An encapsulation paste, its preparation method and application

Abstract

The present invention belongs to the technical field of electronic packaging, and relates to a packaging paste, a preparation method thereof and an application. The present invention provides a packaging paste, which comprises glass powder and a carrier. Among them, the glass powder is composed of SiO2, B2O3, Al2O3, PbO, MgO and SrO; the preparation method of the carrier is: after mixing nano-zirconia and an additive in a mass ratio of 0.5:1-2, placing them in a mixer and blending for 3-5 h to obtain; the additive is composed of isooctyl acetate, γ-aminopropyltrimethoxysilane, propylene glycol polyether and butyl carbitol acetate. The packaging paste of the present invention can improve the water resistance of electronic devices.

Description

Technical Field

[0001] The invention belongs to the technical field of electronic packaging and relates to a packaging slurry and a preparation method and application thereof. Background Art

[0002] In the field of electronic packaging technology, packaging paste, as a key material, plays a vital role in the performance and reliability of electronic devices. Traditional packaging paste usually contains glass powder and organic carrier, which is used to achieve the connection and protection between electronic components and substrates.

[0003] Although traditional encapsulation pastes meet the needs of electronic packaging to a certain extent, they are still insufficient in terms of water resistance. This is mainly due to the fact that the composition of the glass powder and the properties of the carrier are not optimized enough, which makes the encapsulation layer easy to absorb water in a humid environment, thus affecting the electrical performance and long-term reliability of electronic devices. In addition, traditional carrier materials often contain components that are easily hydrolyzed, further exacerbating the water resistance problem of the encapsulation layer.

[0004] Therefore, it is necessary to improve the formulation and preparation process of the encapsulation slurry to improve its water resistance. Summary of the invention

[0005] The present invention proposes a new encapsulation slurry and a preparation method thereof, aiming to solve the problems existing in the prior art. The encapsulation slurry of the present invention significantly improves the water resistance of the encapsulation slurry by selecting a suitable glass component, introducing a specific carrier material and additives, and combining an optimized preparation process. The present invention provides a new solution for the encapsulation and protection of electronic devices.

[0006] To achieve the above object, the technical solution of the present invention is as follows:

[0007] In a first aspect, the present invention provides a packaging paste, wherein the packaging paste comprises glass powder and a carrier, wherein:

[0008] The glass powder consists of SiO2, B2O3, Al2O3, PbO, MgO and SrO;

[0009] The preparation method of the carrier is as follows: nano zirconium dioxide and additives are mixed in a mass ratio of 0.5:1-2, and then placed in a mixer and blended for 3-5 hours to obtain the carrier;

[0010] The additive consists of isooctyl acetate, gamma-aminopropyltrimethoxysilane, propylene glycol polyether and butyl carbitol acetate.

[0011] Preferably, the encapsulation slurry comprises 41-46 parts of glass powder and 30-36 parts of carrier in parts by mass.

[0012] Preferably, by mass parts, the glass powder is composed of 28 - 32 parts of SiO2, 10 - 12 parts of B2O3, 16 - 22 parts of Al2O3, 5 - 8 parts of PbO, 3 - 6 parts of MgO, and 1 - 3 parts of SrO.

[0013] Preferably, by mass parts, the additive is composed of 0.5 - 1 part of isooctyl acetate, 1 - 2 parts of γ-aminopropyltrimethoxysilane, 0.4 - 0.8 part of propylene glycol polyether, and 0.2 - 0.5 part of butyl carbitol acetate.

[0014] More preferably, by mass parts, the glass powder is composed of 31 parts of SiO2, 11 parts of B2O3, 20 parts of Al2O3, 6 parts of PbO, 5 parts of MgO, and 2 parts of SrO.

[0015] More preferably, by mass parts, the additive is composed of 0.6 part of isooctyl acetate, 1 part of γ-aminopropyltrimethoxysilane, 0.6 part of propylene glycol polyether, and 0.3 part of butyl carbitol acetate.

[0016] Preferably, the preparation method of the carrier is as follows: Mix nano-zirconia and the additive according to a mass ratio of 0.5:1, and then place them in a mixer for blending for 3 - 5 h to obtain.

[0017] In the second aspect, a preparation method of the encapsulation paste according to the present invention is provided, and the preparation method includes the following steps:

[0018] 1) Prepare glass powder

[0019] S11. After uniformly mixing the components of the glass powder, melt it at a temperature of 1000 - 1200 °C for 1.5 - 3 h, then perform water quenching and cooling solidification;

[0020] S12. Sequentially crush, ball mill, screen, and dry the solidified mixture to obtain glass powder with a particle size less than 5 μm;

[0021] 2) Prepare the carrier: Mix nano-zirconia and the additive according to a mass ratio of 0.5:1 - 2, and then place them in a mixer for blending for 3 - 5 h to obtain;

[0022] 3) Prepare the paste: At a temperature of 65 - 80 °C, ultrasonically disperse the glass powder and the carrier uniformly to obtain the encapsulation paste.

[0023] In the third aspect, a paste with good water resistance is provided, and the paste includes the encapsulation paste according to the present invention.

[0024] In the fourth aspect, an application of the encapsulation paste according to the present invention in improving the water resistance of electronic devices is provided.

[0025] In the fifth aspect, an application of the paste according to the present invention in improving the water resistance of electronic devices is provided.

[0026] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0027] By introducing specific carrier materials and additives, optimizing the composition of the glass powder and the preparation process, the present invention significantly improves the water resistance of the encapsulation paste. The present invention is applicable to the encapsulation and protection of high-performance electronic devices. Specifically,

[0028] By precisely controlling the proportions of SiO2, B2O3, Al2O3, PbO, MgO, and SrO in the glass powder, the present invention can form a more stable and dense glass phase structure. This structure has a lower water absorption rate and better moisture-proof performance, thus effectively improving the water resistance of the encapsulation layer. The addition of PbO can also adjust the softening point and viscosity of the glass phase, contributing to the formation of a more uniform encapsulation layer, and further reducing the water absorption rate of the glass phase structure.

[0029] When the present invention uses nano-zirconia in combination with an additive composed of isooctyl acetate, γ-aminopropyltrimethoxysilane, polypropylene glycol ether, and butyl carbitol acetate, it can not only enhance the interfacial bonding force between nano-zirconia and other materials in the electronic device, thereby improving the stability and water resistance of the overall structure, but also form a dense protective layer on the surface of the electronic device, effectively preventing the penetration and erosion of moisture.

[0030] In addition, the additive of the present invention not only helps to reduce the viscosity of the carrier, improve the dispersibility of the carrier, but also can form a stronger interaction with the glass powder, enhancing the cohesion of the encapsulation layer, which contributes to further improving the water resistance of the encapsulation layer.

[0031] Furthermore, by precisely controlling the melting temperature and time of the glass powder, as well as the blending conditions of the carrier and the dispersion temperature of the paste, the present invention can ensure that the encapsulation paste has the optimal composition and performance. In particular, the application of the ultrasonic dispersion step can further refine the particle sizes of the glass powder and the carrier, improve the uniformity and stability of the paste, which is conducive to the formation of a more dense and uniform encapsulation layer, thereby improving the water resistance. Specific Embodiments

[0032] The following will specifically elaborate on the present invention in combination with specific embodiments and examples, and the advantages and various effects of the present invention will be presented more clearly therefrom. Those skilled in the art should understand that these specific embodiments and examples are used to illustrate the present invention, rather than limiting the present invention.

[0033] Next, the technical solutions of the present invention will be described in combination with examples. However, the present invention is not limited to the following examples. The experimental methods and detection methods described in each example are conventional methods unless otherwise specified; the reagents and materials described are commercially available unless otherwise specified.

[0034] Example 1

[0035] This example provides a packaging paste. By mass fraction, the packaging paste includes 41 parts of glass powder and 30 parts of carrier. Among them,

[0036] the glass powder is composed of 28 parts of SiO2, 10 parts of B2O3, 16 parts of Al2O3, 5 parts of PbO, 3 parts of MgO and 1 part of SrO;

[0037] The preparation method of the carrier is as follows: nano-zirconia and additives are mixed at a mass ratio of 0.5:1 and then placed in a mixer for 3 h of blending to obtain it;

[0038] the additives are composed of 0.5 part of isooctyl acetate, 1 part of γ-aminopropyltrimethoxysilane, 0.4 part of propylene glycol polyether and 0.2 part of butyl carbitol acetate.

[0039] Example 2

[0040] This example provides a packaging paste. By mass fraction, the packaging paste includes 46 parts of glass powder and 36 parts of carrier. Among them,

[0041] the glass powder is composed of 32 parts of SiO2, 12 parts of B2O3, 22 parts of Al2O3, 8 parts of PbO, 6 parts of MgO and 3 parts of SrO;

[0042] The preparation method of the carrier is as follows: nano-zirconia and additives are mixed at a mass ratio of 0.5:2 and then placed in a mixer for 5 h of blending to obtain it;

[0043] the additives are composed of 1 part of isooctyl acetate, 2 parts of γ-aminopropyltrimethoxysilane, 0.8 part of propylene glycol polyether and 0.5 part of butyl carbitol acetate.

[0044] Example 3

[0045] This example provides a packaging paste. By mass fraction, the packaging paste includes 43 parts of glass powder and 32 parts of carrier. Among them,

[0046] the glass powder is composed of 31 parts of SiO2, 11 parts of B2O3, 20 parts of Al2O3, 6 parts of PbO, 5 parts of MgO and 2 parts of SrO;

[0047] The preparation method of the carrier is as follows: nano-zirconia (Wuhan Lanabai Pharmaceutical Chemical Co., Ltd., 1314-23-4) and additives are mixed at a mass ratio of 0.5:1 and then placed in a mixer for 4 h of blending to obtain it.

[0048] The additive is composed of 0.6 parts of isooctyl acetate, 1 part of γ-aminopropyltrimethoxysilane, 0.6 parts of propylene glycol polyether, and 0.3 parts of butyl carbitol acetate.

[0049] Example 4

[0050] This example provides a method for preparing a packaging paste, and the preparation method includes the following steps:

[0051] 1) Prepare glass powder

[0052] S11. After mixing the components of the glass powder evenly, melt them at a temperature of 1000 - 1200 °C for 1.5 - 3 h, then quench with water and cool and solidify;

[0053] S12. Crush, ball mill, screen, and dry the solidified mixture in sequence to obtain glass powder with a particle size less than 5 μm;

[0054] 2) Prepare the carrier: Mix nano-zirconia and the additive in a mass ratio of 0.5:1 - 2, and place them in a mixer for 3 - 5 h of blending to obtain it;

[0055] 3) Prepare the paste: At a temperature of 65 - 80 °C, ultrasonically disperse the glass powder and the carrier evenly to obtain the packaging paste.

[0056] Comparative Example 1

[0057] This comparative example is the same as Example 3, the difference is that: isooctyl acetate in the additive is replaced by ethyl acetate.

[0058] Comparative Example 2

[0059] This comparative example is the same as Example 3, the difference is that: the mass ratio of nano-zirconia to the additive is adjusted to 0.5:0.5.

[0060] Comparative Example 3

[0061] This comparative example is the same as Example 3, the difference is that: nano-zirconia is replaced by zirconia.

[0062] Effect verification

[0063] Experimental objects: The packaging pastes prepared according to Example 4 for Examples 1 - 3 and Comparative Examples 1 - 3;

[0064] Experimental method:

[0065] Print the above-mentioned packaging pastes on 1206 - sized alumina substrates by screen printing, dry them at 140 °C for 15 min, then cure them at 200 °C for 30 min to make sample pieces, and then immerse the sample pieces completely in distilled water (pure and impurity - free) at 95 °C for 96 h, and calculate the water resistance reduction value;

[0066] Experimental results: As shown in Table 1.

[0067] Table 1 Water resistance test results of each group of sample pieces

[0068]

[0069] To further prove the effect of the present invention, in the embodiments of the present invention, γ-aminopropyltrimethoxysilane, propylene glycol polyether and butyl carbitol acetate in the additive are respectively replaced with other substances with similar properties, and the remaining conditions are the same as those in Example 3. It is found that the effect is equivalent to that of Comparative Example 1.

[0070] To further prove the effect of the present invention, in the embodiments of the present invention, the mass ratio of nano-zirconia to the additive is adjusted to 0.5:2.5, and the remaining conditions are the same as those in Example 3. It is found that the effect is equivalent to that of Comparative Example 2.

[0071] As can be seen from Table 1, the water resistance of each group of sample pieces made of the encapsulation paste of the present invention is relatively good, all lower than 0.1. Among them, the water resistance of the sample piece of Example 3 is the best; while the water resistance of each group of sample pieces of Comparative Examples 1-3 is relatively poor. Therefore, compared with the encapsulation paste that does not use the formula system of the present invention, the encapsulation paste using the formula system of the present invention can be well used for the encapsulation and protection of high-performance electronic devices.

[0072] It can be seen from the effect verification experiment that the present invention significantly improves the water resistance of the encapsulation paste by introducing specific carrier materials and additives, optimizing the composition of the glass powder and the preparation process. The present invention is applicable to the encapsulation and protection of high-performance electronic devices.

[0073] By precisely controlling the proportions of SiO2, B2O3, Al2O3, PbO, MgO and SrO in the glass powder, the present invention can form a more stable and dense glass phase structure, which has a lower water absorption rate and better moisture-proof performance, thereby effectively improving the water resistance of the encapsulation layer. The addition of PbO can also adjust the softening point and viscosity of the glass phase, which helps to form a more uniform encapsulation layer, and further reduces the water absorption rate of the glass phase structure.

[0074] When the present invention uses nano-zirconia in combination with an additive composed of isooctyl acetate, γ-aminopropyltrimethoxysilane, propylene glycol polyether and butyl carbitol acetate, it can not only enhance the interfacial bonding force between nano-zirconia and other materials in the electronic device, thereby improving the stability and water resistance of the overall structure, but also form a dense protective layer on the surface of the electronic device, effectively preventing the penetration and erosion of moisture.

[0075] In addition, the additive of the present invention not only helps to reduce the viscosity of the carrier and improve the dispersibility of the carrier, but also can form a stronger interaction with the glass powder, enhance the cohesion of the encapsulation layer, and contribute to further improving the water resistance of the encapsulation layer.

[0076] Furthermore, by precisely controlling the melting temperature and time of the glass powder, as well as the blending conditions of the carrier and the dispersion temperature of the slurry, the present invention can ensure that the encapsulation slurry has the optimal composition and performance. In particular, the application of the ultrasonic dispersion step can further refine the particle sizes of the glass powder and the carrier, improve the uniformity and stability of the slurry, and thus facilitate the formation of a denser and more uniform encapsulation layer.

[0077] In summary, the formulation system of the encapsulation slurry provided by the present invention is an integral whole. Specifically, the functions of the various raw materials in the encapsulation slurry support each other and interact with each other. It is precisely because the functions of the various raw materials support each other and interact with each other that the encapsulation slurry of the present invention's formulation system has excellent water resistance.

[0078] It should be understood that the present invention disclosed is not limited to the specific methods, schemes, and substances described, as these can vary. It should also be understood that the terms used herein are for the purpose of describing specific embodiments only and are not intended to limit the scope of the present invention, which is limited only by the appended claims.

Claims

1. A packaging slurry, characterized in that: The encapsulation paste comprises glass powder and a carrier, wherein: The glass powder consists of SiO2, B2O3, Al2O3, PbO, MgO and SrO; The preparation method of the carrier is as follows: nano zirconium dioxide and additives are mixed in a mass ratio of 0.5:1-2, and then placed in a mixer and blended for 3-5 hours to obtain the carrier; The additive is composed of isooctyl acetate, γ-aminopropyltrimethoxysilane, propylene glycol polyether and butyl carbitol acetate; In terms of weight, the encapsulation slurry includes 41-46 parts of glass powder and 30-36 parts of carrier; In terms of mass fractions, the glass powder consists of 28-32 parts of SiO2, 10-12 parts of B2O3, 16-22 parts of Al2O3, 5-8 parts of PbO, 3-6 parts of MgO and 1-3 parts of SrO.

2. The encapsulation paste according to claim 1, characterized in that: In terms of weight percentage, the additive consists of 0.5-1 part of isooctyl acetate, 1-2 parts of γ-aminopropyltrimethoxysilane, 0.4-0.8 parts of propylene glycol polyether and 0.2-0.5 parts of butyl carbitol acetate.

3. The encapsulation paste according to claim 1, characterized in that: In terms of mass fraction, the glass powder consists of 31 parts of SiO2, 11 parts of B2O3, 20 parts of Al2O3, 6 parts of PbO, 5 parts of MgO and 2 parts of SrO.

4. The encapsulation paste according to claim 3, characterized in that: In terms of mass parts, the additive consists of 0.6 parts of isooctyl acetate, 1 part of γ-aminopropyltrimethoxysilane, 0.6 parts of propylene glycol polyether and 0.3 parts of butyl carbitol acetate.

5. The encapsulation paste according to claim 1, characterized in that: The preparation method of the carrier is as follows: nano zirconium dioxide and additives are mixed in a mass ratio of 0.5:1, and the mixture is placed in a mixer and blended for 3-5 hours to obtain the carrier.

6. The method for preparing the encapsulation slurry according to any one of claims 1 to 5, characterized in that: The preparation method comprises the following steps: 1) Preparation of glass powder S11. After the components of the glass powder are evenly mixed, they are melted at a temperature of 1000-1200°C for 1.5-3h, quenched with water, and cooled to solidify; S12. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a glass powder having a particle size of less than 5 μm; 2) Preparation of carrier: Mix nano zirconium dioxide and additives in a mass ratio of 0.5:1-2, place in a mixer and blend for 3-5 hours; 3) Preparation of slurry: At a temperature of 65-80°C, the glass powder and the carrier are evenly dispersed by ultrasonic to obtain encapsulation slurry.

7. Use of the encapsulation slurry according to any one of claims 1 to 5 in improving the water resistance of electronic devices.

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