Silicone optical adhesive, method for preparing the same, and electronic packaging material

Abstract

This application provides an organosilicon optical adhesive, its preparation method, and an electronic packaging material. The organosilicon optical adhesive comprises component A, component B, and graphene oxide. By weight, component A comprises 40-80 parts vinyl silicone resin, 30-60 parts vinyl silicone oil, 10-20 parts MQ silicone resin without active hydrogen groups, 1-5 parts vinyl POSS, and 0.01-0.1 parts catalyst. By weight, component B comprises 10-50 parts hydrogen-containing silicone oil, 10-20 parts MQ silicone resin, 0-5 parts vinyl-free POSS, and 0.01-0.1 parts inhibitor. The graphene oxide content is 0.1%-10% by weight, based on the total mass of the organosilicon optical adhesive. The organosilicon optical adhesive of this application possesses both excellent flame retardant and mechanical properties.

Description

Technical Field

[0001] This application relates to the field of silicone material technology, and in particular to an organosilicon optical adhesive and its preparation method, as well as electronic packaging materials. Background Technology

[0002] Silicone optical adhesives are widely used in flexible displays, touch panels, and optical packaging devices due to their excellent optical transparency, flexibility, weather resistance, and chemical stability. However, as electronic devices develop towards higher performance and thinner designs, higher requirements are being placed on the flame retardancy and safety of core optical materials.

[0003] Traditional silicone optical adhesives are mainly based on polysiloxanes. Their molecular structure is easily decomposed under high temperature or open flame conditions, making it difficult to form a dense and continuous char layer. This results in a low limiting oxygen index and poor flame retardant properties, which greatly limits their application in high-end electronic products with stringent safety and reliability requirements.

[0004] Traditional techniques improve the flame retardancy of silicone optical adhesives by adding flame retardants. Common flame retardants include halogenated, phosphorus-based, nitrogen-based, and inorganic hydroxides. However, introducing flame retardants into highly transparent silicone optical adhesives presents several challenges: First, flame retardants significantly reduce the optical transmittance of the adhesive and increase haze, failing to meet the basic requirements for optical applications. Second, flame retardants have poor compatibility with the silicone matrix, easily migrating or separating, which not only causes the flame retardant performance to decay over time but may also affect the long-term bonding stability and mechanical properties of the adhesive. Third, some flame retardants may produce toxic fumes or corrosive gases when exerting their flame-retardant effect, posing secondary safety hazards.

[0005] Therefore, how to improve the flame retardant properties of silicone optical adhesives while maintaining their mechanical and optical properties has become a problem to be solved. Summary of the Invention

[0006] Based on this, one or more embodiments of this application provide an organosilicon optical adhesive with both excellent flame retardant and mechanical properties, a method for preparing the same, and an electronic packaging material.

[0007] According to a first aspect of the embodiments of this application, an organosilicon optical adhesive is provided, comprising component A, component B and graphene oxide;

[0008] By mass, component A comprises 40-80 parts vinyl silicone resin, 30-60 parts vinyl silicone oil, 10-20 parts MQ silicone resin without active hydrogen groups, 1-5 parts vinyl POSS and 0.01-0.1 parts catalyst;

[0009] By weight, component B comprises 10-50 parts of hydrogen-containing silicone oil, 10-20 parts of MQ silicone resin, 0-5 parts of vinyl-free POSS, and 0.01-0.1 parts of inhibitor;

[0010] The graphene oxide has a mass fraction of 0.3% to 1%, based on the total mass of the silicone optical adhesive.

[0011] In some embodiments, the graphene oxide sheet length and sheet width are both less than 2 μm.

[0012] In some embodiments, the thickness of the graphene oxide is 0.7 nm to 1 nm.

[0013] In some embodiments, the graphene oxide has a mass fraction of 1% to 5% based on the total mass of the silicone optical adhesive.

[0014] In some embodiments, by weight, component A comprises 50-60 parts vinyl silicone resin, 40-50 parts vinyl silicone oil, 12-18 parts MQ silicone resin without active hydrogen groups, 2-4 parts vinyl POSS and 0.03-0.08 parts catalyst.

[0015] By weight, component B comprises 20-40 parts of hydrogen-containing silicone oil, 12-18 parts of MQ silicone resin, 2-3 parts of vinyl-free POSS, and 0.03-0.08 parts of inhibitor.

[0016] In some embodiments, the mass ratio of component A to component B is 1:(0.5~1.5).

[0017] According to a second aspect of the embodiments of this application, a method for preparing an organosilicon optical adhesive is provided, comprising the following steps:

[0018] The raw materials are provided according to the above-mentioned silicone optical adhesive;

[0019] The raw materials for preparing component A are mixed to prepare component A;

[0020] The raw materials for preparing component B are mixed to prepare component B;

[0021] The organosilicon optical adhesive is prepared by mixing the components A and B with the graphene oxide and then curing it.

[0022] In some embodiments, mixing component A, component B, and graphene oxide includes the following steps:

[0023] The A component, the graphene oxide, and the solvent are mixed and dispersed to prepare a mixed slurry; then the mixed slurry is mixed with the B component.

[0024] In some embodiments, the curing temperature is 65°C to 75°C and the curing time is 3 to 5 hours.

[0025] According to a third aspect of the present application, an electronic packaging material is provided, including the above-described silicone optical adhesive or the silicone optical adhesive prepared by the above-described method.

[0026] Compared with traditional technologies, this application has the following advantages:

[0027] In the silicone optical adhesive of this application, graphene oxide has a large specific surface area and excellent barrier properties. When burning, it can form a dense, continuous and strong carbonaceous barrier layer on the surface of the silicone optical adhesive material, thus effectively isolating heat and oxygen. This significantly improves the limiting oxygen index of the silicone optical adhesive, reduces its heat release rate, and maintains its high light transmittance, excellent bonding strength and weather resistance. Detailed Implementation

[0028] To make the above-mentioned objectives, features, and advantages of this application more apparent and understandable, a detailed description of specific embodiments of this application is provided. Many specific details are set forth in the following description to provide a thorough understanding of this application. However, this application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of this application. Therefore, this application is not limited to the specific embodiments disclosed below.

[0029] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. Unless otherwise specifically stated, all raw materials, reagents, instruments, and equipment used in this application are commercially available or can be prepared by existing methods.

[0030] The terms "and / or," "or / and," and "and / or" as used herein include any one of two or more of the related listed items, as well as any and all combinations of the related listed items. These arbitrary and all combinations include any two related listed items, any more related listed items, or a combination of all related listed items. It should be noted that when at least three items are connected by at least two conjunctions selected from "and / or," "or / and," and "and / or," it should be understood that in this application, the technical solution undoubtedly includes technical solutions connected by "logical AND," and also undoubtedly includes technical solutions connected by "logical OR." For example, "A and / or B" includes three parallel solutions: A, B, and A+B. For example, the technical solution of "A, and / or, B, and / or, C, and / or, D" includes any one of A, B, C, and D (that is, a technical solution that is connected by "logical OR"), as well as any and all combinations of A, B, C, and D, that is, combinations of any two or three of A, B, C, and D, and also combinations of all four of A, B, C, and D (that is, a technical solution that is connected by "logical AND").

[0031] In this application, the terms "multiple", "various", "multiple times", "multi-dimensional", etc., unless otherwise specified, refer to a quantity greater than or equal to 2. For example, "one or more" means one or more than or equal to two.

[0032] The terms “combinations of,” “any combination of,” and “any combination of” used in this article include all suitable combinations of any two or more of the listed items.

[0033] In this document, the term "suitable" as used in phrases such as "suitable combination," "suitable method," and "any suitable method" refers to the ability to implement the technical solution of this application, solve the technical problem of this application, and achieve the expected technical effect of this application.

[0034] In this document, terms such as “preferred,” “better,” “more suitable,” and “ideal” are merely used to describe implementation methods or examples that achieve better results, and should be understood not to limit the scope of protection of this application.

[0035] In this application, terms such as "further," "even further," and "particularly" are used to describe purposes and indicate differences in content, but should not be construed as limiting the scope of protection of this application.

[0036] In this application, "optionally," "optionally," and "optional" mean that something is optional, that is, it means that it is selected from either "with" or "without." If there are multiple "optional" entries in a technical solution, unless otherwise specified and there are no contradictions or mutual constraints, each "optional" entry shall be independent.

[0037] In this application, the terms "first aspect," "second aspect," "third aspect," "fourth aspect," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or quantity, nor should they be construed as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first," "second," "third," "fourth," etc., serve only as a non-exhaustive enumeration and should be understood not to constitute a closed limitation on quantity.

[0038] In this application, the technical features described in an open-ended manner include both closed technical solutions consisting of the listed features and open technical solutions that include the listed features.

[0039] In this application, numerical intervals (i.e., numerical ranges) are involved. Unless otherwise specified, the selected numerical distributions within the aforementioned numerical intervals are considered continuous and include the two endpoints (i.e., the minimum and maximum values) of the numerical range, as well as every value between these two endpoints. Unless otherwise specified, when a numerical interval refers only to integers within that interval, it includes the two endpoint integers of the numerical range, as well as every integer between the two endpoints. In this document, this is equivalent to directly listing every integer. For example, if t is an integer selected from 1 to 10, it means that t is any integer selected from the group of integers consisting of 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10. Furthermore, when multiple ranges are provided to describe features or characteristics, these ranges can be merged. In other words, unless otherwise specified, the ranges disclosed herein should be understood to include any and all subranges to which they are included.

[0040] Unless otherwise specified, the temperature parameters in this application are permitted to be either constant-temperature treatment or variations within a certain temperature range. It should be understood that the constant-temperature treatment allows temperature fluctuations within the precision range of the instrument control, such as ±5℃, ±4℃, ±3℃, ±2℃, or ±1℃.

[0041] In this application, "room temperature" or "normal temperature" generally refers to 4℃~35℃, for example, 20℃±5℃. In some embodiments of this application, "room temperature" or "normal temperature" refers to 10℃~30℃. In some embodiments of this application, "room temperature" or "normal temperature" refers to 20℃~30℃.

[0042] In this application, %(w / w) and wt% both represent weight percentage, %(v / v) refers to volume percentage, and %(w / v) refers to mass-volume percentage.

[0043] Some embodiments of this application provide an organosilicon optical adhesive, comprising component A, component B, and graphene oxide;

[0044] By mass, component A comprises 40-80 parts vinyl silicone resin, 30-60 parts vinyl silicone oil, 10-20 parts MQ silicone resin without active hydrogen groups, 1-5 parts vinyl POSS and 0.01-0.1 parts catalyst;

[0045] By weight, component B comprises 10-50 parts of hydrogen-containing silicone oil, 10-20 parts of MQ silicone resin, 0-5 parts of vinyl-free POSS, and 0.01-0.1 parts of inhibitor;

[0046] The graphene oxide has a mass fraction of 0.1% to 10% based on the total mass of the silicone optical adhesive.

[0047] It should be noted that MQ silicone resin is a type of organosilicon resin with siloxane as the main chain. Its molecular structure consists of M units (monofunctional siloxane units) and Q units (tetrafunctional siloxane units). POSS refers to polyhedral oligomeric silsesquioxane.

[0048] This application incorporates graphene oxide into silicone optical adhesives. Due to its large specific surface area and excellent barrier properties, graphene oxide can form a dense, continuous, and robust carbonaceous barrier layer on the surface of the silicone optical adhesive material during combustion. This effectively isolates the AB adhesive from external heat and oxygen, thereby increasing the limiting oxygen index of the silicone optical adhesive, reducing its heat release rate, and maintaining its high light transmittance, excellent adhesive strength, and weather resistance.

[0049] As an example, based on the total mass of the silicone optical adhesive, the mass fraction of graphene oxide can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, or any value within the range of any two of the above points.

[0050] Furthermore, based on the total mass of the silicone optical adhesive, the mass fraction of graphene oxide is 0.3% to 1%.

[0051] By controlling the mass fraction of graphene oxide within the above-mentioned range, this application can not only effectively improve the flame retardant properties of silicone optical adhesives, but also avoid affecting the improvement of their mechanical properties.

[0052] Understandably, graphene oxide has a large thickness and strong sheet rigidity. The carbon layer structure formed under high temperature conditions has good stability and is not easy to crack, thus having good heat insulation and oxygen barrier effects.

[0053] In some embodiments, the graphene oxide of this application is a single-layer graphene oxide.

[0054] Understandably, component A, vinyl silicone resin, is a three-dimensional network structure polysiloxane containing multiple reactive vinyl groups (such as Vi and CH2=CH-); it has a significant impact on the hardness, strength, modulus, heat resistance, and adhesion of adhesives. Vinyl silicone oil, as an active diluent and toughening agent, can adjust the flowability, modulus, and elongation of adhesives. MQ silicone resin, without active hydrogen groups, acts as a reinforcing agent, improving the mechanical strength and adhesion of adhesives. POSS is a polyhedral oligomeric silsesquioxane, an organic-inorganic hybrid material with a nanoscale cage structure; each corner of vinyl POSS contains a vinyl group, which can chemically bond to the vulcanized network, significantly improving the strength, hardness, heat resistance, and abrasion resistance of adhesives at extremely low dosages, while also improving optical transparency and flame retardancy.

[0055] In component B, under the action of a platinum catalyst, the Si-H bonds of the polysiloxane containing active Si-H bonds undergo a hydrosilylation reaction with the vinyl (Vi) in component A to form a Si-CH2-CH2-Si bridging structure, thereby achieving three-dimensional network cross-linking and curing from liquid to elastomer.

[0056] As an example, the mass fraction of vinyl silicone resin in component A can be 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, or 80 parts, or any value within the range formed by any two of the above points.

[0057] In some embodiments, the vinyl content in the vinyl silicone resin is 0.9% to 1.9% by mass. As an example, the vinyl content in the vinyl silicone resin can be 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, or any value within the range formed by any two of the above points.

[0058] As an example, the mass fraction of vinyl silicone oil in component A can be 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, or 60 parts, or any value within the range formed by any two of the above points.

[0059] In some embodiments, the vinyl content in the vinyl silicone oil is 0.1% to 0.5% by mass. As an example, the vinyl content in the vinyl silicone oil can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, or any value within the range formed by any two of the above points.

[0060] In some embodiments, the viscosity of the vinyl silicone oil is 300 cps to 10000 cps. As an example, the viscosity of the vinyl silicone oil can be 300 cps, 400 cps, 500 cps, 600 cps, 700 cps, 800 cps, 900 cps, 1000 cps, 1000 cps, 2000 cps, 3000 cps, 4000 cps, 5000 cps, 6000 cps, 7000 cps, 8000 cps, 9000 cps, 10000 cps, or any value within the range formed by any two of the above points.

[0061] Unless otherwise specified, the viscosity of ethylene ester silicone oil in this application refers to the viscosity measured at 25°C.

[0062] As an example, the mass fraction of MQ silicone resin in component A that does not contain active hydrogen groups can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, or 20 parts, or any value within the range formed by any two of the above points.

[0063] As an example, the mass fraction of vinyl POSS in component A can be 1 part, 2 parts, 3 parts, 4 parts, 5 parts, or any value within the range formed by any two of the above points.

[0064] As an example, the mass fraction of catalyst in component A can be 0.01 parts, 0.02 parts, 0.03 parts, 0.04 parts, 0.05 parts, 0.06 parts, 0.07 parts, 0.08 parts, 0.09 parts, or 0.1 parts, or any value within the range formed by any two of the above points.

[0065] In some embodiments, the catalyst in component A comprises a platinum complex. Further, the catalyst in component A comprises a diluted platinum complex. Even further, the catalyst is diluted with a vinyl silicone oil with a viscosity of 100 cps. Even further, the dilution factor is 1000 times.

[0066] In some specific examples, the platinum complex is selected from platinum-divinylsiloxane complexes.

[0067] As an example, the mass fraction of hydrogen-containing silicone oil in component B can be 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, or 50 parts, or any value within the range formed by any two of the above points.

[0068] In some embodiments, the hydrogen content in the hydrogen-containing silicone oil is 0.1% to 0.5% by mass. As an example, the hydrogen content in the hydrogen-containing silicone oil can be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, or any value within the range formed by any two of the above points.

[0069] As an example, the mass fraction of MQ silicone resin in component B can be 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, or 20 parts, or any value within the range formed by any two of the above points.

[0070] As an example, the mass fraction of vinyl-free POSS in component B can be 0, 1, 2, 3, 4, or 5 parts, or any value within the range of any two of the above points.

[0071] As an example, the mass fraction of the inhibitor in component B can be 0.01 parts, 0.02 parts, 0.03 parts, 0.04 parts, 0.05 parts, 0.06 parts, 0.07 parts, 0.08 parts, 0.09 parts, or 0.1 parts, or any value within the range formed by any two of the above points.

[0072] In some embodiments, the inhibitor in component B includes one or more of alkynyl alcohol inhibitors and silicone-based inhibitors. Further, the inhibitor is diluted with a vinyl silicone oil with a viscosity of 100 cps. Even further, the dilution factor is 1000 times.

[0073] In some embodiments, the graphene oxide sheet length and sheet width are both less than 2 μm according to the above-described silicone optical adhesive.

[0074] It is understandable that controlling the length and width of graphene oxide sheets within the aforementioned specific range allows them to be more uniformly distributed in the resin matrix and less prone to agglomeration; moreover, smaller-sized graphene oxide has a larger specific surface area and more oxygen-containing functional groups on its surface, which can more fully combine with the resin matrix and promote the formation of a stable carbon layer at high temperatures.

[0075] In some embodiments, the thickness of the graphene oxide is 0.7 nm to 1 nm. As an example, the thickness of the graphene oxide can be 0.7 nm, 0.8 nm, 0.9 nm, 1 nm, or any value within the range formed by any two of the above values.

[0076] In some embodiments, the mass ratio of component A to component B is 1:(0.5~1.5).

[0077] As an example, the mass ratio of component A to component B can be 1:0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9, 1:1, 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, or any value within the range formed by any two of the above ratios.

[0078] In some specific examples, the mass ratio of component A to component B is 1:(0.8~1.2).

[0079] In some specific examples, the mass ratio of component A to component B is 1:1.

[0080] The organic optical adhesive described in this application not only improves the flame retardancy rating but also maintains good mechanical properties and processability, making it suitable for mass production. Furthermore, the organic optical adhesive of this application is halogen-free and non-toxic, meeting environmental protection requirements and applicable to high-end electronics and new energy fields.

[0081] Some embodiments of this application also provide a method for preparing an organosilicon optical adhesive, comprising the following steps:

[0082] The raw materials are provided according to the above-mentioned silicone optical adhesive;

[0083] Mix the raw materials for preparing component A to prepare component A;

[0084] Mix the raw materials for preparing component B to prepare component B;

[0085] Components A and B are mixed with graphene oxide and cured to prepare an organosilicon optical adhesive.

[0086] In some embodiments, mixing component A, component B, and graphene oxide includes the following steps:

[0087] Component A, graphene oxide, and solvent are mixed and dispersed to prepare a mixed slurry; then the mixed slurry is mixed with component B.

[0088] In some specific examples, the dispersion processing method includes ultrasonic processing.

[0089] In some embodiments, the curing temperature is 65°C to 75°C and the curing time is 3 to 5 hours.

[0090] As an example, the curing temperature can be 65℃, 66℃, 67℃, 68℃, 69℃, 70℃, 71℃, 72℃, 73℃, 74℃, 75℃, or any value within the range of any two of the above values.

[0091] As an example, the curing time can be 3h, 4h, 5h, or any value within the range of any two of the above values.

[0092] In some of these embodiments, graphene oxide is prepared by the Hummers method.

[0093] The preparation method of the above-mentioned organosilicon optical adhesive has the advantages of simple and mature process, low cost and easy large-scale production.

[0094] Some embodiments of this application also provide an electronic packaging material, including the above-described silicone optical adhesive or the silicone optical adhesive prepared by the above-described method.

[0095] The present application will be further described below with reference to specific embodiments and comparative examples, but these should not be construed as limiting the scope of protection of the present application. Unless otherwise specified, the raw materials involved in the following specific embodiments are all commercially available, the instruments used are all commercially available, and the processes involved are conventionally selected by those skilled in the art unless otherwise specified.

[0096] The raw materials used in the embodiments and comparative examples of this application are from the following sources:

[0097] The vinyl silicone resin was purchased from Hubei Longsheng Sihai New Material Co., Ltd., model number SH-5202.

[0098] The vinyl silicone oil was purchased from Hubei Longsheng Sihai New Material Co., Ltd., model number JP-01V-10000;

[0099] The MQ silicone resin without active hydrogen groups was purchased from Hubei Xinyuhong Biomedical Technology Co., Ltd., model number MQ0012MQ0520;

[0100] The vinyl POSS was purchased from Anhui Aiyota Silicone Oil Co., Ltd., model IOTA 9502;

[0101] The platinum-divinylsiloxane complex was purchased from Guangzhou Silicon Friends New Materials Technology Co., Ltd., model number PT-5000YC;

[0102] The hydrogen-containing silicone oil was purchased from Jiujiang Runhe Synthetic Materials Co., Ltd., model number RH202-20;

[0103] The MQ silicone resin was purchased from Jiujiang Runhe Synthetic Materials Co., Ltd., and the model number is RH-CMQ-60.

[0104] Vinyl-free POSS was purchased from Anhui Aiyota Silicone Oil Co., Ltd., model IOTA 9501;

[0105] The ethynylcyclohexanol inhibitor was purchased from Guangzhou Silicon Friends New Materials Technology Co., Ltd., model number YZJ-1;

[0106] The graphene oxide was purchased from Shanghai McLean Biochemical Technology Co., Ltd., model number G699086.

[0107] Example 1

[0108] (1) Provide 60 parts of vinyl silicone resin, 35 parts of vinyl silicone oil, 15 parts of MQ silicone resin without active hydrogen groups, 3 parts of vinyl POSS, and 0.5 parts of platinum-divinylsiloxane complex diluted with vinyl silicone oil with a viscosity of 100 cps (dilution ratio of 1000:1); mix the above substances evenly to prepare component A.

[0109] (2) Provide 10 parts of hydrogen-containing silicone oil, 15 parts of MQ silicone resin, 2 parts of vinyl-free POSS, and 0.3 parts of ethynyl cyclohexanol inhibitor diluted with vinyl silicone oil with a viscosity of 100 cps (dilution ratio of 1000:1); mix the above substances evenly to prepare component B.

[0110] (3) Provide 230 mL of 98% sulfuric acid, 10 g of graphite powder, 5 g of sodium nitrate, and 30 g of potassium permanganate. Slowly add the above substances to a volumetric flask with an ice bath of 2 L, heat to 35 °C and stir for 30 min; then add 460 mL of water, heat to 95 °C and stir for 15 min; then add 700 mL of warm water and stir; finally add 25 mL of hydrogen peroxide, stir and filter in time, and wash with 5% hydrochloric acid solution to detect residual sulfate ions; place the sample in a vacuum dryer at 50 °C to obtain graphene oxide; screen graphene oxide with sheet length and width less than 2 μm and thickness between 0.7 nm and 1 nm for later use.

[0111] (4) Based on the total mass of component A, component B and graphene oxide, add 0.3 wt% graphene oxide to component A, and at the same time add n-heptane solution to dilute component A (the mass ratio of n-heptane to component A is 1:1). Use a 600W ultrasonic cell disruptor for 20 min, and then stir at 90℃ for 4 h; wait until there is no odor.

[0112] (5) Mix component A and component B at a mass ratio of 1:1 to remove bubbles, and bake at 70°C for 4 hours to cure, thus obtaining the silicone optical adhesive.

[0113] Example 2

[0114] It is basically the same as Example 1, except that the mass fraction of graphene oxide in step (4) is different; specifically, the mass fraction of graphene oxide in Example 2 is 5 wt%.

[0115] Example 3

[0116] It is basically the same as Example 1, except that the mass fraction of graphene oxide in step (4) is different; specifically, the mass fraction of graphene oxide in Example 3 is 10 wt%.

[0117] Example 4

[0118] It is basically the same as Example 1, except that the mass fraction of graphene oxide in step (4) is different; specifically, the mass fraction of graphene oxide in Example 4 is 20 wt%.

[0119] Example 5

[0120] It is basically the same as Example 1, except that the length and width of the graphene oxide sheets are between 3μm and 5μm.

[0121] Comparative Example 1

[0122] It is basically the same as Example 1, except that it does not include steps (3) and (4), that is, it directly mixes component A and component B in proportion, degasses and cures.

[0123] Comparative Example 2

[0124] It is basically the same as Example 2, except that graphene oxide is replaced with an equal mass of graphene.

[0125] The viscosity of components A and B after mixing with graphene oxide in the above examples and comparative examples was tested according to GB / T2794, and the results are shown in Table 1.

[0126] Table 1

[0127]

[0128] The thermal conductivity of the silicone optical adhesives prepared in the above examples and comparative examples was determined according to GB / T 10295-2008; the pull-out force and shear force of the silicone optical adhesives on the glass surface were determined according to GB / T 7124; the elongation at break and tensile strength were determined according to GB / T 528; and the dielectric constant was determined according to GB / T 1409. The test results are shown in Table 2.

[0129] Table 2

[0130]

[0131] The heat release rate, total heat release, CO release rate, and total smoke release of the silicone optical adhesives prepared in the above embodiments and comparative examples were measured in accordance with GB / T 16172, and the results are shown in Table 3.

[0132] Table 3

[0133]

[0134] The above results demonstrate that this application significantly improves the fire safety performance of the adhesive through formulation optimization. Among them, the graphene oxide content in Example 3, at 10% by mass, exhibits the most outstanding performance, with a peak heat release rate of 264.84 kW / m³. 2 ) and total heat release (27.94 MJ / m 2 Both were reduced to their lowest levels, decreasing by approximately 64% and 37% compared to Comparative Example 1, respectively. Simultaneously, the carbon monoxide release rate (0.002 g / s) and total smoke emission (491.28 m³) were also reduced. 2 / m 2 It also reaches the lowest level, achieving the best balance between flame retardancy, smoke suppression and low toxicity.

[0135] It is worth noting that, although the peak heat release rate of Comparative Example 2 was 447 kW / m², 2 The total heat release (40.15 MJ / m³) is relatively low, but its total heat release is relatively low. 2 The flame retardant effect is still close to the worst level, indicating that its flame retardant mechanism may only delay combustion and fail to effectively reduce the total amount of combustibles, which is a potential defect.

[0136] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0137] The embodiments described above are merely illustrative of several implementation methods of this application, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this application, and these all fall within the protection scope of this application. Therefore, the protection scope of this application should be determined by the appended claims.

Claims

1. An organosilicon optical adhesive, characterized in that, It includes component A, component B, and graphene oxide; the mass ratio of component A to component B is 1:(0.5~1.5). By mass, component A comprises 40-80 parts vinyl silicone resin, 30-60 parts vinyl silicone oil, 10-20 parts MQ silicone resin without active hydrogen groups, 1-5 parts vinyl POSS and 0.01-0.1 parts catalyst; By weight, component B comprises 10-50 parts of hydrogen-containing silicone oil, 10-20 parts of MQ silicone resin, 0-5 parts of vinyl-free POSS, and 0.01-0.1 parts of inhibitor; The graphene oxide has a mass fraction of 0.1% to 10% based on the total mass of the silicone optical adhesive; the graphene oxide has a sheet length and sheet width of less than 2 μm; and the graphene oxide has a thickness of 0.7 nm to 1 nm.

2. The silicone optical adhesive according to claim 1, characterized in that, Based on the total mass of the silicone optical adhesive, the mass fraction of the graphene oxide is 0.3% to 1%.

3. The silicone optical adhesive according to any one of claims 1 to 2, characterized in that, By mass, component A comprises 50-60 parts vinyl silicone resin, 40-50 parts vinyl silicone oil, 12-18 parts MQ silicone resin without active hydrogen groups, 2-4 parts vinyl POSS and 0.03-0.08 parts catalyst; By weight, component B comprises 20-40 parts of hydrogen-containing silicone oil, 12-18 parts of MQ silicone resin, 2-3 parts of vinyl-free POSS, and 0.03-0.08 parts of inhibitor.

4. A method for preparing an organosilicon optical adhesive, characterized in that, Includes the following steps: The raw material is provided according to any one of claims 1 to 3 for the organosilicon optical adhesive; The raw materials for preparing component A are mixed to prepare component A; The raw materials for preparing component B are mixed to prepare component B; The organosilicon optical adhesive is prepared by mixing the components A and B with the graphene oxide and then curing it.

5. The method for preparing the organosilicon optical adhesive according to claim 4, characterized in that, Mixing component A, component B, and graphene oxide includes the following steps: The A component, the graphene oxide, and the solvent are mixed and dispersed to prepare a mixed slurry; then the mixed slurry is mixed with the B component.

6. The method for preparing the organosilicon optical adhesive according to any one of claims 4 to 5, characterized in that, The curing temperature is 65℃~75℃, and the time is 3h~5h.

7. An electronic packaging material, characterized in that, The silicone optical adhesive includes the silicone optical adhesive prepared by any one of claims 1 to 3 or any one of claims 4 to 6.

Images