CN107286902A - A kind of preparation method of high heat conduction organosilicon filling and sealing gum - Google Patents

Abstract

The invention discloses a preparation method of a high thermal conductivity silicone potting glue, comprising the following steps: mixing and stirring boron phosphide and concentrated nitric acid for 5 hours, filtering, washing the solid with deionized water, and drying to obtain pretreated boron phosphide; Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate for 1 hour at a power of 1000W, add hydroxyl silicone oil, and continue to sonicate for 2-5 hours. After the sonication is completed, filter and dry to obtain a modified composite Filler: Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, defoamer and defoam to obtain silicone potting compound. The silicone potting glue prepared by the invention has excellent mechanical properties and good thermal conductivity.

Description

A kind of preparation method of high thermal conductivity silicone potting glue

Technical field:

The invention relates to the field of adhesives, in particular to a preparation method of high thermal conductivity silicone potting adhesive.

Background technique:

Since the 21st century, people are increasingly concerned about the global energy shortage, and the light-emitting diode (Light-Emitting Diode) LED, which is synonymous with low energy consumption and high-efficiency green light source, has attracted people's attention. LED is a semiconductor light-emitting device that can directly convert electrical energy into light energy. It has the advantages of simple structure, energy saving, long life, environmental protection, high luminous efficiency, and bright and rich colors. It is expected to become the fourth-generation lighting source. As a new type of lighting technology, LED is developing in the direction of high color, high luminous efficiency, high luminous uniformity, and high reliability in recent years. It has a very wide range of applications in landscape lighting, automotive lighting, traffic lighting, and special lighting. Applications. The performance of LED potting glue has an important impact on the brightness, luminous efficiency and service life of LED devices. The role of LED potting glue mainly has the following four aspects: (1) Seal and protect the LED chip, avoid the influence of moisture and temperature, improve reliability, and ensure the normal operation of the chip; (2) Improve heat dissipation capacity, timely and effectively eliminate The heat generated by the chip; (3) Optical control, reducing the difference in refractive index between the LED chip and the air, optimizing the distribution of the beam to achieve a specific optical distribution, maximizing the output of luminous flux, and playing the role of lens concentrating; (4 ) to mechanically hold and support the wire.

With the introduction of policies and plans for the development of the semiconductor lighting industry at home and abroad, the continuous improvement and improvement of LED technology has led to the rapid development of GaN-based power white light LEDs, and put forward more stringent requirements for the performance of LED potting compounds. However, the traditional epoxy resin potting compound has exposed many shortcomings and cannot meet the development needs of power LEDs. Therefore, it is necessary to develop materials with high light transmittance, high refractive index, high thermal conductivity, high adhesion, high strength, light aging resistance, heat aging resistance, thermal shock resistance, low thermal expansion coefficient, low stress, low ion content and low moisture absorption. Advanced silicone potting compound is the development trend of LED packaging and meets the development requirements of power LEDs.

Invention content:

The object of the present invention is to provide a method for preparing a high thermal conductivity silicone potting compound. The potting compound prepared by the method has good mechanical properties and excellent thermal conductivity.

To achieve the above object, the present invention adopts the following technical solutions:

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) boron phosphide and concentrated nitric acid were mixed and stirred for 5 hours, filtered, the solid was washed with deionized water, and dried to obtain pretreated boron phosphide;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate at 1000W for 1h, add hydroxyl silicone oil, and continue to sonicate for 2-5h. After sonication, filter and dry to obtain Modified composite filler;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, cross-linking agent, catalyst, inhibitor, and defoamer for defoaming to prepare silicone potting compound.

As a preference of the above technical solution, in step (1), the mass ratio of boron phosphide to concentrated nitric acid is 1:(20-40).

As a preference of the above technical solution, in step (2), the mass ratio of boron phosphide to h-BN is (0.3-0.6):1.

As a preference of the above technical solution, in step (2), the dosage ratio of h-BN to isopropanol is 1 g: (30-50) mL.

As the preference of the above technical solution, in step (2), the volume ratio of hydroxyl silicone oil to isopropanol is 10:1.

As a preference for the above technical solution, in step (3), the amounts of each component are in parts by weight: 40-70 parts of vinyl silicone oil, 30-50 parts of hydrogen-containing silicone oil, 3-7 parts of modified composite filler, 1-4 parts of dispersant, 0.5-1 part of crosslinking agent, 0.5-1 part of catalyst, 0.02-0.06 part of inhibitor, 1-2 parts of defoamer.

As a preference of the above technical solution, in step (3), the crosslinking agent is styryl polysiloxane.

As a preference of the above technical solution, in step (3), the catalyst is one of a platinum-vinylsiloxane complex, an alcohol-modified chloroplatinic acid catalyst, and a platinum-alkyne complex.

As a preference of the above technical solution, in step (3), the inhibitor is one of diethyl fumarate, diallyl maleate, and ethynylcyclohexanol.

As a preference of the above technical solution, in step (3), the dispersant is carboxyl-containing siloxane.

The present invention has the following beneficial effects:

The present invention uses boron phosphide and boron nitride compound to modify the silicone potting compound, and before the modification, the present invention firstly treats the composite filler, and treats the boron phosphide with nitric acid, so that the boron phosphide surface It has a small active point and can absorb macromolecules, and then in the process of stripping boron nitride, the present invention adds an appropriate amount of pretreated boron phosphide, and boron phosphide can effectively enter the stripped boron nitride layer between layers, effectively avoiding the polymerization between boron nitride layers, and more effectively improving the thermal conductivity of the filler; at the same time, the added hydroxyl silicone oil can be effectively adsorbed on the surface of boron phosphide with more active points, making the modified compound The compatibility between the filler and the matrix is greatly improved; the silicone potting adhesive prepared by the invention has excellent mechanical properties and good thermal conductivity.

detailed description:

In order to better understand the present invention, the present invention will be further described through the following examples, which are only used to explain the present invention and will not constitute any limitation to the present invention.

Example 1

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) Mix and stir boron phosphide and concentrated nitric acid for 5 hours, filter, wash the solid with deionized water, and dry to obtain pretreated boron phosphide; wherein, the mass ratio of boron phosphide to concentrated nitric acid is 1:20; The mass ratio of boron and h-BN is 0.3:1;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate for 1 hour at a power of 1000W, add hydroxyl silicone oil, and continue to sonicate for 2 hours. After sonication, filter and dry to obtain the modified Composite filler; wherein, the amount ratio of h-BN to isopropanol is 1g:30mL; the volume ratio of hydroxyl silicone oil to isopropanol is 10:1;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, and defoamer to prepare silicone potting glue; The dosage is in parts by weight: 40 parts of vinyl silicone oil, 30 parts of hydrogen-containing silicone oil, 3 parts of modified composite filler, 1 part of dispersant, 0.5 part of crosslinking agent, 0.5 part of catalyst, 0.02 part of inhibitor, defoamer 1 serving.

Example 2

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) Mix and stir boron phosphide and concentrated nitric acid for 5 hours, filter, wash the solid with deionized water, and dry to obtain pretreated boron phosphide; wherein, the mass ratio of boron phosphide to concentrated nitric acid is 1:40; The mass ratio of boron and h-BN is 0.6:1;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate at 1000W for 1h, add hydroxyl silicone oil, and continue to sonicate for 5h. After sonication, filter and dry to obtain the modified Composite filler; wherein, the amount ratio of h-BN to isopropanol is 1g:50mL; the volume ratio of hydroxyl silicone oil to isopropanol is 10:1;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, and defoamer to prepare silicone potting glue; The dosage in parts by weight is: 70 parts of vinyl silicone oil, 50 parts of hydrogen-containing silicone oil, 7 parts of modified composite filler, 4 parts of dispersant, 1 part of crosslinking agent, 1 part of catalyst, 0.06 part of inhibitor, defoamer 2 servings.

Example 3

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) Mix and stir boron phosphide and concentrated nitric acid for 5 hours, filter, wash the solid with deionized water, and dry to obtain pretreated boron phosphide; wherein, the mass ratio of boron phosphide to concentrated nitric acid is 1:24; The mass ratio of boron and h-BN is 0.4:1;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate at 1000W for 1h, add hydroxyl silicone oil, and continue to sonicate for 3h. After sonication, filter and dry to obtain the modified Composite filler; wherein, the amount ratio of h-BN to isopropanol is 1g:35mL; the volume ratio of hydroxyl silicone oil to isopropanol is 10:1;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, and defoamer to prepare silicone potting glue; The dosage is in parts by weight: 50 parts of vinyl silicone oil, 34 parts of hydrogen-containing silicone oil, 4 parts of modified composite filler, 2 parts of dispersant, 0.6 part of crosslinking agent, 0.6 part of catalyst, 0.03 part of inhibitor, defoamer 1.2 servings.

Example 4

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) Mix and stir boron phosphide and concentrated nitric acid for 5 hours, filter, wash the solid with deionized water, and dry to obtain pretreated boron phosphide; wherein, the mass ratio of boron phosphide to concentrated nitric acid is 1:28; The mass ratio of boron and h-BN is 0.4:1;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate for 1 hour at a power of 1000W, add hydroxyl silicone oil, and continue to sonicate for 3.5 hours. After sonication is completed, filter and dry to obtain modified permanent composite filler; wherein, the amount ratio of h-BN to isopropanol is 1g:40mL; the volume ratio of hydroxyl silicone oil to isopropanol is 10:1;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, and defoamer to prepare silicone potting glue; The dosage is in parts by weight: 55 parts of vinyl silicone oil, 38 parts of hydrogen-containing silicone oil, 5 parts of modified composite filler, 2 parts of dispersant, 0.7 part of crosslinking agent, 0.7 part of catalyst, 0.04 part of inhibitor, defoamer 1.4 servings.

Example 5

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) Mix and stir boron phosphide and concentrated nitric acid for 5 hours, filter, wash the solid with deionized water, and dry to obtain pretreated boron phosphide; wherein, the mass ratio of boron phosphide to concentrated nitric acid is 1:32; The mass ratio of boron and h-BN is 0.5:1;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then sonicate at 1000W for 1h, add hydroxyl silicone oil, and continue to sonicate for 4h. After sonication, filter and dry to obtain the modified Composite filler; wherein, the amount ratio of h-BN to isopropanol is 1g:40mL; the volume ratio of hydroxyl silicone oil to isopropanol is 10:1;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, and defoamer to prepare silicone potting glue; The dosage in parts by weight is: 60 parts of vinyl silicone oil, 42 parts of hydrogen-containing silicone oil, 6 parts of modified composite filler, 3 parts of dispersant, 0.8 part of crosslinking agent, 0.8 part of catalyst, 0.05 part of inhibitor, defoamer 1.6 servings.

Example 6

A preparation method of high thermal conductivity silicone potting compound, comprising the following steps:

(1) Mix and stir boron phosphide and concentrated nitric acid for 5 hours, filter, wash the solid with deionized water, and dry to obtain pretreated boron phosphide; wherein, the mass ratio of boron phosphide to concentrated nitric acid is 1:36; The mass ratio of boron and h-BN is 0.55:1;

(2) Mix and stir the boron phosphide and h-BN prepared above with isopropanol evenly, then ultrasonicate for 1 hour under 1000W power, add hydroxyl silicone oil, and continue ultrasonicating for 4.5 hours. After the ultrasonication is completed, filter and dry to obtain modified permanent composite filler; wherein, the amount ratio of h-BN to isopropanol is 1g:45mL; the volume ratio of hydroxyl silicone oil to isopropanol is 10:1;

(3) Mix vinyl silicone oil, hydrogen-containing silicone oil, modified composite filler, dispersant, crosslinking agent, catalyst, inhibitor, and defoamer to prepare silicone potting glue; The dosage is in parts by weight: 65 parts of vinyl silicone oil, 46 parts of hydrogen-containing silicone oil, 6 parts of modified composite filler, 3.5 parts of dispersant, 0.9 part of crosslinking agent, 0.9 part of catalyst, 0.05 part of inhibitor, defoamer 1.8 servings.

After testing, the tensile shear strength of the potting glue prepared by the present invention is as high as 6.7MPa, and the thermal conductivity is as high as 5.6W/m·k.

Claims (10)

1. a kind of preparation method of high heat conduction organosilicon filling and sealing gum, it is characterised in that comprise the following steps：

(1) boron phosphide and concentrated nitric acid are mixed into 5h, filtering, solid is washed with deionized, and dries, obtains pre-processing phosphatization Boron；

(2) boron phosphide obtained above and h-BN are mixed evenly with isopropanol, then ultrasound 1h under 1000W power, plus Enter hydroxy silicon oil, continue ultrasound 2-5h, after ultrasound is finished, filter, dry, modified compounded mix is made；

(3) by vinyl silicone oil, containing hydrogen silicone oil, modified compounded mix, dispersant, crosslinking agent, catalyst, inhibitor, defoamer Mix deaeration and organic silicon potting adhesive is made.

2. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (1), The mass ratio of the boron phosphide and concentrated nitric acid is 1：(20-40).

3. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (2), The boron phosphide, h-BN mass ratio are (0.3-0.6)：1.

4. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (2), The amount ratio of the h-BN and isopropanol are 1g：(30-50)mL.

5. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (2), The volume ratio of hydroxy silicon oil and isopropanol is 10:1.

6. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (3), The consumption of each component is respectively in parts by weight：40-70 parts of vinyl silicone oil, 30-50 parts of containing hydrogen silicone oil, modified compounded mix 3- 7 parts, 1-4 parts of dispersant, 0.5-1 parts of crosslinking agent, 0.5-1 parts of catalyst, 0.02-0.06 parts of inhibitor, 1-2 parts of defoamer.

7. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (3), The crosslinking agent is benzene alkenyl polysiloxanes.

8. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (3), The catalyst is one kind in platinum-vinyl siloxane complex, alcohol modification chloroplatinic acid catalyst, platinum-alkynes basigamy compound.

9. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：In step (3), The inhibitor is one kind in diethyl fumarate, diallyl maleate, ethynylcyclohexanol.

10. a kind of preparation method of high heat conduction organosilicon filling and sealing gum as claimed in claim 1, it is characterised in that：Step (3) In, the dispersant is siloxanes containing carboxyl.