Glass encapsulation slurry and preparation method and application thereof
By selecting suitable glass components and introducing modified hydrogen-containing silicone oil crosslinking agents, the problem of degradation in existing glass encapsulation slurries in acidic and humid environments has been solved, and the effect of significantly improving acid resistance and water resistance is achieved, and its stability and applicability are enhanced.
Patent Information
- Application Number
- CN202510088020.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-21
- Publication Date
- 2025-05-13
- Estimated Expiration
- 2045-01-21
AI Technical Summary
Existing glass encapsulation slurries are susceptible to erosion in acidic and humid environments, resulting in reduced performance and poor packaging.
By selecting suitable glass ingredients, introducing a modified hydrogen-containing silicone oil crosslinking agent and a specific additive formulation, and optimizing the preparation process, the first and second mixes are formed, and combining dispersants and solvents, a glass encapsulated slurry with significant acid resistance and water resistance is prepared.
It significantly improves the acid and water resistance of glass encapsulated slurry, enhances its stability and electrical properties at high temperatures, and is suitable for packaging and protection of high-performance electronic devices.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of glass encapsulation slurry and relates to a glass encapsulation slurry and a preparation method and application thereof. Background Art
[0002] In the current glass encapsulation slurry technology, acid resistance and water resistance are important indicators to measure its performance. However, existing glass encapsulation slurries still have some problems in terms of acid resistance and water resistance. On the one hand, some glass encapsulation slurries are easily corroded in acidic environments, resulting in performance degradation and shortening service life; on the other hand, some slurries are easy to absorb water in humid environments, resulting in expansion, cracking and other adverse phenomena, affecting the encapsulation effect.
[0003] These problems in the prior art are mainly due to inappropriate selection of glass components, inappropriate types of additives, and imperfect preparation processes.
[0004] Therefore, it is necessary to improve the formula and preparation process of glass encapsulation slurry to improve its acid resistance and water resistance. Summary of the invention
[0005] The present invention proposes a new glass encapsulation slurry and a preparation method thereof, aiming to solve the problems existing in the prior art. The glass encapsulation slurry of the present invention significantly improves the acid resistance and water resistance of the slurry by selecting a suitable glass component, introducing a specific modified hydrogen-containing silicone oil cross-linking agent and an auxiliary agent formula, and combining an optimized preparation process. The glass encapsulation slurry of the present invention has significant advantages in improving the acid resistance and water resistance of electronic devices, and provides a new solution for the packaging 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 glass encapsulation slurry, the glass encapsulation slurry comprising a first batch material, a second batch material, a dispersant and a solvent;
[0008] The first batch material consists of a first glass powder and a first auxiliary agent;
[0009] The first glass powder consists of SiO2, H3BO3, Al2O3, TiO2, PbO, ZnO and MgO;
[0010] The preparation method of the first auxiliary agent is: after vinyl triethoxysilane, β-cellulose and beryllium oxide are mixed, a modified hydrogen-containing silicone oil cross-linking agent is added, stirred and reacted at 60-70° C. for 6-8 hours, and then washed and dried to obtain the first auxiliary agent;
[0011] The modified hydrogen-containing silicone oil cross-linking agent is obtained by modifying the hydrogen-containing silicone oil cross-linking agent with epoxy resin and distearoyloxyisopropylaluminate;
[0012] The second batch material consists of a second glass powder and a second auxiliary agent;
[0013] The second glass powder consists of SiO2, H3BO3, Al2O3, BaO and Sb2O3;
[0014] The preparation method of the second auxiliary agent is as follows: adding a mixture of polydimethylsiloxane, terpineol and polypropylene glycol to a mixture of polyanionic cellulose, zirconium oxide and polyvinyl alcohol, uniformly dispersing by ultrasonication, reacting at 50-60° C. for 5-7 hours, and washing and drying to obtain the second auxiliary agent.
[0015] Preferably, the glass encapsulation slurry comprises 50-60 parts of the first batch material, 30-40 parts of the second batch material, 1-2 parts of the dispersant and 15-20 parts of the solvent in parts by mass.
[0016] Preferably, the mass ratio of the first glass powder to the first auxiliary agent is 1:3-5.
[0017] Preferably, the mass ratio of the second glass powder to the second auxiliary agent is 1:2-3.
[0018] Preferably, the first glass powder is composed of 30-40 parts of SiO2, 20-30 parts of H3BO3, 10-20 parts of Al2O3, 3-5 parts of TiO2, 1-2 parts of PbO, 1-3 parts of ZnO and 2-5 parts of MgO in parts by mass;
[0019] Preferably, the second glass powder consists of 35-50 parts of SiO2, 15-20 parts of H3BO3, 15-20 parts of Al2O3, 0.5-2 parts of BaO and 3-5 parts of Sb2O3, calculated by mass.
[0020] Preferably, the mass ratio of vinyl triethoxysilane, β-cellulose and beryllium oxide is 1:1:1; the mass ratio of hydrogen-containing silicone oil crosslinking agent, epoxy resin and distearoyloxyisopropylaluminate is 8:2:1.
[0021] Preferably, the mass ratio of polydimethylsiloxane, terpineol and polypropylene glycol is 2:1.5:1; the mass ratio of polyanionic cellulose, zirconium oxide and polyvinyl alcohol is 2:1:0.5.
[0022] Preferably, the dispersant is propylene glycol polyether or polyethylene glycol.
[0023] Preferably, the solvent is selected from one of anhydrous ethanol, deionized water and isooctyl alcohol.
[0024] In a second aspect, the present invention provides a method for preparing a glass encapsulation slurry, the preparation method comprising the following steps:
[0025] 1) Preparation of the first batch
[0026] S11. After the components of the first glass powder are evenly mixed, the first additive is added and ultrasonically dispersed uniformly, melted at a temperature of 1000-1100 ℃ for 1-2h, quenched with water, and cooled to solidify;
[0027] S12. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a first batch material with a particle size of less than 5 μm;
[0028] 2) Preparation of the second batch
[0029] S21. After the components of the second glass powder are mixed uniformly, the second additive is added and ultrasonically dispersed uniformly, melted at a temperature of 1000-1100 ℃ for 1-2h, quenched with water, and cooled to solidify;
[0030] S22. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a second batch material with a particle size of less than 5 μm;
[0031] 3) At a temperature of 40-50° C., the first batch material and the second batch material are stirred evenly, and a dispersant and a solvent are added in sequence and mixed evenly to obtain a glass encapsulation slurry.
[0032] In a third aspect, there is provided a use of the glass encapsulation slurry of the present invention in improving the acid resistance and / or water resistance of electronic devices.
[0033] In a fourth aspect, there is provided application of the glass encapsulation slurry of the present invention in improving the stability of electronic devices.
[0034] Preferably, the stability includes thermal stability and electrical stability.
[0035] A fifth aspect provides use of the glass encapsulation slurry of the present invention in improving the dispersibility and / or fluidity of electronic devices.
[0036] In the present invention, the preparation method of the hydrogen-containing silicone oil cross-linking agent is as follows:
[0037] Mix methylhydrogendichlorosilane and hexamethyldisiloxane and add them into a reactor;
[0038] Concentrated sulfuric acid is added to the reactor as a catalyst to start the reaction, and water is slowly added during the reaction to maintain the catalytic equilibrium reaction;
[0039] After the reaction is completed, the product is washed to neutrality, the solvent and low-boiling substances are removed, and then filtered to obtain the hydrogen-containing silicone oil cross-linking agent.
[0040] In the present invention, the modified hydrogenated silicone oil crosslinking agent is obtained by modifying the hydrogenated silicone oil crosslinking agent with epoxy resin and distearyloxyisopropylaluminate. During the modification process, the silicon-hydrogen bond in the hydrogenated silicone oil crosslinking agent has a high reactivity; epoxy resin and distearyloxyisopropylaluminate are used as modifiers, and the specific functional groups they contain can react with the hydrogen atoms in the hydrogenated silicone oil crosslinking agent to form new chemical bonds. The formation of new chemical bonds not only changes the composition and arrangement of the molecular chains of the hydrogenated silicone oil crosslinking agent, but also has a profound impact on its performance. For example, the new chemical bonds (such as Si-C bonds) formed during the modification process are more stable than the original silicon-hydrogen bonds and are more resistant to the erosion of water molecules. For another example, the composition and arrangement of the molecular chains of the modified hydrogenated silicone oil crosslinking agent change, forming a tighter and more ordered structure. This structural change reduces the channels for water molecules to penetrate, thereby improving water resistance.
[0041] The possible reaction mechanism is as follows: the hydrogen atoms in the hydrogen-containing silicone oil crosslinker react with the epoxy groups in the epoxy resin to form new Si-C bonds, thereby introducing the chain segments of the epoxy resin into the molecular chain of the hydrogen-containing silicone oil crosslinker. The hydrocarbon part of distearoyloxyisopropylaluminate reacts with the hydrogen atoms in the hydrogen-containing silicone oil crosslinker, thereby introducing the ester group in distearoyloxyisopropylaluminate into the molecular chain of the hydrogen-containing silicone oil crosslinker.
[0042] Compared with the prior art, the beneficial effects of the present invention are:
[0043] The present invention significantly improves the acid resistance and water resistance of the glass encapsulation slurry by introducing a modified hydrogen-containing silicone oil crosslinking agent, optimizing the glass powder composition and the auxiliary agent formula, and the present invention also has good thermal stability and electrical stability. In short, the overall performance of the glass encapsulation slurry of the present invention is improved, and it is suitable for the packaging and protection of various high-performance electronic devices. Specifically,
[0044] (1) Improve acid resistance: On the one hand, SiO2 can form a tight silicon-oxygen network structure, improve the hardness and density of glass, and thus enhance its resistance to acid. The addition of Al2O3 can not only enhance the chemical stability of glass, but also react with hydrogen ions in acid to form a protective film to prevent further acid corrosion of glass. Other components such as TiO2, PbO, ZnO, MgO and BaO play a role in regulating the melting temperature, viscosity and chemical stability of glass, and also help to improve the acid resistance of glass. On the other hand, vinyl triethoxysilane, β-cellulose and beryllium oxide in the first auxiliary agent can react with the components in the glass powder to form a tighter glass network structure, reducing acid corrosion of glass; the second auxiliary agent can also form a protective film on the glass surface to prevent acid corrosion of glass. The first batch material composed of the first glass powder and the first auxiliary agent combined with the second batch material composed of the second glass powder and the second auxiliary agent can maximize the acid resistance of the glass encapsulation slurry.
[0045] (2) Improve water resistance: On the one hand, H3BO3 can react with other components in the glass to form a tighter glass network structure, reduce the penetration of water molecules, and thus improve the water resistance of the glass; SiO2 and Al2O3 can also form a tight silicon-oxygen network structure, improve the density and hardness of the glass, and reduce the erosion of water molecules. On the other hand, the modified hydrogenated silicone oil crosslinking agent in the first auxiliary agent can undergo a crosslinking reaction with the components in the glass powder to form a dense waterproof layer to prevent the penetration of water molecules; the components such as pine oil and polypropylene glycol in the second auxiliary agent can form a hydrophobic film on the glass surface, further improving the water resistance of the glass. The first batch composed of the first glass powder and the first auxiliary agent combined with the second batch composed of the second glass powder and the second auxiliary agent can maximize the water resistance of the glass encapsulation slurry.
[0046] (3) Improving thermal stability: By introducing modified hydrogenated silicone oil crosslinking agent, the high temperature resistance of the slurry is enhanced, so that it can maintain stable structure and performance in high temperature environment.
[0047] (4) Optimizing electrical stability: Through the specific glass powder composition and the first and second additive formulas, the components in the slurry that may cause changes in electrical properties are reduced, thereby improving the electrical stability of electronic devices.
[0048] (5) Good dispersibility and fluidity: The slurry of the present invention can be evenly coated on the surface of electronic devices during the preparation process, further improving the packaging effect and protection performance.
[0049] (6) Enhanced mechanical strength: The addition of modified hydrogenated silicone oil crosslinking agent and other auxiliary ingredients enables the slurry to form a stronger protective layer after curing, thereby improving the mechanical strength of electronic devices.
[0050] In summary, the present invention has significantly improved the acid resistance, water resistance and stability of the glass encapsulation slurry by carefully selecting the components of the glass powder and the additives and optimizing the preparation process. This is mainly due to the effects of the components such as SiO2, Al2O3, H3BO3 in the glass powder, and the synergistic effect of the first additive, the second additive and the glass powder. DETAILED DESCRIPTION
[0051] The present invention will be described in detail below in conjunction with specific implementations and examples, and the advantages and various effects of the present invention will be more clearly presented. It should be understood by those skilled in the art that these specific implementations and examples are used to illustrate the present invention, rather than to limit the present invention.
[0052] The technical scheme of the present invention is described below in conjunction with the examples, but 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.
[0053] Example 1
[0054] This embodiment provides a glass encapsulation slurry, which includes 50 parts of a first batch material, 30 parts of a second batch material, 1 part of propylene glycol polyether and 15 parts of anhydrous ethanol in parts by weight;
[0055] The first batch material consists of a first glass powder and a first auxiliary agent, and the mass ratio of the first glass powder to the first auxiliary agent is 1:3;
[0056] The first glass powder is composed of 30 parts of SiO2, 20 parts of H3BO3, 10 parts of Al2O3, 3 parts of TiO2, 1 part of PbO, 1 part of ZnO and 2 parts of MgO in terms of mass fractions;
[0057] The preparation method of the first auxiliary agent is: vinyl triethoxysilane, β-cellulose and beryllium oxide are mixed in a mass ratio of 1:1:1, and a modified hydrogen-containing silicone oil cross-linking agent is added to react at 65° C. with stirring for 7 hours, and then the first auxiliary agent is obtained after washing and drying;
[0058] The modified hydrogenated silicone oil crosslinking agent is obtained by modifying the hydrogenated silicone oil crosslinking agent with epoxy resin and distearoyloxyisopropylaluminate, and the mass ratio of the hydrogenated silicone oil crosslinking agent, the epoxy resin and the distearoyloxyisopropylaluminate is 8:2:1;
[0059] The second batch material consists of a second glass powder and a second auxiliary agent, and the mass ratio of the second glass powder to the second auxiliary agent is 1:2;
[0060] The second glass powder is composed of 35 parts of SiO2, 15 parts of H3BO3, 15 parts of Al2O3, 0.5 parts of BaO and 33 parts of Sb2O3 in terms of mass fractions;
[0061] The preparation method of the second auxiliary agent is as follows: adding a mixture of polydimethylsiloxane, terpineol and polypropylene glycol to a mixture of polyanionic cellulose, zirconium oxide and polyvinyl alcohol, uniformly dispersing by ultrasonication, reacting at 60° C. for 6 hours, and washing and drying to obtain the second auxiliary agent;
[0062] The mass ratio of polydimethylsiloxane, terpineol and polypropylene glycol is 2:1.5:1; the mass ratio of polyanionic cellulose, zirconium oxide and polyvinyl alcohol is 2:1:0.5.
[0063] Example 2
[0064] This embodiment provides a glass encapsulation slurry, which includes 60 parts of a first batch material, 40 parts of a second batch material, 2 parts of polyethylene glycol and 20 parts of deionized water, in terms of weight percentage;
[0065] The first batch material consists of a first glass powder and a first auxiliary agent, and the mass ratio of the first glass powder to the first auxiliary agent is 1:5;
[0066] The first glass powder is composed of 40 parts of SiO2, 30 parts of H3BO3, 20 parts of Al2O3, 5 parts of TiO2, 2 parts of PbO, 3 parts of ZnO and 5 parts of MgO in terms of mass fractions;
[0067] The preparation method of the first auxiliary agent is: vinyl triethoxysilane, β-cellulose and beryllium oxide are mixed in a mass ratio of 1:1:1, and a modified hydrogen-containing silicone oil cross-linking agent is added to react at 65° C. with stirring for 7 hours, and then the first auxiliary agent is obtained after washing and drying;
[0068] The modified hydrogenated silicone oil crosslinking agent is obtained by modifying the hydrogenated silicone oil crosslinking agent with epoxy resin and distearoyloxyisopropylaluminate, and the mass ratio of the hydrogenated silicone oil crosslinking agent, the epoxy resin and the distearoyloxyisopropylaluminate is 8:2:1;
[0069] The second batch material consists of a second glass powder and a second auxiliary agent, and the mass ratio of the second glass powder to the second auxiliary agent is 1:3;
[0070] The second glass powder is composed of 50 parts of SiO2, 320 parts of H3BO, 320 parts of Al2O3, 2 parts of BaO and 35 parts of Sb2O in terms of mass fractions;
[0071] The preparation method of the second auxiliary agent is as follows: adding a mixture of polydimethylsiloxane, terpineol and polypropylene glycol to a mixture of polyanionic cellulose, zirconium oxide and polyvinyl alcohol, uniformly dispersing by ultrasonication, reacting at 60° C. for 6 hours, and washing and drying to obtain the second auxiliary agent;
[0072] The mass ratio of polydimethylsiloxane, terpineol and polypropylene glycol is 2:1.5:1; the mass ratio of polyanionic cellulose, zirconium oxide and polyvinyl alcohol is 2:1:0.5.
[0073] Example 3
[0074] This embodiment provides a glass encapsulation slurry, which includes 55 parts of a first batch material, 35 parts of a second batch material, 2 parts of polyethylene glycol, and 16 parts of isooctyl alcohol, in terms of weight percentage;
[0075] The first batch material consists of a first glass powder and a first auxiliary agent, and the mass ratio of the first glass powder to the first auxiliary agent is 1:4;
[0076] The first glass powder is composed of 32 parts of SiO2, 22 parts of H3BO3, 16 parts of Al2O3, 4 parts of TiO2, 2 parts of PbO, 2 parts of ZnO and 3 parts of MgO in terms of mass fractions;
[0077] The preparation method of the first auxiliary agent is: vinyl triethoxysilane, β-cellulose and beryllium oxide are mixed in a mass ratio of 1:1:1, and a modified hydrogen-containing silicone oil cross-linking agent is added to react at 65° C. with stirring for 7 hours, and then the first auxiliary agent is obtained after washing and drying;
[0078] The modified hydrogenated silicone oil crosslinking agent is obtained by modifying the hydrogenated silicone oil crosslinking agent with epoxy resin and distearoyloxyisopropylaluminate, and the mass ratio of the hydrogenated silicone oil crosslinking agent, the epoxy resin and the distearoyloxyisopropylaluminate is 8:2:1;
[0079] The second batch material consists of a second glass powder and a second auxiliary agent, and the mass ratio of the second glass powder to the second auxiliary agent is 1:2-3;
[0080] The second glass powder consists of 36 parts of SiO2, 17 parts of H3BO3, 16 parts of Al2O3, 1 part of BaO and 34 parts of Sb2O in terms of mass fractions;
[0081] The preparation method of the second auxiliary agent is as follows: adding a mixture of polydimethylsiloxane, terpineol and polypropylene glycol to a mixture of polyanionic cellulose, zirconium oxide and polyvinyl alcohol, uniformly dispersing by ultrasonication, reacting at 60° C. for 6 hours, and washing and drying to obtain the second auxiliary agent;
[0082] The mass ratio of polydimethylsiloxane, terpineol and polypropylene glycol is 2:1.5:1; the mass ratio of polyanionic cellulose, zirconium oxide and polyvinyl alcohol is 2:1:0.5.
[0083] Example 4
[0084] This embodiment provides a method for preparing a glass encapsulation slurry, the preparation method comprising the following steps:
[0085] 1) Preparation of the first batch
[0086] S11. After the components of the first glass powder are uniformly mixed in proportion, the prepared first additive is added in proportion, melted at a temperature of 1000-1100 ℃ for 1-2h, quenched with water, and cooled to solidify;
[0087] S12. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a first batch material with a particle size of less than 5 μm;
[0088] 2) Preparation of the second batch
[0089] S21. After the components of the second glass powder are uniformly mixed in proportion, the prepared second additive is added in proportion, melted at a temperature of 1000-1100 ℃ for 1-2h, quenched in water, and cooled to solidify;
[0090] S22. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a second batch material with a particle size of less than 5 μm;
[0091] 3) At a temperature of 40-50° C., the prepared first batch material and the second batch material are stirred evenly according to a proportion, and a dispersant and a solvent are added in sequence according to a proportion and mixed evenly to obtain a glass encapsulation slurry.
[0092] Comparative Example 1
[0093] This comparative example is the same as Example 3, except that the vinyl triethoxy silane in the first auxiliary agent is replaced by vinyl trimethoxy silane.
[0094] Comparative Example 2
[0095] This comparative example is the same as Example 3, except that the polyvinyl alcohol in the second auxiliary agent is replaced by polyethylene glycol.
[0096] Comparative Example 3
[0097] This comparative example is the same as Example 3, except that the first auxiliary agent is not added.
[0098] Effect verification
[0099] Experimental objects: glass encapsulation slurry prepared according to Example 4 in Examples 1-3 and Comparative Examples 1-3;
[0100] Experimental methods:
[0101] The above glass encapsulation slurry was screen-printed on a 1206-size alumina substrate, dried at 150°C for 12 minutes, and then cured at 200°C for 32 minutes to prepare a sample, and then the performance test was performed;
[0102] Acid resistance test: Soak the sample in 20% dilute sulfuric acid solution for 48 hours, tear off the sample with 3M tape, and observe whether it falls off;
[0103] Water resistance test: Place the sample in 95°C distilled water (pure and free of impurities) and immerse it completely for 48 hours, and calculate the water resistance loss value;
[0104] Thermal stability test: quickly heat the sample to 500°C, then quickly cool it down to observe whether the sample has cracks, deformation or falling off;
[0105] Breakdown voltage test: Apply gradually increasing voltage to the sample until it breaks down, record the breakdown voltage value, and evaluate the electrical insulation performance and voltage resistance of the sample;
[0106] Experimental results: as shown in Table 1.
[0107] Table 1 Performance test results of each group of samples
[0108]
[0109] In order to further demonstrate the effect of the present invention, the β-cellulose, beryllium oxide, epoxy resin and distearoyloxyisopropylaluminate in the first auxiliary agent are replaced by other substances with similar properties in the embodiment of the present invention, and the other conditions are consistent with those in Example 3. The results show that the effect is equivalent to that of Comparative Example 1.
[0110] In order to further demonstrate the effect of the present invention, the polydimethylsiloxane, terpineol, polypropylene glycol, polyanionic cellulose and zirconium oxide in the second auxiliary agent are replaced by other substances with similar properties in the embodiment of the present invention, and the other conditions are consistent with those in Example 3. The results show that the effect is equivalent to that of Comparative Example 2.
[0111] In order to further demonstrate the effect of the present invention, the second auxiliary agent was not added in the example of the present invention, and the other conditions were consistent with those in Example 3. It was found that the effect was equivalent to that in Comparative Example 3.
[0112] It can be seen from Table 1 that the performances of each group of samples made from the glass encapsulation slurry of the present invention are relatively good. Specifically, with regard to acid resistance, each group of samples made from the glass encapsulation slurry of the present invention has excellent acid resistance, and no shedding occurs; while each group of samples in Comparative Examples 1-3 has a large amount of shedding, which means that it cannot maintain sufficient durability in an acidic environment. With regard to water resistance, each group of samples made from the glass encapsulation slurry of the present invention has excellent water resistance, all <0.1, among which the water resistance of the sample in Example 3 is the best; while each group of samples in Comparative Examples 1-3 has poor water resistance. With regard to thermal stability, each group of samples made from the glass encapsulation slurry of the present invention has excellent thermal stability, with no cracks, deformation, or shedding at 500°C; while each group of samples in Comparative Examples 1-3 has a large degree of deformation and shedding. Regarding the breakdown voltage, the breakdown voltage of each group of samples of the present invention can reach a relatively high level and is very stable, among which the breakdown voltage value of the sample of Example 3 is the highest; while the breakdown voltage of each group of samples of Comparative Examples 1-3 is relatively low. Therefore, compared with the glass encapsulation slurry without the formula system of the present invention, the glass encapsulation slurry using the formula system of the present invention can be well used for the packaging and protection of various high-performance electronic devices.
[0113] In addition, the present invention also verified the electrical stability, dispersibility and fluidity of each group of samples. The results showed that each group of samples made of the glass encapsulation slurry of the present invention performed well in terms of electrical stability, dispersibility and fluidity, among which the electrical stability, dispersibility and fluidity of the samples in Example 3 were even better.
[0114] Through the effect verification experiment, it can be known that the formula system of the glass encapsulation slurry provided by the present invention is a whole. Specifically, the functions of the various raw materials in the glass encapsulation slurry support each other and there is an interactive relationship. It is precisely because the functions of the various raw materials support each other and there is an interactive relationship that the glass encapsulation slurry of the formula system of the present invention can be well used for the packaging and protection of various high-performance electronic devices.
[0115] It should be understood that the disclosed invention is not limited only to the specific method, scheme and material of description, because these all can change.It should also be understood that the terminology used herein is only for the purpose of describing specific embodiment scheme, rather than being intended to limit the scope of the present invention, and the scope of the present invention is only limited to the appended claims.
Claims
1. A glass encapsulation slurry, characterized in that: The glass encapsulation slurry comprises a first batch material, a second batch material, a dispersant and a solvent; The first batch material consists of a first glass powder and a first auxiliary agent; The first glass powder consists of SiO2, H3BO3, Al2O3, TiO2, PbO, ZnO and MgO; The preparation method of the first auxiliary agent is: after vinyl triethoxysilane, β-cellulose and beryllium oxide are mixed, a modified hydrogen-containing silicone oil cross-linking agent is added, stirred and reacted at 60-70° C. for 6-8 hours, and then washed and dried to obtain the first auxiliary agent; The modified hydrogen-containing silicone oil cross-linking agent is obtained by modifying the hydrogen-containing silicone oil cross-linking agent with epoxy resin and distearoyloxyisopropylaluminate; The second batch material consists of a second glass powder and a second auxiliary agent; The second glass powder consists of SiO2, H3BO3, Al2O3, BaO and Sb2O3; The preparation method of the second auxiliary agent is as follows: adding a mixture of polydimethylsiloxane, terpineol and polypropylene glycol to a mixture of polyanionic cellulose, zirconium oxide and polyvinyl alcohol, uniformly dispersing by ultrasonication, reacting at 50-60° C. for 5-7 hours, and washing and drying to obtain the second auxiliary agent; Calculated by weight, the glass encapsulation slurry includes 50-60 parts of a first batch material, 30-40 parts of a second batch material, 1-2 parts of a dispersant and 15-20 parts of a solvent.
2. The glass encapsulation slurry according to claim 1, characterized in that: The mass ratio of the first glass powder to the first auxiliary agent is 1:3-5.
3. The glass encapsulation slurry according to claim 1, characterized in that: The mass ratio of the second glass powder to the second auxiliary agent is 1:2-3.
4. The glass encapsulation slurry according to claim 1, characterized in that: Calculated by weight, the first glass powder consists of 30-40 parts of SiO2, 20-30 parts of H3BO3, 10-20 parts of Al2O3, 3-5 parts of TiO2, 1-2 parts of PbO, 1-3 parts of ZnO and 2-5 parts of MgO.
5. The glass encapsulation slurry according to claim 1, characterized in that: Calculated by weight, the second glass powder consists of 35-50 parts of SiO2, 15-20 parts of H3BO3, 15-20 parts of Al2O3, 0.5-2 parts of BaO and 3-5 parts of Sb2O3.
6. The glass encapsulation slurry according to claim 1, characterized in that: The mass ratio of vinyltriethoxysilane, β-cellulose and beryllium oxide is 1:1:1; The mass ratio of hydrogen-containing silicone oil crosslinking agent, epoxy resin and distearoyloxyisopropylaluminate is 8:2:
1.
7. The glass encapsulation slurry according to claim 1, characterized in that: The mass ratio of polydimethylsiloxane, terpineol and polypropylene glycol is 2:1.5:1; The mass ratio of polyanionic cellulose, zirconium oxide and polyvinyl alcohol is 2:1:0.
5.
8. The method for preparing the glass encapsulation slurry according to any one of claims 1 to 7, characterized in that: The preparation method comprises the following steps: 1) Preparation of the first batch S11. After the components of the first glass powder are uniformly mixed, a first additive is added, melted at a temperature of 1000-1100 ℃ for 1-2h, quenched with water, and cooled to solidify; S12. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a first batch material with a particle size of less than 5 μm; 2) Preparation of the second batch S21. After the components of the second glass powder are evenly mixed, a second additive is added, melted at a temperature of 1000-1100 ℃ for 1-2h, quenched with water, and cooled to solidify; S22. The solidified mixture is successively crushed, ball-milled, sieved and dried to obtain a second batch material with a particle size of less than 5 μm; 3) At a temperature of 40-50° C., the first batch material and the second batch material are stirred evenly, and a dispersant and a solvent are added in sequence and mixed evenly to obtain a glass encapsulation slurry.
9. Use of the glass encapsulation slurry according to any one of claims 1 to 7 in improving the acid resistance and / or water resistance of electronic devices.
Citation Information
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