CN102850804A - Transparent two-component organic silicon pouring sealant for LED and preparation method thereof - Google Patents
Transparent two-component organic silicon pouring sealant for LED and preparation method thereof Download PDFInfo
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- CN102850804A CN102850804A CN2012103003623A CN201210300362A CN102850804A CN 102850804 A CN102850804 A CN 102850804A CN 2012103003623 A CN2012103003623 A CN 2012103003623A CN 201210300362 A CN201210300362 A CN 201210300362A CN 102850804 A CN102850804 A CN 102850804A
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Abstract
The invention discloses a transparent two-component organic silicon pouring sealant for LED and a preparation method thereof. The pouring sealant comprises a component A and a component B mixed according to a mass ratio of 1:1. The component A comprises vinyl silicone oil, hydrogen-containing silicone oil and methyl vinyl MQ silicone resin in a mass ratio of 100:5-20:20-50; and the B component comprises vinyl silicone oil and a platinum catalyst in a mass ratio of 100:0.01-1.
Description
Technical field
The present invention relates to the joint sealant Material Field, relate in particular to that a kind of transparency is strong, mechanical property reaches well the good LED of humidity resistance with transparent two-pack organic silicon potting adhesive and preparation method thereof.
Background technology
At present, LED adopts cheaply epoxide resin material with joint sealant more, but the high thermal resistance of Resins, epoxy, wet fastness are poor.The poor easy damage element of high thermal resistance shortens element work-ing life, and the poor aqueous vapor that then can cause of wet fastness easily enters element internal, easily causes the problems such as short circuit.Along with continuing to bring out of flourish, high-power, the high brightness of LED illuminating industry, illumination level LED device that the long lifetime requires, need a kind of high performance packaged material satisfy the requirement of LED encapsulation.
And existing joint sealant glue sample embrittlement, frangibility, tensile property and flexility all also do not reach the requirement of LED encapsulation, and use properties has much room for improvement.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of LED with transparent two-pack organic silicon potting adhesive and preparation method thereof, be intended to solve that existing LED packaged material high thermal resistance is poor, wet fastness is poor, glue sample embrittlement, flexility and the not good problem of tensile property.
Technical scheme of the present invention is as follows:
The two component transparent organic silicon joint sealants of a kind of LED, wherein, it comprises A component and the B component of mixing for 1:1 in mass ratio;
Described A component comprises:
Vinyl silicone oil;
Containing hydrogen silicone oil;
The methyl vinyl MQ silicone resin;
Described B component comprises:
Vinyl silicone oil;
Platinum catalyst;
Wherein, the mass ratio of the vinyl silicone oil in the described A component, containing hydrogen silicone oil and methyl vinyl MQ silicone resin is 100:5 ~ 20:20 ~ 50, and the vinyl silicone oil in the described B component and the mass ratio of platinum catalyst are 100:0.01 ~ 1.
The two component transparent organic silicon joint sealants of described LED, wherein, the structure of described vinyl silicone oil is for containing the linear methyl vinyl silicon oil of two vinyl-functional end groups on each polysiloxane molecule.
The two component transparent organic silicon joint sealants of described LED, wherein, the structure of described containing hydrogen silicone oil directly with Siliciumatom with chemical bond links to each other for containing two hydrogen atoms in each polysiloxane molecule at least.
The two component transparent organic silicon joint sealants of described LED, wherein, the hydrogen mass content of described containing hydrogen silicone oil is 0.3 ~ 1.0%.
The two component transparent organic silicon joint sealants of described LED, wherein, the M in the described methyl vinyl MQ silicone resin is single functionality siloxanes sealing chain link (CH3)
3SiO
1/2(CH
2=CH) (CH
3)
2SiO
1/2
The two component transparent organic silicon joint sealants of described LED, wherein, the Q in the described methyl vinyl MQ silicone resin is four functionality siloxanes polycondensation chain link SiO
4/2
The two component transparent organic silicon joint sealants of described LED, wherein, the molecular formula of described methyl vinyl MQ silicone resin is [(CH3)
3SiO
1/2]
a[(CH
2=CH) (CH
3)
2SiO
1/2]
b[SiO
4/2]
c, wherein, (a+b)/mol ratio of c is 0.6 ~ 1.2.
The two component transparent organic silicon joint sealants of described LED, wherein, the massfraction of the vinyl in the described methyl vinyl MQ silicone resin is 0.1 ~ 10%.
A kind of LED preparation method of two component transparent organic silicon joint sealants wherein, comprises step:
A, vinyl silicone oil, methyl vinyl MQ silicone resin and containing hydrogen silicone oil are carried out blend for 100:5 ~ 20:20 ~ 50 in mass ratio, processed under the heat temperature raising, vacuum condition 1.5 ~ 2.5 hours, get component A;
B, vinyl silicone oil and platinum catalyst are mixed for 100:0.01 ~ 1 in mass ratio, be warming up to 100 ℃, processed 1.5 ~ 2.5 hours to get B component under the vacuum condition;
C, with described component A and B component in mass ratio for 1:1 mixes, vacuum defoamation is solidified at ambient temperature and is obtained LED with two component transparent organic silicon joint sealants.
Described preparation method, wherein, described A component and B component all are to process to obtain in 2 hours under vacuum condition.
Beneficial effect: LED of the present invention is with transparent two-pack organic silicon potting adhesive and preparation method thereof, by the vinyl on the vinyl silicone oil under the effect of platinum catalyst with containing hydrogen silicone oil in si-h bond generation addition reaction, generation-CH
2-CH
2-Si-cross-link bond, because reaction discharges without small molecules, so nothing is shunk after solidifying, it is excellent Embedding Material, prepared joint sealant has good dielectric properties, wider use temperature scope and excellent damping property, joint sealant high thermal resistance of the present invention, wet fastness, tensile property and snappiness obviously improve, and do not affect its transparency.
Embodiment
The invention provides a kind of LED with transparent two-pack organic silicon potting adhesive and preparation method thereof, clearer, clear and definite for making purpose of the present invention, technical scheme and effect, below the present invention is described in more detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The two component transparent organic silicon joint sealants of LED provided by the invention, it comprises A component and the B component of mixing for 1:1 in mass ratio;
Described A component comprises:
Vinyl silicone oil;
Containing hydrogen silicone oil;
The methyl vinyl MQ silicone resin;
Described B component comprises:
Vinyl silicone oil;
Platinum catalyst;
Wherein, the mass ratio of the vinyl silicone oil in the described A component, containing hydrogen silicone oil and methyl vinyl MQ silicone resin is 100:5 ~ 20:20 ~ 50, and the vinyl silicone oil in the described B component and the mass ratio of platinum catalyst are 100:0.01 ~ 1.
Described vinyl silicone oil is with the low molecular weight polysiloxane of vinyl on the part Siliciumatom, vinyl silicone oil is the main raw material of organic silicon potting adhesive of the present invention, can adopt specifically that the vinyl silicone oil of several different viscosity is composite to reach required viscosity, the viscosity of vinyl silicone oil of the present invention is generally 300 ~ 5000 centipoises (least unit of kinetic viscosity, 1 centipoise equal 0.01 pool).The structure of the vinyl silicone oil that adopts among the present invention is for containing the linear methyl vinyl silicon oil of two vinyl-functional end groups on each polysiloxane molecule, wherein, the vinyl molar mass is 0.05 ~ 0.5%, adopts the prepared organic silicon potting adhesive of vinyl silicone oil of said structure to have good elongation, humidity resistance and insulativity.
Described containing hydrogen silicone oil is under the metal solvent effect, can be crosslinked at proper temperature, thereby improve snappiness and the tensile property of organic silicon potting adhesive, the containing hydrogen silicone oil that containing hydrogen silicone oil preferred structure of the present invention directly with Siliciumatom with chemical bond links to each other for containing two hydrogen atoms in each polysiloxane molecule at least, further, the hydrogen mass content of described containing hydrogen silicone oil is 0.3 ~ 1.0%, adopts the prepared organic silicon potting adhesive of containing hydrogen silicone oil of said structure all relative better with tensile property through the evidence snappiness.
Described methyl vinyl MQ silicone resin is the organic resin that is made of four functionality siloxanes polycondensation chain links (Q) and single functionality siloxane unit (M), and its Main Function is intended for strengthening agent.In the molecular structure of described methyl vinyl MQ silicone resin the when structures shape of the amount of M chain link and Q chain link the character of resin.M chain link among the present invention is preferably single functionality siloxanes sealing chain link (CH3)
3SiO
1/2(CH
2=CH) (CH
3)
2SiO
1/2, and the Q chain link is preferably four functionality siloxanes polycondensation chain link SiO
4/2Further, the structure of described methyl vinyl MQ silicone resin is [(CH3)
3SiO
1/2]
a[(CH
2=CH) (CH
3)
2SiO
1/2]
b[SiO
4/2]
c, wherein, (a+b)/mol ratio of c is 0.6 ~ 1.2.Adopt the methyl vinyl MQ silicone resin of said structure that tensile strength and the snappiness of the organic silicon potting adhesive glue sample that makes are at last strengthened greatly, and do not affect the transparency, thereby improved sample embrittlement, frangibility, the bad problem of use properties of removing photoresist of crossing.
Preferably, the massfraction of the vinyl in the described methyl vinyl MQ silicone resin is 0.1 ~ 1.0%, with tensile strength and the snappiness of further raising organic silicon potting adhesive.
Described platinum catalyst is mainly take the platinum catalyst of Platinic chloride precious metal as the main raw material activeconstituents, adopts wire netting, platinum black or platinum is stated from the carrier such as aluminum oxide.The catalytic efficiency of platinum catalyst is high, and anti-yellowing property is good, and high reactivity has higher stability in use.
The present invention also provides the preparation method of a kind of LED with two component transparent organic silicon joint sealants, and it comprises step:
A, vinyl silicone oil, methyl vinyl MQ silicone resin and containing hydrogen silicone oil are carried out blend for 100:5 ~ 20:20 ~ 50 in mass ratio, processed under the heat temperature raising, vacuum condition 1.5 ~ 2.5 hours, get component A;
B, vinyl silicone oil and platinum catalyst are mixed for 100:0.01 ~ 1 in mass ratio, be warming up to 100 ℃, processed 1.5 ~ 2.5 hours to get B component under the vacuum condition;
C, with described component A and B component in mass ratio for 1:1 mixes, vacuum defoamation is solidified at ambient temperature and is obtained LED with two component transparent organic silicon joint sealants.
Further, described heat temperature raising is for being heated to 100 ℃, and described vacuum condition is-0.06MPa, and even more preferably processes under vacuum condition respectively and obtained component A and B component in 2 hours, and this moment, sufficient reacting can make component A and the B component of better performances.
Before step c, with component A with B component prepares and packaging and storing respectively, be that 1:1 mixes according to mass ratio in use, vacuum defoamation encapsulated the LED device about 5 minutes, and then left standstill 2 ~ 4h under the room temperature condition and can solidify fully.
The present invention adopts LED that aforesaid method makes to have good thermotolerance, wet fastness, intensity is high, packaging effect is good characteristics with two component transparent organic silicon joint sealants, can effectively protect the LED device, and manufacture craft is simple.In addition, the LED of the present invention preparation is good with two component transparent organic silicon joint sealant transparencys, good, the anti-xanthochromia of snappiness, has esy to use, safe and reliable, environmentally safe, stable performance, characteristics such as can not ftracture at low temperatures.In the encapsulation of LED, not only play certain mechanical support, the effect of sealed environment, can also play good printing opacity, protection against the tide, dustproof, protection against corrosion and shockproof effect.
The present invention will be described below in conjunction with embodiment, vinyl silicone oil among the following embodiment is and adopts structure for containing the linear methyl vinyl silicon oil of two vinyl-functional end groups on each polysiloxane molecule, and vinyl molar mass mark is 0.05 ~ 0.5%; The methyl vinyl MQ silicone resin is [(CH3)
3SiO
1/2]
a[(CH
2=CH) (CH
3)
2SiO
1/2]
b[SiO
4/2]
c, wherein, (a+b)/mol ratio of c is 0.6 ~ 1.2, the massfraction of vinyl is 0.1 ~ 10%; The containing hydrogen silicone oil structure is to contain at least two hydrogen atoms in the polysiloxane per molecule directly to link to each other with chemical bond with Siliciumatom, and the hydrogen mass content is 0.3 ~ 1.0%.
Embodiment 1
Getting viscosity is the vinyl silicone oil 100g of 400 centipoises, and methyl vinyl MQ silicone resin 5g, viscosity are the containing hydrogen silicone oil 20g of 200 centipoises, mix in kneader, are warming up to 100 ℃, and vacuum-0.06MPa processed 1.5 hours, obtained the A component.Getting viscosity is the vinyl silicone oil 100g of 400 centipoises, and platinum catalyst 0.01g mixes in the planet stirring tank, is warming up to 100 ℃, and vacuum-0.06MPa processed 1.5 hours, forms the B component.Before use, A, B component are prepared and the difference packaging and storing, mix according to weight ratio 1:1 during use, vacuum defoamation 5 minutes encapsulates the LED light fixture, and then at room temperature leaving standstill 2-4h can solidify fully.
Embodiment 2
Getting viscosity is the vinyl silicone oil 100g of 1000 centipoises, and methyl vinyl MQ silicone resin 10g, viscosity are the containing hydrogen silicone oil 30g of 100 centipoises, mix in kneader, are warming up to 100 ℃, and vacuum-0.06MPa processed 2 hours, obtained the A component.Getting viscosity is the vinyl silicone oil 100g of 1000 centipoises, and platinum catalyst 0.1g mixes in the planet stirring tank, is warming up to 100 ℃, and vacuum-0.06MPa processed 2 hours, forms the B component.Before use, A, B component are prepared and the difference packaging and storing, mix according to weight ratio 1:1 during use, vacuum defoamation 5 minutes encapsulates the LED light fixture, and then at room temperature leaving standstill 2-4h can solidify fully.
Embodiment 3
Getting viscosity is the vinyl silicone oil 100g of 4000 centipoises, and methyl vinyl MQ silicone resin 20g, viscosity are the containing hydrogen silicone oil 40g of 50 centipoises, mix in kneader, are warming up to 100 ℃, and vacuum-0.06MPa processed 2.5 hours, obtained the A component.Getting viscosity is the vinyl silicone oil 100g of 4000 centipoises, and platinum catalyst 0.5g mixes in the planet stirring tank, is warming up to 100 ℃, and vacuum-0.06MPa processed 2.5 hours, forms the B component.Before use, A, B component are prepared and the difference packaging and storing, mix according to weight ratio 1:1 during use, vacuum defoamation 5 minutes encapsulates the LED light fixture, and then at room temperature leaving standstill 2-4h can solidify fully.
The contrast sample
Getting viscosity is the vinyl silicone oil 100g of 4000 centipoises, and viscosity is the containing hydrogen silicone oil 40g of 50 centipoises, mixes in kneader, is warming up to 100 ℃, and vacuum-0.06MPa processed 2 hours, obtained the A component.Getting viscosity is the vinyl silicone oil 100g of 4000 centipoises, and platinum catalyst 0.5g mixes in the planet stirring tank, is warming up to 100 ℃, and vacuum-0.06MPa processed 2 hours, forms the B component.Before use, A, B component are prepared and the difference packaging and storing, mix according to weight ratio 1:1 during use, vacuum defoamation 5 minutes encapsulates the LED light fixture, and then at room temperature leaving standstill 2-4h can solidify fully.
Table one performance test table
| Test event | Unit | Testing method | Instrument | Example 1 product | Example 2 products | Example 3 products | The contrast sample |
| Outward appearance | — | Range estimation | Range estimation | Water white transparency | Water white transparency | Water white transparency | Water white transparency |
| Hardness | Shore A | GB/T 531-1999 | Sclerometer | 30 | 22 | 18 | 13 |
| Proportion | g/cm 3 | GB/T 533-2008 | Densometer | 0.95 | 0.98 | 1.00 | 0.92 |
| Surface drying time | min | ASTM 0242 | － | 23 | 17 | 10 | 10 |
| Tensile strength | MPa | GB/T 528-2009 | Puller system | 1.31 | 1.16 | 0.95 | 0.43 |
| Elongation at break | % | GB/T 528-2009 | Puller system | 117 | 152 | 183 | 78 |
| Humidity resistance | — | GB2423.34-1986 | Climatic chamber | Well | Well | Well | Generally |
| Specific inductivity | (1MHz) | GB/T1693-2007 | HF Q meter | 2.8 | 2.7 | 2.7 | 2.7 |
| The dielectric loss tangent value | (1MHz) | GB/T1693-2007 | HF Q meter | 0.001 | 0.001 | 0.001 | 0.001 |
From table one as can be known: the LED product that adopts the present invention to make, not only transmittance, good fluidity, and have the advantages such as good elongation, humidity resistance, insulativity, and having in addition good dielectric properties, various aspects of performance obviously is better than the epoxy resin material.And after adding the methyl vinyl MQ silicone resin, its mechanical property such as tensile strength and elongation at break obviously improve, and do not affect its transparency.
In sum, the present invention is the alkene addition reaction of hydrogen by the curing mechanism of two-component addition type room temperature vulcanized silicone rubber, vinyl on the vinyl silicone oil under the effect of platinum catalyst with containing hydrogen silicone oil in si-h bond generation addition reaction, generation-CH2-CH2-Si-cross-link bond, because reaction discharges without small molecules, so without shrinking, be excellent Embedding Material after solidifying.It has good dielectric properties, and wider use temperature scope and excellent damping property use more and more general in LED embedding industry.The transparent addition glue glue sample embrittlement that does not add reinforced filling, frangibility, use properties is bad.
Should be understood that, application of the present invention is not limited to above-mentioned giving an example, and for those of ordinary skills, can be improved according to the above description or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (10)
1. a LED is characterized in that with two component transparent organic silicon joint sealants, and it comprises A component and the B component of mixing for 1:1 in mass ratio;
Described A component comprises:
Vinyl silicone oil;
Containing hydrogen silicone oil;
The methyl vinyl MQ silicone resin;
Described B component comprises:
Vinyl silicone oil;
Platinum catalyst;
Wherein, the mass ratio of the vinyl silicone oil in the described A component, containing hydrogen silicone oil and methyl vinyl MQ silicone resin is 100:5 ~ 20:20 ~ 50, and the vinyl silicone oil in the described B component and the mass ratio of platinum catalyst are 100:0.01 ~ 1.
2. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 1, and the structure of described vinyl silicone oil is for containing the linear methyl vinyl silicon oil of two vinyl-functional end groups on each polysiloxane molecule.
3. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 1, and the structure of described containing hydrogen silicone oil directly with Siliciumatom with chemical bond links to each other for containing two hydrogen atoms in each polysiloxane molecule at least.
4. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 3, and the hydrogen mass content of described containing hydrogen silicone oil is 0.3 ~ 1.0%.
5. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 1, and the M in the described methyl vinyl MQ silicone resin is single functionality siloxanes sealing chain link (CH3)
3SiO
1/2(CH
2=CH) (CH
3)
2SiO
1/2
6. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 1, and the Q in the described methyl vinyl MQ silicone resin is four functionality siloxanes polycondensation chain link SiO
4/2
7. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 1, and the molecular formula of described methyl vinyl MQ silicone resin is [(CH
3)
3SiO
1/2]
a[(CH
2=CH) (CH
3)
2SiO
1/2]
b[SiO
4/2]
c, wherein, (a+b)/mol ratio of c is 0.6 ~ 1.2.
8. described LED is characterized in that with two component transparent organic silicon joint sealants according to claim 7, and the massfraction of the vinyl in the described methyl vinyl MQ silicone resin is 0.1 ~ 10%.
9. the preparation method of the two component transparent organic silicon joint sealants of LED usefulness is characterized in that, comprises step:
A, vinyl silicone oil, methyl vinyl MQ silicone resin and containing hydrogen silicone oil are carried out blend for 100:5 ~ 20:20 ~ 50 in mass ratio, processed under the heat temperature raising, vacuum condition 1.5 ~ 2.5 hours, get component A;
B, vinyl silicone oil and platinum catalyst are mixed for 100:0.01 ~ 1 in mass ratio, be warming up to 100 ℃, processed 1.5 ~ 2.5 hours to get B component under the vacuum condition;
C, with described component A and B component in mass ratio for 1:1 mixes, vacuum defoamation is solidified at ambient temperature and is obtained LED with two component transparent organic silicon joint sealants.
10. preparation method according to claim 9 is characterized in that, described A component and B component all are to process to obtain in 2 hours under vacuum condition.
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| CN108424652A (en) * | 2018-04-16 | 2018-08-21 | 吉林大学 | A kind of add-on type silica gel and the preparation method and application thereof |
| CN109320969A (en) * | 2018-09-28 | 2019-02-12 | 唐山市第中学 | Anti-blue light film is at film liquid and preparation method thereof and anti-blue light film |
| CN111207173A (en) * | 2020-01-09 | 2020-05-29 | 苏州赛伍应用技术股份有限公司 | Buffering silica gel sheet used between electric cores of power battery pack, preparation method of buffering silica gel sheet and power battery pack comprising buffering silica gel sheet |
| CN111207173B (en) * | 2020-01-09 | 2021-11-16 | 苏州赛伍应用技术股份有限公司 | Buffering silica gel sheet used between electric cores of power battery pack, preparation method of buffering silica gel sheet and power battery pack comprising buffering silica gel sheet |
| CN114958288A (en) * | 2021-02-27 | 2022-08-30 | 华为技术有限公司 | Organosilicon conducting resin, crystal oscillator and electronic equipment |
| CN114958288B (en) * | 2021-02-27 | 2023-12-08 | 华为技术有限公司 | Organic silicon conductive adhesive, crystal oscillator and electronic equipment |
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