CN103044924A - Addition type liquid pouring sealant for semiconductor assembling piece and preparation method thereof - Google Patents
Addition type liquid pouring sealant for semiconductor assembling piece and preparation method thereof Download PDFInfo
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- CN103044924A CN103044924A CN2012105502382A CN201210550238A CN103044924A CN 103044924 A CN103044924 A CN 103044924A CN 2012105502382 A CN2012105502382 A CN 2012105502382A CN 201210550238 A CN201210550238 A CN 201210550238A CN 103044924 A CN103044924 A CN 103044924A
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Abstract
The invention discloses addition type liquid pouring sealant for a semiconductor assembling piece. The addition type liquid pouring sealant for the semiconductor assembling piece consists of the following components in part by weight: 40 to 50 parts of vinyl polysiloxane, 30 to 40 parts of reinforcing agent, 30 to 40 parts of inorganic filler, 5 to 10 parts of flame-retardant aid, 2 to 3 parts of functional aid, 3.0 to 6.0 parts of methyl hydrogen polysiloxane and 0.5 to 1.2 parts of catalyst. The invention also discloses a preparation method for the addition type liquid pouring sealant. The addition type liquid pouring sealant has excellent bubble discharge construction property, high-efficiency flame resistance, low thermal expansion coefficient, high low-temperature stress slackness and excellent thermal shock resistance, wherein the flame-retardant level reaches the UL-94 V-0 requirement. The preparation method is simple and practicable. After being solidified, the addition type liquid pouring sealant has certain thermal conductivity, can completely meet the protective requirement on electrical/electronic devices and components of various semiconductor assembling pieces and does not damage key parts such as welding and lead.
Description
Technical field
The present invention relates to the high molecule sealing materials technical field, relate in particular to a kind of semiconductor assemblies add-on type liquid joint sealant and preparation method thereof.
Background technology
Along with the technical progress of semiconductor assemblies, used potting compound is had higher requirement.After the liquid silastic that uses at present solidifies, thermal expansivity and Young's modulus will increase several times usually under transformation temperature, and stress relaxation is relatively poor when low-temperature working, and the expansion of potting compound and contraction all can cause semiconductor assemblies to bear larger stress concentration phenomenon, thereby cause easily being partially damaged of the outbalance such as weld or lead-in wire in the assembly, so that the reliability decrease of subassembly, even lost efficacy.
At present, prior art can add the mineral fillers such as silica powder or aluminum oxide in joint sealant, but meeting is so that the viscosity of potting compound increases the usability variation in order to reduce the thermal expansivity of liquid silastic potting compound; Thereby also add the Young's modulus of non-functional group reactions silicone oil control potting compound in the oriented potting compound, but the contraction of joint sealant can cause separating out of silicone oil after solidifying, thus to around components and parts pollute.Therefore, but the preparation that how to utilize simple mode to realize taking into account the liquid joint sealant of excellent flame retardancy, low thermal coefficient of expansion, low temperature stress relaxation and excellent thermal shock resistance is that the organosilicon industry is difficult to break through problem in the urgent need to address always.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, providing a kind of had both had good row and had steeped application property, can guarantee again to have highly effective flame-retardant after the liquid silastic potting compound solidifies, low thermal coefficient of expansion, low temperature stress relaxation and excellent thermal shock resistance.Another object of the present invention is to provide the preparation method of above-mentioned semiconductor assemblies with the add-on type liquid silicon rubber potting compound.
Purpose of the present invention is achieved by the following technical programs:
A kind of semiconductor assemblies add-on type liquid silicon rubber potting compound provided by the invention is comprised of following component and weight part proportioning:
Vinyl polysiloxane 40～50,
Strengthening agent 30～40,
Mineral filler 30～40,
Flame retardant 5～10,
Functional agent 2～3,
Methylhydrogenpolysi,oxane 3.0～6.0,
Catalyzer 0.5～1.0.
The viscosity of vinyl polysiloxane of the present invention is 1000～50000cps.
Described strengthening agent is the hydroxylation vinyl MQ resin, M/Q=0.9～1.1 in the therein ethylene base MQ resin, the massfraction of Si-OH≤0.8%.
The present invention uses the hydroxylation vinyl MQ resin as strengthening agent, reactive group in this strengthening agent is incorporated in the organosilicon matrix by modes such as crosslinked, grafting, condensations, better with the consistency of base-material, be beneficial to and disperse and have fabulous reinforcement and an increasing tougheness; Can be configured to-65 ℃～150 ℃ and keep elasticity ,-50 ℃～150 ℃ lower volume coefficient≤250ppmK-1, low thermal coefficient of expansion and the low elastic modulus potting compound of the storage elastic modulus of-65 ℃ storage elastic modulus/20 ℃≤4.
The present invention is by adding special functional agent, as contain a kind of or its combination of isopropoxy coupling agent, activated polyethylene radical siloxane, methylphenyl siloxane multipolymer, dispersion treatment is carried out in mineral filler to required interpolation, so that the dispersiveness of liquid silastic potting compound improves, potting compound still possesses mobile preferably after mixing; The bubble that produces in the time of can also mixing mineral filler suppresses and froth breaking, so that potting compound can possess good row's bubble property before sulfuration; And with after can also improve low temperature stress relaxation after the liquid silastic potting compound sulfuration, semiconductor subassembly after the embedding is placed 30min in-65 ℃, place 30min as 1 circulation for 150 ℃, after 3000 times, the on-state rate of all semiconductor subassemblies is all qualified.
The present invention can take following further measure: described mineral filler is a kind of or its combination in silica powder, aluminum oxide, magnesium oxide and the aluminium hydroxide.Described flame retardant is a kind of or its combination in Shawinigan black, triazole class compounds and the zinc carbonate.The massfraction of H is 0.5%-2.5% in the described methylhydrogenpolysi,oxane.Described catalyzer is a kind of or its combination in Platinic chloride-Virahol, Platinic chloride-vinylsiloxane and the pure modification Platinic chloride.
Another object of the present invention is achieved by the following technical programs:
A kind of semiconductor assemblies provided by the invention preparation method of add-on type liquid joint sealant may further comprise the steps:
A. vinyl polysiloxane and strengthening agent high-speed stirring blending dispersion under 120～160r/min is even;
B. mineral filler is carried out in advance behind the drying and dehydrating minutes for 3～5 times and is added, and then dispersed with stirring 30～45min adds flame retardant and again carry out high-speed stirring and be uniformly dispersed;
C. add functional agent middling speed dispersed with stirring 20～40min under 80～100r/min, make base-material;
D. above-mentioned base-material is divided into 2 parts, 1 part of adding methylhydrogenpolysi,oxane is dispersed in 10～20min under 80～100r/min, vacuumizes the A component that discharging namely gets the liquid joint sealant; Other 1 part adds catalyzer low speed dispersed with stirring 15～20min under 40～60r/min; Vacuumize the B component that discharging namely gets the liquid joint sealant.
E. equivalent takes by weighing A, B component, mixes and is made into joint sealant.
During use, 80 ℃ of joint sealants are solidified 20min namely can realize solidifying fully.
The present invention has following beneficial effect:
(1) the present invention is the add-on type liquid silicon rubber potting compound, is mobile liquid before solidifying, and forms flexible elastomer after solidifying, solvent-free or by product, curing speed is even, and is irrelevant with the airtight degree of the thickness of embedding and environment, need not regelate, be easy to reprocessing and repairing.
(2) have good storage stability, temperature tolerance and excellent electrical property after the present invention is solidified.Flame retardant properties can reach the UL-94V-0 rank after solidifying, and indices is zero in the ROHS instruction of SGS, meets the export standard of European Union.
(3) the present invention uses the hydroxylation vinyl MQ resin to be strengthening agent, so that the potting compound after solidifying possesses low thermal coefficient of expansion and excellent thermal shock resistance, can the significant points of semiconductor assemblies not caused damage.
(4) the composite functional agent of the present invention can not cause restriction to other interpolation components in the sizing material, neither intoxicating phenomenon can occur, can not cause processing and constructional difficulties yet, has general practicality.
(5) compared with prior art; the present invention by selecting ad hoc structure strengthening agent and the means of composite functional agent; realized under the condition that guarantees liquid joint sealant good fluidity and row's bubble property; the key propertys such as the volume expansivity of joint sealant, Young's modulus, cryogenic relaxation are improved; the protection of the electric/electronic devices of classes of semiconductors subassembly and first device be can satisfy after the curing fully, wherein welding and the key part such as lead-in wire can not damaged.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but the invention is not restricted to following embodiment, and equivalent variations or nonessential adjustment for those skilled in the art does according to the present invention also are considered as dropping within protection scope of the present invention.
Embodiment one
Present embodiment add-on type liquid joint sealant is comprised of following component and weight part proportioning:
The preparation method of present embodiment add-on type liquid joint sealant is as follows:
A. vinyl polysiloxane and strengthening agent high-speed stirring blending dispersion under 120r/min is even;
B. mineral filler is carried out in advance behind the drying and dehydrating minutes for 3 times and is added, dispersed with stirring 30min, then add flame retardant again 120r/min carry out high-speed stirring and be uniformly dispersed;
C. add functional agent middling speed dispersed with stirring 20min under 80r/min, make base-material;
D. above-mentioned base-material is divided into 2 parts, 1 part of adding methylhydrogenpolysi,oxane is dispersed in 10min under the 80r/min, vacuumizes the A component that discharging namely gets the liquid joint sealant; Other 1 part adds catalyzer low speed dispersed with stirring 15min under 40r/min; Vacuumize the B component that discharging namely gets the liquid joint sealant.
E. equivalent takes by weighing A, B component, mixes and is made into potting compound.
During use, 80 ℃ solidify the 20min realization and solidify fully.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 1.
The performance index of table 1 embodiment one add-on type liquid joint sealant
| Test item | The result |
| Shore hardness | 70 |
| Tensile strength | 7.5MPa |
| Elongation at break | 69% |
| Volume expansivity (40 ℃～-50 ℃) (K -1) | 245ppm |
| Storage elastic modulus (65 ℃) | 48.5MPa |
| The UL-94 vertical combustion | V-0 |
Embodiment two:
Present embodiment add-on type liquid joint sealant is comprised of following component and weight part proportioning:
The preparation method of present embodiment add-on type liquid joint sealant is as follows:
A. vinyl polysiloxane and strengthening agent high-speed stirring blending dispersion under 160r/min is even;
B. mineral filler is carried out in advance behind the drying and dehydrating minutes for 5 times and is added, and then dispersed with stirring 45min adds flame retardant and again carry out high-speed stirring and be uniformly dispersed;
C. add functional agent middling speed dispersed with stirring 40min under 100r/min, make base-material;
D. above-mentioned base-material is divided into 2 parts, 1 part of adding methylhydrogenpolysi,oxane is dispersed in 20min under the 100r/min, vacuumizes the A component that discharging namely gets the liquid joint sealant; Other 1 part adds catalyzer low speed dispersed with stirring 20min under 60r/min; Vacuumize the B component that discharging namely gets the liquid joint sealant.
E. equivalent takes by weighing A, B component, mixes and is made into potting compound.
During use, 80 ℃ solidify the 20min realization and solidify fully.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 2.
The performance index of table 2 embodiment two add-on type liquid joint sealants
| Test item | The result |
| Shore hardness | 78 |
| Tensile strength | 8.5MPa |
| Elongation at break | 45% |
| Volume expansivity (40 ℃～-50 ℃) (K -1) | 250ppm |
| Storage elastic modulus (65 ℃) | 38.5MPa |
| The UL-94 vertical combustion | V-0 |
Embodiment three:
Present embodiment add-on type liquid joint sealant, it forms and embodiment one difference is:
The preparation method of present embodiment add-on type liquid joint sealant is as follows:
A. vinyl polysiloxane and strengthening agent high-speed stirring blending dispersion under 160r/min is even;
B. mineral filler is carried out in advance behind the drying and dehydrating minutes for 5 times and is added, dispersed with stirring 30min, then add flame retardant again 160r/min carry out high-speed stirring and be uniformly dispersed;
C. add functional agent middling speed dispersed with stirring 40min under 80r/min, make base-material;
D. above-mentioned base-material is divided into 2 parts, 1 part of adding methylhydrogenpolysi,oxane is dispersed in 10min under the 100r/min, vacuumizes the A component that discharging namely gets the liquid joint sealant; Other 1 part adds catalyzer low speed dispersed with stirring 20min under 40r/min; Vacuumize the B component that discharging namely gets the liquid joint sealant.
E. equivalent takes by weighing A, B component, mixes and is made into potting compound.
During use, 80 ℃ solidify the 20min realization and solidify fully.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 3.
The performance index of table 3 embodiment three add-on type liquid joint sealants
Embodiment four:
Present embodiment add-on type liquid joint sealant, it forms and embodiment one difference is:
The preparation method of present embodiment add-on type liquid joint sealant is identical with embodiment one.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 4.
The performance index of table 4 embodiment four add-on type liquid joint sealants
| Test item | The result |
| Shore hardness | 70 |
| Tensile strength | 6.9MPa |
| Elongation at break | 70% |
| Volume expansivity (40 ℃～-50 ℃) (K -1) | 260ppm |
| Storage elastic modulus (65 ℃) | 50.5MPa |
| The UL-94 vertical combustion | V-0 |
Embodiment five:
Present embodiment add-on type liquid joint sealant, it forms and embodiment one difference is:
Strengthening agent 30
Aluminium hydroxide 10
The preparation method of present embodiment add-on type liquid joint sealant is identical with embodiment one.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 5.
The performance index of table 5 embodiment slender acanthopanax moulding liquid joint sealant
Embodiment six:
Present embodiment add-on type liquid joint sealant, it forms and embodiment two differences are:
Strengthening agent 30
Aluminum oxide 10
Activated polyethylene radical siloxane 1
The preparation method of present embodiment add-on type liquid joint sealant is identical with embodiment three.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 6.
The performance index of table 6 embodiment six add-on type liquid joint sealants
Embodiment seven:
Present embodiment add-on type liquid joint sealant, it forms and embodiment two differences are:
Vinyl polysiloxane (20000cps) 40
Strengthening agent 35
Magnesium oxide 10
The preparation method of present embodiment add-on type liquid joint sealant is identical with embodiment two.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 7.
The performance index of table 7 embodiment seven add-on type liquid joint sealants
| Test item | The result |
| Shore hardness | 68 |
| Tensile strength | 7.0MPa |
| Elongation at break | 80% |
| Volume expansivity (40 ℃～-50 ℃) (K -1) | 265ppm |
| Storage elastic modulus (65 ℃) | 60.5MPa |
| The UL-94 vertical combustion | V-0 |
Embodiment eight:
Present embodiment add-on type liquid joint sealant, it forms and embodiment two differences are:
Strengthening agent 35
Aluminium hydroxide 10
The preparation method of present embodiment add-on type liquid joint sealant is identical with embodiment two.
Performance after present embodiment add-on type liquid joint sealant solidifies is as shown in table 8.
The performance index of table 8 embodiment eight add-on type liquid joint sealants
| Test item | The result |
| Shore hardness | 75 |
| Tensile strength | 7.0MPa |
| Elongation at break | 69% |
| Volume expansivity (40 ℃～-50 ℃) (K -1) | 243ppm |
| Storage elastic modulus (65 ℃) | 53.5MPa |
| The UL-94 vertical combustion | V-0 |
Add-on type liquid joint sealant of the present invention and preparation method thereof, the consumption of each component and processing parameter are not limited to the above-mentioned embodiment that enumerates.
Claims (9)
1. semiconductor assemblies add-on type liquid joint sealant is characterized in that being comprised of following component and weight part proportioning:
Vinyl polysiloxane 40～50,
Strengthening agent 30～40,
Mineral filler 30～40,
Flame retardant 5～10,
Functional agent 2～3,
Methylhydrogenpolysi,oxane 3.0～6.0,
Catalyzer 0.5～1.0.
2. a kind of semiconductor assemblies add-on type liquid joint sealant according to claim 1, it is characterized in that: the viscosity of described vinyl polysiloxane is 1000～50000cps.
3. a kind of semiconductor assemblies add-on type liquid joint sealant according to claim 1, it is characterized in that: described strengthening agent is the hydroxylation vinyl MQ resin, M/Q=0.9-1.1 in the therein ethylene base MQ resin, the massfraction of Si-OH≤0.8%.
4. a kind of semiconductor assemblies add-on type liquid joint sealant according to claim 1, it is characterized in that: described mineral filler is a kind of or its combination in silica powder, aluminum oxide, magnesium oxide and the aluminium hydroxide.
5. a kind of semiconductor assemblies add-on type liquid joint sealant according to claim 1, it is characterized in that: described flame retardant is a kind of or its combination in Shawinigan black, triazole class compounds and the zinc carbonate.
6. a kind of semiconductor assemblies add-on type liquid joint sealant according to claim 1, it is characterized in that: described functional agent is a kind of or its combination that contains isopropoxy coupling agent, activated polyethylene radical siloxane, methylphenyl siloxane multipolymer.
7. semiconductor assemblies according to claim 1 add-on type liquid joint sealant, it is characterized in that: the massfraction of H is 0.5%-2.5% in the described methylhydrogenpolysi,oxane.
8. semiconductor assemblies according to claim 1 add-on type liquid joint sealant, it is characterized in that: described catalyzer is a kind of or its combination in Platinic chloride-Virahol, Platinic chloride-vinylsiloxane and the pure modification Platinic chloride.
9. the described semiconductor assemblies of one of claim 1-8 may further comprise the steps with the preparation method of add-on type liquid joint sealant:
A. vinyl polysiloxane and strengthening agent high-speed stirring blending dispersion under 120～160r/min is even;
B. mineral filler is carried out in advance behind the drying and dehydrating minutes for 3～5 times and is added, and then dispersed with stirring 30～45min adds flame retardant and again carry out high-speed stirring and be uniformly dispersed;
C. add functional agent middling speed dispersed with stirring 20～40min under 80～100r/min, make base-material;
D. above-mentioned base-material is divided into 2 parts, 1 part of adding methylhydrogenpolysi,oxane is dispersed in 10～20min under 80～100r/min, vacuumizes the A component that discharging namely gets the liquid joint sealant; Other 1 part adds catalyzer low speed dispersed with stirring 15～20min under 40～60r/min; Vacuumize the B component that discharging namely gets the liquid joint sealant.
E. equivalent takes by weighing A, B component, mixes and is made into joint sealant.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450690A (en) * | 2013-08-01 | 2013-12-18 | 广东信翼新材料股份有限公司 | Heating-forming polysiloxane composition for LED (light emitting diode) components |
| CN104292843B (en) * | 2014-09-24 | 2016-08-17 | 惠州市安品新材料有限公司 | The preparation method of bi-component addition type organosilicon heat conduction casting glue |
| CN106057689A (en) * | 2016-06-01 | 2016-10-26 | 东莞兆舜有机硅科技股份有限公司 | Integral glue-pouring process for heat-conducting and flame-retardant material |
| CN109337640A (en) * | 2018-08-28 | 2019-02-15 | 佛山市南海区长彤新材料科技有限公司 | A kind of MQ resin modified organic silicon packaging glue and preparation method thereof |
| CN110256853A (en) * | 2019-05-10 | 2019-09-20 | 肇庆皓明有机硅材料有限公司 | A kind of in-place molding foamed silastic sealing ring composition and preparation method thereof |
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| CN101054507A (en) * | 2007-05-30 | 2007-10-17 | 南京工业大学 | High heat conduction organosilicon filling and sealing gum |
| CN102174309A (en) * | 2011-01-13 | 2011-09-07 | 深圳市森日有机硅材料有限公司 | Solvent-free organic silicon pressure-sensitive adhesive and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101054507A (en) * | 2007-05-30 | 2007-10-17 | 南京工业大学 | High heat conduction organosilicon filling and sealing gum |
| CN102174309A (en) * | 2011-01-13 | 2011-09-07 | 深圳市森日有机硅材料有限公司 | Solvent-free organic silicon pressure-sensitive adhesive and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450690A (en) * | 2013-08-01 | 2013-12-18 | 广东信翼新材料股份有限公司 | Heating-forming polysiloxane composition for LED (light emitting diode) components |
| CN103450690B (en) * | 2013-08-01 | 2016-03-02 | 矽时代材料科技股份有限公司 | LED element hot briquetting polysiloxane composition |
| CN104292843B (en) * | 2014-09-24 | 2016-08-17 | 惠州市安品新材料有限公司 | The preparation method of bi-component addition type organosilicon heat conduction casting glue |
| CN106057689A (en) * | 2016-06-01 | 2016-10-26 | 东莞兆舜有机硅科技股份有限公司 | Integral glue-pouring process for heat-conducting and flame-retardant material |
| CN106057689B (en) * | 2016-06-01 | 2019-06-07 | 东莞兆舜有机硅科技股份有限公司 | The whole process for filling colloid of heat conductive flame-retarding material |
| CN109337640A (en) * | 2018-08-28 | 2019-02-15 | 佛山市南海区长彤新材料科技有限公司 | A kind of MQ resin modified organic silicon packaging glue and preparation method thereof |
| CN110256853A (en) * | 2019-05-10 | 2019-09-20 | 肇庆皓明有机硅材料有限公司 | A kind of in-place molding foamed silastic sealing ring composition and preparation method thereof |
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Application publication date: 20130417 |