CN109852337A - A kind of LED transparent organic silicon casting glue of high refractive index high viscosity and preparation method thereof - Google Patents
A kind of LED transparent organic silicon casting glue of high refractive index high viscosity and preparation method thereof Download PDFInfo
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- CN109852337A CN109852337A CN201910134497.9A CN201910134497A CN109852337A CN 109852337 A CN109852337 A CN 109852337A CN 201910134497 A CN201910134497 A CN 201910134497A CN 109852337 A CN109852337 A CN 109852337A
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Abstract
The invention discloses a kind of LED transparent organic silicon casting glues of high refractive index high viscosity, it is made of component one and component two: the parts by weight proportion of one raw material of component are as follows: 60~70 parts of vinyl silicone oil, 15~25 parts of bleached shellac resin, 5~8 parts of containing hydrogen silicone oil, 8~15 parts of melamino-formaldehyde resin, 5~10 parts of beeswax liquid, 0.5~1 part of tertiary sodium phosphate, 15~40 parts of modified gas phase titanic oxide, the parts by weight of the component two match are as follows: 10~15 parts and 0.4~0.8 part of platinum catalyst of vinyl silicone oil, the present invention discloses a kind of preparation methods of the LED transparent organic silicon casting glue of high refractive index high viscosity.A kind of LED transparent organic silicon casting glue of high refractive index high viscosity of the invention has high refractive index and preferable mechanical property and adhesive property on the basis of translucidus is good.
Description
Technical field
The present invention relates to adhesive and preparation technical fields, and in particular to a kind of LED of high refractive index high viscosity is transparent to be had
Machine silicon casting glue and preparation method thereof.
Background technique
Casting glue, for the bonding of electronic component, encapsulating, sealing and coating protection.Casting glue belongs to before uncured
With the liquid of mobility, glue viscosity is according to the material of product, performance, the difference of production technology and different from.Encapsulating
Its use value can be achieved in glue after being fully cured, can be played after solidification it is waterproof and dampproof, insulation, it is dust-proof, thermally conductive, secrecy, it is resistance to
Temperature, anticorrosion, it is shockproof the effects of, be widely used for electronic device manufacturing industry at present, be that electronics industry is indispensable important
Rapidoprint.
The referred to as LED of forth generation light source have energy-saving and environmental protection, safety, low-power consumption, low-heat, light beam concentration, high brightness,
The features such as easy maintenance, can be widely applied to the fields such as various instructions, decoration, display, backlight, general lighting.It mentions at present
The luminous efficiency of high LED is still a key technical problem, and the materials such as casting glue shine to product in LED production process
Efficiency and service life have significant impact, it is desirable that the materials such as casting glue have high transparency, Gao Zheguang, high bond strength, resistance to
The performances such as light, heat ageing.Currently used casting glue mainly has epoxy resin embedding adhesive, organic siliconresin casting glue, polyurethane
Casting glue, organic siliconresin have higher light transmittance and resistance to ultraviolet, heat-resistant stability compared with other kinds of casting glue, are mesh
Preceding ideal casting glue basis material, however the refractive index of organosilicon material, mechanical property and adhesive property be not good enough, and
And moisture-inhibiting oxygen permeability is big, this is biggish lack for playing bonding, encapsulating, sealing and the casting glue of coating protective effect
It falls into, and only after the caking property by adding the improvement organosilicon material such as coupling agent, moisture-inhibiting oxygen permeability is hardly resulted in further
Improvement, these defects greatly limit it in the application in Electronic Packaging field.
Summary of the invention
In view of the shortcomings of the prior art, the present invention provides the LED of a kind of high refractive index, high viscosity, strong mechanical performance is transparent
Organic silicon potting adhesive and preparation method thereof.
The present invention solves the technical solution that above-mentioned technical problem uses are as follows: a kind of LED of high refractive index high viscosity is transparent to be had
Machine silicon casting glue, is made of component one and component two:
The constitutive material of the component one are as follows: vinyl silicone oil, bleached shellac resin, containing hydrogen silicone oil, melamine formaldehyde (MF) tree
Rouge, beeswax liquid, tertiary sodium phosphate, modified gas phase titanic oxide, the constitutive material of the component two are as follows: vinyl silicone oil and platinum are urged
Agent；
The parts by weight of the component one match are as follows: 60~70 parts of vinyl silicone oil, 15~25 parts of bleached shellac resin,
5~8 parts of containing hydrogen silicone oil, 8~15 parts of melamino-formaldehyde resin, 5~10 parts of beeswax liquid, 0.5~1 part of tertiary sodium phosphate, modified gas phase two
15~40 parts of titanium oxide, the parts by weight of the component two proportion are as follows: 10~15 parts of vinyl silicone oil and platinum catalyst 0.4~
0.8 part.
Further, the modified gas phase titanic oxide the preparation method comprises the following steps: the gas phase titanium dioxide that will be dried
Titanium and gas phase aluminum oxide are placed in the NaOH solution that concentration is 10mol/L, are heated with stirring to 60 DEG C, are added under insulated and stirred
The epoxychloropropane solution for being 5:1 with gas phase titanium dioxide mass ratio, heat preservation return stirring react 4h, then use methanol, pure water
Cleaning product obtains modified gas phase titanic oxide, modified gas phase titanium dioxide after being 7,100 DEG C of vacuum dryings to pH repeatedly
With nonpolar substrates dissolve each other or favorable dispersibility, be not in clustering phenomena and influence be blended after composite material performance.
A kind of preparation method of the LED transparent organic silicon casting glue of the high refractive index high viscosity, comprising the following steps:
(1) bleached shellac resin and tertiary sodium phosphate are mixed and heated to 80~90 DEG C, insulated and stirred is uniform；
(2) it is added after beeswax liquid being heated to 80~90 DEG C to step (1) and obtains in lac resin liquid, and insulated and stirred
Then 0.5~1h is cooled to 50~60 DEG C to uniform；
(3) vinyl silicone oil, containing hydrogen silicone oil, melamino-formaldehyde resin, modified gas phase titanic oxide are obtained with step (2)
Solution is kept the temperature at 50~60 DEG C to be sufficiently mixed uniformly, and high-pressure homogeneous primary at 40~60MPa, obtains component one；
(4) component two is obtained after being sufficiently mixed vinyl silicone oil and platinum catalyst uniformly；
(5) above-mentioned parts by weight are matched into component one made from raw material and component two is applied after mixing.
A kind of LED transparent organic silicon casting glue of high refractive index high viscosity of the invention has on the basis of translucidus is good
There are high refractive index and preferable mechanical property and adhesive property.Specifically, the modified gas phase titanic oxide powder of addition high refractive index
Body is greatly improved the refractive index of organosilicon material, and nanoscale gas phase titanium dioxide does not influence organic silicon potting adhesive body
Light transmission；Lac resin and tertiary sodium phosphate are mixed to the polymerization that can prevent lac resin active group itself to a certain extent
Effect increases its thermal life and reduces brittleness；By lac resin and beeswax liquid, tertiary sodium phosphate, melamino-formaldehyde resin and organic
After silicon materials etc. are mixed and modified, the flowability of lac resin and beeswax is increased, while increasing the mechanics of organosilicon material
Performance and adhesive property, while obtained casting glue moisture-inhibiting oxygen permeability is smaller, is a kind of good Electronic Packaging of comprehensive performance
Material.
Specific embodiment
Below by way of specific embodiment, the present invention will be further described, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
Embodiment 1: a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, by component one and two groups of component
At:
The parts by weight of one raw material of component match are as follows: 65 parts of vinyl silicone oil, 20 parts of bleached shellac resin, hydrogeneous
6 parts of silicone oil, 12 parts of melamino-formaldehyde resin, 8 parts of beeswax liquid, 0.8 part of tertiary sodium phosphate, 30 parts of modified gas phase titanic oxide, it is described
The parts by weight of two raw material of component match are as follows: 12 parts and 0.6 part of platinum catalyst of vinyl silicone oil.
Further, the modified gas phase titanic oxide the preparation method comprises the following steps: the gas phase titanium dioxide that will be dried
Titanium and gas phase aluminum oxide are placed in the NaOH solution that concentration is 10mol/L, are heated with stirring to 60 DEG C, are added under insulated and stirred
The epoxychloropropane solution for being 5:1 with gas phase titanium dioxide mass ratio, heat preservation return stirring react 4h, then use methanol, pure water
Cleaning product obtains modified gas phase titanic oxide after being 7,100 DEG C of vacuum dryings to pH repeatedly.
A kind of preparation method of the LED transparent organic silicon casting glue of the high refractive index high viscosity, comprising the following steps:
(1) bleached shellac resin and tertiary sodium phosphate are mixed and heated to 85 DEG C, insulated and stirred is uniform；
(2) it is added after beeswax liquid being heated to 85 DEG C to step (1) and obtains in lac resin liquid, and insulated and stirred 45min
To uniform, it is then cooled to 55 DEG C；
(3) vinyl silicone oil, containing hydrogen silicone oil, melamino-formaldehyde resin, modified gas phase titanic oxide are obtained with step (2)
Solution is kept the temperature at 55 DEG C to be sufficiently mixed uniformly, and high-pressure homogeneous primary at 50MPa, obtains component one；
(4) component two is obtained after being sufficiently mixed vinyl silicone oil and platinum catalyst uniformly；
(5) component one and component two are applied after mixing.
Embodiment 2: a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, by component one and two groups of component
At:
The parts by weight of one raw material of component match are as follows: 60 parts of vinyl silicone oil, 15 parts of bleached shellac resin, hydrogeneous
5 parts of silicone oil, 8 parts of melamino-formaldehyde resin, 5 parts of beeswax liquid, 0.5 part of tertiary sodium phosphate, 15 parts of modified gas phase titanic oxide, the group
Divide the parts by weight proportion of two raw materials are as follows: 10 parts and 0.4 part of platinum catalyst of vinyl silicone oil.
Further, the preparation method is the same as that of Example 1 for the modified gas phase titanic oxide.
A kind of preparation method of the LED transparent organic silicon casting glue of the high refractive index high viscosity, comprising the following steps:
(1) bleached shellac resin and tertiary sodium phosphate are mixed and heated to 80 DEG C, insulated and stirred is uniform；
(2) it is added after beeswax liquid being heated to 80 DEG C to step (1) and obtains in lac resin liquid, and insulated and stirred 1h is to equal
It is even, then it is cooled to 50 DEG C；
(3) vinyl silicone oil, containing hydrogen silicone oil, melamino-formaldehyde resin, modified gas phase titanic oxide are obtained with step (2)
Solution is kept the temperature at 50 DEG C to be sufficiently mixed uniformly, and high-pressure homogeneous primary at 40MPa, obtains component one；
(4) component two is obtained after being sufficiently mixed vinyl silicone oil and platinum catalyst uniformly；
(5) component one and component two are applied after mixing.
Embodiment 3: a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, by component one and two groups of component
At:
The parts by weight of one raw material of component match are as follows: 70 parts of vinyl silicone oil, 25 parts of bleached shellac resin, hydrogeneous
8 parts of silicone oil, 15 parts of melamino-formaldehyde resin, 10 parts of beeswax liquid, 1 part of tertiary sodium phosphate, 40 parts of modified gas phase titanic oxide, the group
Divide two parts by weight proportion are as follows: 15 parts and 0.8 part of platinum catalyst of vinyl silicone oil.
Further, the preparation method is the same as that of Example 1 for the modified gas phase titanic oxide.
A kind of preparation method of the LED transparent organic silicon casting glue of the high refractive index high viscosity, comprising the following steps:
(1) bleached shellac resin and tertiary sodium phosphate are mixed and heated to 90 DEG C, insulated and stirred is uniform；
(2) it is added after beeswax liquid being heated to 90 DEG C to step (1) and obtains in lac resin liquid, and insulated and stirred 0.5h is extremely
Uniformly, 60 DEG C are then cooled to；
(3) vinyl silicone oil, containing hydrogen silicone oil, melamino-formaldehyde resin, modified gas phase titanic oxide are obtained with step (2)
Solution is kept the temperature at 60 DEG C to be sufficiently mixed uniformly, and high-pressure homogeneous primary at 60MPa, obtains component one；
(4) component two is obtained after being sufficiently mixed vinyl silicone oil and platinum catalyst uniformly；
(5) component one and component two are applied after mixing.
Embodiment 4: a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, by component one and two groups of component
At:
The parts by weight of one raw material of component match are as follows: 70 parts of vinyl silicone oil, 15 parts of bleached shellac resin, hydrogeneous
8 parts of silicone oil, 8 parts of melamino-formaldehyde resin, 10 parts of beeswax liquid, 0.5 part of tertiary sodium phosphate, 40 parts of modified gas phase titanic oxide, it is described
The parts by weight of component two match are as follows: 10 parts and 0.8 part of platinum catalyst of vinyl silicone oil.
Further, the preparation method is the same as that of Example 1 for the modified gas phase titanic oxide.
A kind of preparation method of the LED transparent organic silicon casting glue of high refractive index high viscosity, specific steps are the same as real
Apply example 1.
Embodiment 5: a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, by component one and two groups of component
At:
The parts by weight of one raw material of component match are as follows: 62 parts of vinyl silicone oil, 22 parts of bleached shellac resin, hydrogeneous
7 parts of silicone oil, 10 parts of melamino-formaldehyde resin, 7 parts of beeswax liquid, 0.9 part of tertiary sodium phosphate, 25 parts of modified gas phase titanic oxide, it is described
The parts by weight of component two match are as follows: 14 parts and 0.5 part of platinum catalyst of vinyl silicone oil.
Further, the preparation method is the same as that of Example 1 for the modified gas phase titanic oxide.
A kind of preparation method of the LED transparent organic silicon casting glue of high refractive index high viscosity, specific steps are the same as real
Apply example 1.
Comparative example 1: a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, by component one and two groups of component
At:
The parts by weight of one raw material of component match are as follows: 65 parts of vinyl silicone oil, 20 parts of bleached shellac resin, hydrogeneous
6 parts of silicone oil, 12 parts of melamino-formaldehyde resin, 8 parts of beeswax liquid, 0.8 part of tertiary sodium phosphate, 30 parts of gas phase titanium dioxide, the component
The parts by weight of two raw materials match are as follows: 12 parts and 0.6 part of platinum catalyst of vinyl silicone oil.
A kind of preparation method of the LED transparent organic silicon casting glue of the high refractive index high viscosity, comprising the following steps:
(1) bleached shellac resin and tertiary sodium phosphate are mixed and heated to 85 DEG C, insulated and stirred is uniform；
(2) it is added after beeswax liquid being heated to 85 DEG C to step (1) and obtains in lac resin liquid, and insulated and stirred 45min
To uniform, it is then cooled to 55 DEG C；
(3) solution for obtaining vinyl silicone oil, containing hydrogen silicone oil, melamino-formaldehyde resin, gas phase titanium dioxide with step (2)
Heat preservation is sufficiently mixed uniformly at 55 DEG C, and high-pressure homogeneous primary at 50MPa, obtains component one；
(4) component two is obtained after being sufficiently mixed vinyl silicone oil and platinum catalyst uniformly；
(5) component one and component two are applied after mixing.
The performance of the obtained casting glue of above-described embodiment 1-5 and comparative example 1 is tested, it will be in above-described embodiment 1-5
Casting glue component one and component two are placed in container and are quickly uniformly mixed, and are placed in vacuum tank and place under the vacuum degree of 10 supports
10min is poured and solidifies the film for being prepared into 2mm thickness, its basic performance of standardized test, and with commercial clear organic silicon potting adhesive
Identical test is done for comparative example 2, as a result as shown in the table:
The average grain diameter of gas phase titanium dioxide is 21nm, is lower than visible wavelength 1/10th, nanoscale gas phase titanium dioxide
Titanium is applied to can avoid the rayleigh scattering phenomenon of colloid in encapsulating colloid, but directly gas phase titanium dioxide is added to organosilicon and fills
It processes and uses in adhesive body, generate serious aggregation between powder particle, cause the scattering of light, the serious light for reducing composite colloid is worn
Saturating rate and refractive index, particle buildup cause particle uneven distribution while to affect particle heating conduction in organic silicon substrate
Performance.Therefore gas phase titanium dioxide has been carried out modification by the present invention, to realize gas phase titanium dioxide and organic silicon substrate
Between it is good dissolve each other or dispersibility.Meanwhile the present invention by lac resin and beeswax liquid, tertiary sodium phosphate, melamino-formaldehyde resin and
After organosilicon material etc. is mixed and modified, the mechanical property and adhesive property of organosilicon material are considerably increased, while obtaining
Encapsulating glue material moisture-inhibiting oxygen permeability is smaller, is a kind of good electronic package material of comprehensive performance.
Claims (4)
1. a kind of LED transparent organic silicon casting glue of high refractive index high viscosity, which is characterized in that by component one and two groups of component
At:
The constitutive material of the component one are as follows: vinyl silicone oil, bleached shellac resin, containing hydrogen silicone oil, melamino-formaldehyde resin, bee
Wax liquor, tertiary sodium phosphate, modified gas phase titanic oxide, the constitutive material of the component two are as follows: vinyl silicone oil and platinum catalyst；
The parts by weight of the component one match are as follows: 60~70 parts of vinyl silicone oil, 15~25 parts of bleached shellac resin, hydrogeneous
5~8 parts of silicone oil, 8~15 parts of melamino-formaldehyde resin, 5~10 parts of beeswax liquid, 0.5~1 part of tertiary sodium phosphate, modified gas phase titanium dioxide
15~40 parts of titanium, the parts by weight proportion of the component two are as follows: 10~15 parts of vinyl silicone oil and platinum catalyst 0.4~0.8
Part.
2. a kind of LED transparent organic silicon casting glue of high refractive index high viscosity according to claim 1, it is characterised in that:
It is made of component one and component two, the parts by weight proportion of one raw material of component are as follows: 65 parts of vinyl silicone oil, bleached shellac
20 parts of resin, 6 parts of containing hydrogen silicone oil, 12 parts of melamino-formaldehyde resin, 8 parts of beeswax liquid, 0.8 part of tertiary sodium phosphate, modified gas phase titanium dioxide
30 parts of titanium, the parts by weight proportion of two raw material of component are as follows: 12 parts and 0.6 part of platinum catalyst of vinyl silicone oil.
3. a kind of LED transparent organic silicon casting glue of high refractive index high viscosity according to claim 1 or 2, feature exist
In: the modified gas phase titanic oxide the preparation method comprises the following steps: the gas phase titanium dioxide and gas phase three that will be dried aoxidize
Two aluminium are placed in the NaOH solution that concentration is 10mol/L, are heated with stirring to 60 DEG C, are added and gas phase titanium dioxide under insulated and stirred
Mass ratio is the epoxychloropropane solution of 5:1, and heat preservation return stirring reacts 4h, and then with methanol, pure water, cleaning product is extremely repeatedly
PH is to obtain modified gas phase titanic oxide after 7,100 DEG C of vacuum dryings.
4. a kind of described in any item preparation sides of the LED transparent organic silicon casting glue of high refractive index high viscosity claim 1-3
Method, which comprises the following steps:
(1) bleached shellac resin and tertiary sodium phosphate are mixed and heated to 80~90 DEG C, insulated and stirred is uniform；
(2) it is added after beeswax liquid being heated to 80~90 DEG C to step (1) and obtains in lac resin liquid, and insulated and stirred 0.5~
Then 1h is cooled to 50~60 DEG C to uniform；
(3) solution for obtaining vinyl silicone oil, containing hydrogen silicone oil, melamino-formaldehyde resin, modified gas phase titanic oxide with step (2)
Heat preservation is sufficiently mixed uniformly at 50~60 DEG C, and high-pressure homogeneous primary at 40~60MPa, obtains component one；
(4) component two is obtained after being sufficiently mixed vinyl silicone oil and platinum catalyst uniformly；
(5) component one and component two are applied after mixing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110066634A (en) * | 2019-05-22 | 2019-07-30 | 谢灵卫 | A kind of wear-resisting high-strength degree epoxyn, preparation method and application |
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| CN107974232A (en) * | 2017-12-27 | 2018-05-01 | 烟台德邦先进硅材料有限公司 | A kind of LED chip insulating heat-conductive crystal-bonding adhesive and preparation method thereof |
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2019
- 2019-02-23 CN CN201910134497.9A patent/CN109852337A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107974232A (en) * | 2017-12-27 | 2018-05-01 | 烟台德邦先进硅材料有限公司 | A kind of LED chip insulating heat-conductive crystal-bonding adhesive and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 严吴南 等: "《建筑材料性能学》", 31 December 1996, 重庆大学出版社 * |
| 王杏 等: "《纳米二氧化钛的生产与应用》", 31 July 2014, 贵州科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110066634A (en) * | 2019-05-22 | 2019-07-30 | 谢灵卫 | A kind of wear-resisting high-strength degree epoxyn, preparation method and application |
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Application publication date: 20190607 |