi package MQ side chain modified silicone resin polymkeric substance according to claim 1, it is characterized in that, described α, it is 5-30 that alpha, omega-dihydroxy polydimethyl siloxane or α, ω-hydroxyl gather polymerization degree scope in (dimethyl-methyl vinyl) siloxanes.
3. the preparation method for lsi package MQ side chain modified silicone resin polymkeric substance according to claim 1, it is characterized in that, it is described that to state M/Q ratio range in methyl vinyl MQ silicon resin or methyl MQ silicone resin be 0.6-0.9, wherein M is single functionality siloxane chain joint number, Q is four functionality siloxane polycondensation chain numbers, is 2.0-4.0% at methyl vinyl MQ silicon resin medium vinyl percentage composition.
4. the preparation method for lsi package MQ side chain modified silicone resin polymkeric substance according to claim 1, is characterized in that, described catalyzer is trimethyl silicane sodium alkoxide or trimethyl silicane potassium alcoholate.
5. the preparation method for lsi package MQ side chain modified silicone resin polymkeric substance according to any one of Claims 1-4, is characterized in that, in second step, stir 45 minutes, rotating speed is 70 revs/min, is warming up to 50-130 ° of C, and temperature rise rate is 2 ° of C/ minute.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928510A (en) * | 2017-02-23 | 2017-07-07 | 苏州纳贝通环境科技有限公司 | A kind of oil-resisting and heat-resisting elastomeric material and preparation method thereof |
| CN108165014A (en) * | 2017-12-23 | 2018-06-15 | 苏州赛源微电子有限公司 | A kind of packaging method of IC chip |
| CN112289528A (en) * | 2020-09-23 | 2021-01-29 | 湖北平安电工实业有限公司 | Method for manufacturing calcined mica tape and calcined mica tape |
| CN115537120A (en) * | 2022-11-03 | 2022-12-30 | 山东省科学院新材料研究所 | Heat-resistant grafted silicone resin coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788657A (en) * | 2014-01-24 | 2014-05-14 | 东南大学 | Preparation method of polymer for packaging large-scale integrated circuit |
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- 2015-03-30 CN CN201510143900.6A patent/CN104804192A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103788657A (en) * | 2014-01-24 | 2014-05-14 | 东南大学 | Preparation method of polymer for packaging large-scale integrated circuit |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106928510A (en) * | 2017-02-23 | 2017-07-07 | 苏州纳贝通环境科技有限公司 | A kind of oil-resisting and heat-resisting elastomeric material and preparation method thereof |
| CN108165014A (en) * | 2017-12-23 | 2018-06-15 | 苏州赛源微电子有限公司 | A kind of packaging method of IC chip |
| CN112289528A (en) * | 2020-09-23 | 2021-01-29 | 湖北平安电工实业有限公司 | Method for manufacturing calcined mica tape and calcined mica tape |
| CN115537120A (en) * | 2022-11-03 | 2022-12-30 | 山东省科学院新材料研究所 | Heat-resistant grafted silicone resin coating and preparation method thereof |
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Application publication date: 20150729 |