A high-temperature resistant addition-type one-component silicone rubber for electronic packaging

Abstract

The present invention provides a high-temperature resistant addition-type one-component silicone rubber for electronic packaging, which relates to the technical field of organic silicone rubber. The silicone rubber raw materials include vinyl-terminated polysiloxane, phenyl vinyl silicone oil, fumed silica, phenyltrimethoxysilane, high-temperature resistant filler, Al2O3-CeO2-Sb2O3 composite, hydrogen-containing silicone oil, platinum-alkyne complex, inhibitor, and antioxidant; the high-temperature resistant filler is prepared from aluminum phenylphosphinate, ammonium polyphosphate, and γ-aminopropyltriethoxysilane; the Al2O3-CeO2-Sb2O3 composite is prepared from aluminum nitrate, cerium nitrate, and potassium antimony tartrate. A preparation method for a high-temperature resistant addition-type one-component silicone rubber for electronic packaging includes the steps of synthesizing the Al2O3-CeO2-Sb2O3 composite, preparing the high-temperature resistant filler, dispersing the base filler, adding an auxiliary agent, and preparing the silicone rubber. The silicone rubber prepared by the present invention has strong high-temperature resistance, high mechanical strength, and excellent electrical insulation stability.

Description

Technical Field

[0001] The present invention relates to the technical field of organic silicone rubber, in particular to a high-temperature resistant addition-type single-component silicone rubber for electronic packaging. Background Art

[0002] Silicone rubber is a polymeric elastomer with a silicon-oxygen bond as its backbone, exhibiting properties such as high and low temperature resistance, chemical inertness, biocompatibility, and excellent electrical insulation. It is primarily classified into three types: high-temperature vulcanized, room-temperature vulcanized, and liquid silicone. Its applications span the electrical power, medical, automotive, food-grade products, and electronic seals sectors. While costlier than traditional rubber, silicone rubber offers significant advantages in extreme environmental stability, safety, and longevity.

[0003] With the widespread application of silicone rubber in electronic packaging, higher performance requirements are being placed on silicone rubber. Prior art publication CN116239990A discloses a high-temperature-resistant silicone sealant and its preparation method. This sealant's overall performance is enhanced through a cross-linking reaction between a hydrogenated polysilazane resin and α,ω-dihydroxypolydimethylsiloxane, combined with hydrogen adsorption and curing by a platinum-loaded 5A molecular sieve, chopped carbon fiber reinforcement, and vinyl fluorosilicone oil modification. However, the following issues remain: high-temperature resistance relies on a two-component system, which is less stable than a single-component system; and electrical insulation stability is poor.

[0004] In summary, although the existing technical solutions have improved certain properties of silicone rubber to a certain extent, the following technical problems still exist: poor high temperature resistance, low mechanical strength, and low electrical insulation stability. Summary of the Invention

[0005] In order to solve the above problems existing in the prior art, the present invention provides a high-temperature resistant addition-type one-component silicone rubber for electronic packaging, and achieves the following invention objectives: to prepare silicone rubber with strong high-temperature resistance, high mechanical strength and excellent electrical insulation stability.

[0006] To achieve the above objectives, the technical solutions adopted are as follows:

[0007] A high-temperature resistant addition-type one-component silicone rubber for electronic packaging comprises the following raw materials, measured in parts by weight: 30-40 parts of vinyl-terminated polysiloxane, 20-30 parts of phenyl vinyl silicone oil, 25-40 parts of fumed silica, 3-8 parts of phenyltrimethoxysilane, 10-15 parts of high-temperature resistant filler, 3-5 parts of Al2O3-CeO2-Sb2O3 composite, 8-12 parts of hydrogen-containing silicone oil, 0.3-0.5 part of platinum-alkyne complex, 0.1-0.15 part of inhibitor, and 0.5-1 part of antioxidant.

[0008] The viscosity of the vinyl terminated polysiloxane is 5000-10000 cSt, and the vinyl content is 0.15-0.35%.

[0009] The phenyl content of the phenyl vinyl silicone oil is 15-25%, and the vinyl content is 0.2-0.5%.

[0010] The particle size of the fumed silica is 7-16 nm.

[0011] The high-temperature resistant filler is prepared from aluminum phenylphosphinate, ammonium polyphosphate and gamma-aminopropyltriethoxysilane.

[0012] The Al2O3-CeO2-Sb2O3 composite is prepared from aluminum nitrate, cerium nitrate and potassium antimony tartrate.

[0013] The purity of the phenyltrimethoxysilane is ≥98%.

[0014] The Si—H content of the hydrogen-containing silicone oil is 0.8-1.6%.

[0015] The platinum-alkyne complex is Wacker CATALYST OL catalyst.

[0016] The inhibitor is a maleate inhibitor.

[0017] The antioxidant is a phosphite antioxidant.

[0018] The present invention also provides a method for preparing a high-temperature resistant addition-type single-component silicone rubber for electronic packaging, comprising the following steps:

[0019] Step 1: Synthesis of Al2O3-CeO2-Sb2O3 composite

[0020] Aluminum nitrate (Al(NO3)3), cerium nitrate (Ce(NO3)3・6H2O), and potassium antimony tartrate (KSbC4H4O7・1 / 2H2O) are dissolved in deionized water to prepare a mixed metal salt solution with a total metal ion concentration of 0.3-0.5 mol / L. The molar ratio of aluminum nitrate, cerium nitrate, and potassium antimony tartrate is 5:(2.8-3):(2-2.3).

[0021] The mixed metal salt solution is heated to 60-80°C, stirred at a rate of 300-500 rpm, and ammonia water is added dropwise while stirring to adjust the pH value of the solution to 9-10.5; after the addition is completed, the stirring reaction is continued for 1-2 hours; after the reaction is completed, the solution is allowed to stand for aging at a temperature of 60-80°C for 2-4 hours; after the aging is completed, the solution is washed alternately with deionized water and anhydrous ethanol for 3-5 times; the washed precipitate is dried at a temperature of 100-120°C for 12-18 hours to obtain a precursor; the precursor is calcined by heating to 600-700°C at a heating rate of 5-10°C / min and holding for 3-4 hours, and then cooled to obtain an Al2O3-CeO2-Sb2O3 complex.

[0022] Step 2: Prepare high temperature resistant filler

[0023] Aluminum phenylphosphinate and ammonium polyphosphate are added to a high-speed mixer at a speed of 800-900 rpm and stirred for 30-40 minutes. The mass ratio of aluminum phenylphosphinate to ammonium polyphosphate is (2-3):1 to obtain a mixed powder. γ-Aminopropyltriethoxysilane is added to the mixed powder and stirred. The γ-Aminopropyltriethoxysilane accounts for 3-4% of the mixed powder mass. The mixture is heated to 80-90°C, the speed is set to 500-600 rpm, and the stirring time is 40-60 minutes. The mixture is then vacuum dried at a temperature of 90-100°C, a vacuum degree of -0.09 MPa to -0.095 MPa, and a drying time of 2-3 hours to obtain a high-temperature resistant filler.

[0024] Step 3: Dispersion of basic fillers

[0025] Add vinyl-terminated polysiloxane and phenyl vinyl silicone oil to a planetary mixer at a speed of 100-200 rpm and stir for 10-15 minutes to obtain a base gum matrix. Add fumed silica and phenyltrimethoxysilane to the base gum matrix, raise the temperature to 80-120°C, set the vacuum degree to -0.09MPa to -0.095MPa, rotate at 50-100rpm, and stir for 2-4 hours. After stirring, cool to 50-60°C, add high-temperature resistant filler and Al2O3-CeO2-Sb2O3 composite, rotate at 80-150rpm, and stir for 30-60 minutes to obtain a basic mixed filler.

[0026] Step 4: Add additives

[0027] The hydrogen-containing silicone oil and the platinum-alkyne complex are mixed evenly to obtain a catalyst mother liquid; the inhibitor and the antioxidant are added to the basic mixed filler and stirred evenly; the catalyst mother liquid is added dropwise while stirring at a rotation speed of 100-150 rpm to obtain a mixed material after the addition is completed.

[0028] Step 5: Prepare silicone rubber

[0029] The mixed material is transferred to a vacuum degassing kettle, the vacuum degree is set to -0.095 MPa to -0.098 MPa, and the degassing time is 30-45 minutes; after the degassing is completed, it is filtered through a 200-mesh stainless steel filter and packaged in an aluminum-plastic composite tube or a vacuum sealed barrel to obtain silicone rubber.

[0030] The beneficial effects of the present invention are as follows:

[0031] (1) The silicone rubber prepared by the present invention has excellent mechanical strength, with a Shore A hardness of 69-74 Shore A, a tensile strength of 4.68-4.79 MPa, and an elongation at break of 382-395%.

[0032] (2) The silicone rubber prepared by the present invention has excellent high temperature resistance. After high temperature treatment, the Shore hardness reaches 73-79 Shore A, the tensile strength reaches 4.32-4.41 MPa, and has a high tensile strength retention rate.

[0033] (3) The silicone rubber prepared by the present invention has excellent electrical insulation stability, and its high-temperature volume resistivity reaches 1.9×10 14 -3.1×10 14 Ω·cm. DETAILED DESCRIPTION

[0034] To make the purpose, technical solutions and advantages of the present invention clearer, the embodiments of the present invention will be described in further detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention and are not intended to limit the present invention.

[0035] Example 1 A high-temperature resistant addition-type one-component silicone rubber for electronic packaging

[0036] A high-temperature resistant, addition-type, one-component silicone rubber for electronic packaging comprises the following raw materials, measured in parts by weight: 30 parts of vinyl-terminated polysiloxane, 30 parts of phenyl vinyl silicone oil, 25 parts of fumed silica, 8 parts of phenyltrimethoxysilane, 15 parts of high-temperature resistant filler, 5 parts of Al2O3-CeO2-Sb2O3 composite, 8 parts of hydrogen-containing silicone oil, 0.3 part of platinum-alkyne complex, 0.1 part of inhibitor, and 0.5 part of antioxidant.

[0037] A method for preparing a high-temperature resistant addition-type single-component silicone rubber for electronic packaging, comprising the following steps:

[0038] Step 1: Synthesis of Al2O3-CeO2-Sb2O3 composite

[0039] Aluminum nitrate, cerium nitrate and potassium antimony tartrate were dissolved in deionized water to prepare a mixed metal salt solution with a total metal ion concentration of 0.3 mol / L. The molar ratio of aluminum nitrate, cerium nitrate and potassium antimony tartrate was 5:2.8:2.

[0040] The mixed metal salt solution was heated to 60°C, stirred at a rate of 500 rpm, and ammonia water was added dropwise while stirring to adjust the pH value of the solution to 9; after the addition was completed, the stirring reaction was continued for 1 hour; after the reaction was completed, the solution was allowed to stand for aging at 60°C for 4 hours; after the aging was completed, the solution was washed alternately with deionized water and anhydrous ethanol 3 times; the washed precipitate was dried at 100°C for 18 hours to obtain a precursor; the precursor was calcined, the temperature was raised to 600°C, the heating rate was 5°C / min, the holding time was 4 hours, and the Al2O3-CeO2-Sb2O3 complex was obtained after cooling.

[0041] Step 2: Prepare high temperature resistant filler

[0042] Aluminum phenylphosphinate and ammonium polyphosphate were added to a high-speed mixer at a speed of 800 rpm and stirred for 40 minutes. The mass ratio of aluminum phenylphosphinate to ammonium polyphosphate was 2:1 to obtain a mixed powder. γ-Aminopropyltriethoxysilane was added to the mixed powder and stirred. The mixture was heated to 80°C, the speed was set to 500 rpm, and the stirring time was 60 minutes. The mixture was then vacuum dried at a temperature of 90°C, a vacuum degree of -0.09 MPa, and a drying time of 3 hours to obtain a high-temperature resistant filler.

[0043] Step 3: Dispersion of basic fillers

[0044] Vinyl-terminated polysiloxane and phenyl vinyl silicone oil were added to a planetary mixer at 100 rpm and stirred for 15 minutes to obtain a base gum matrix. Fumed silica and phenyltrimethoxysilane were added to the base gum matrix, and the mixture was heated to 80°C, vacuum set to -0.095 MPa, and stirred at 50 rpm for 4 hours. After stirring, the mixture was cooled to 50°C, and a high-temperature resistant filler and an Al2O3-CeO2-Sb2O3 composite were added at 80 rpm and stirred for 60 minutes to obtain a basic mixed filler.

[0045] Step 4: Add additives

[0046] The hydrogenated silicone oil and the platinum-alkyne complex are uniformly mixed to obtain a catalyst mother solution. An inhibitor and an antioxidant are added to the base mixed filler and stirred uniformly. The catalyst mother solution is added dropwise while stirring at a speed of 100 rpm to obtain a mixed material after the addition is complete. The inhibitor is diallyl maleate, and the antioxidant is triphenyl phosphite.

[0047] Step 5: Prepare silicone rubber

[0048] The mixed material is transferred to a vacuum degassing kettle, the vacuum degree is set to -0.095 MPa, and the degassing time is 45 minutes; after the degassing is completed, it is filtered through a 200-mesh stainless steel filter and packaged in an aluminum-plastic composite tube or a vacuum sealed barrel to obtain silicone rubber.

[0049] Example 2 A high-temperature resistant addition-type one-component silicone rubber for electronic packaging

[0050] A high-temperature resistant, addition-type, one-component silicone rubber for electronic packaging comprises the following raw materials, measured in parts by weight: 35 parts of vinyl-terminated polysiloxane, 25 parts of phenyl vinyl silicone oil, 30 parts of fumed silica, 8 parts of phenyltrimethoxysilane, 15 parts of high-temperature resistant filler, 5 parts of Al2O3-CeO2-Sb2O3 composite, 10 parts of hydrogen-containing silicone oil, 0.5 parts of platinum-alkyne complex, 0.15 parts of inhibitor, and 1 part of antioxidant.

[0051] A method for preparing a high-temperature resistant addition-type single-component silicone rubber for electronic packaging, comprising the following steps:

[0052] Step 1: Synthesis of Al2O3-CeO2-Sb2O3 composite

[0053] Aluminum nitrate, cerium nitrate and potassium antimony tartrate were dissolved in deionized water to prepare a mixed metal salt solution with a total metal ion concentration of 0.4 mol / L. The molar ratio of aluminum nitrate, cerium nitrate and potassium antimony tartrate was 5:3:2.

[0054] The mixed metal salt solution was heated to 70°C, stirred at a rate of 400 rpm, and ammonia water was added dropwise while stirring to adjust the pH value of the solution to 10; after the addition was completed, the stirring reaction was continued for 2 hours; after the reaction was completed, the solution was allowed to stand for aging at 70°C for 4 hours; after the aging was completed, the solution was washed alternately with deionized water and anhydrous ethanol 5 times; the washed precipitate was dried at 120°C for 16 hours to obtain a precursor; the precursor was calcined, the temperature was raised to 700°C, the heating rate was 10°C / min, the holding time was 4 hours, and the Al2O3-CeO2-Sb2O3 complex was obtained after cooling.

[0055] Step 2: Prepare high temperature resistant filler

[0056] Aluminum phenylphosphinate and ammonium polyphosphate were added to a high-speed mixer at a speed of 900 rpm and stirred for 40 minutes, with a mass ratio of aluminum phenylphosphinate to ammonium polyphosphate of 2:1, to obtain a mixed powder. γ-Aminopropyltriethoxysilane was added to the mixed powder and stirred, with the γ-Aminopropyltriethoxysilane accounting for 3% of the mixed powder mass. The mixture was heated to 80°C, the speed was set to 500 rpm, and the stirring time was 60 minutes. The mixture was then vacuum dried at a temperature of 100°C, a vacuum degree of -0.09 MPa, and a drying time of 2 hours to obtain a high-temperature resistant filler.

[0057] Step 3: Dispersion of basic fillers

[0058] Vinyl-terminated polysiloxane and phenyl vinyl silicone oil were added to a planetary mixer at 200 rpm and stirred for 15 minutes to obtain a base gum matrix. Fumed silica and phenyltrimethoxysilane were added to the base gum matrix, and the mixture was heated to 100°C, set to a vacuum of -0.095 MPa, and stirred at 100 rpm for 4 hours. After stirring, the mixture was cooled to 50°C, and a high-temperature resistant filler and an Al2O3-CeO2-Sb2O3 composite were added. The mixture was stirred at 150 rpm for 60 minutes to obtain a basic mixed filler.

[0059] Step 4: Add additives

[0060] The hydrogenated silicone oil and the platinum-alkyne complex are mixed uniformly to obtain a catalyst mother solution. An inhibitor and an antioxidant are added to the base mixed filler and stirred uniformly. The catalyst mother solution is added dropwise while stirring at a speed of 150 rpm to obtain a mixed material. The inhibitor is diallyl maleate, and the antioxidant is triphenyl phosphite.

[0061] Step 5: Prepare silicone rubber

[0062] The mixed material is transferred to a vacuum degassing kettle, the vacuum degree is set to -0.098 MPa, and the degassing time is 45 minutes; after the degassing is completed, it is filtered through a 200-mesh stainless steel filter and packaged in an aluminum-plastic composite tube or a vacuum sealed barrel to obtain silicone rubber.

[0063] Example 3 A high-temperature resistant addition-type one-component silicone rubber for electronic packaging

[0064] A high-temperature resistant, addition-type, one-component silicone rubber for electronic packaging comprises the following raw materials, measured in parts by weight: 40 parts of vinyl-terminated polysiloxane, 20 parts of phenyl vinyl silicone oil, 40 parts of fumed silica, 3 parts of phenyltrimethoxysilane, 10 parts of high-temperature resistant filler, 3 parts of Al2O3-CeO2-Sb2O3 composite, 12 parts of hydrogen-containing silicone oil, 0.5 parts of platinum-alkyne complex, 0.15 parts of inhibitor, and 1 part of antioxidant.

[0065] A method for preparing a high-temperature resistant addition-type single-component silicone rubber for electronic packaging, comprising the following steps:

[0066] Step 1: Synthesis of Al2O3-CeO2-Sb2O3 composite

[0067] Aluminum nitrate, cerium nitrate and potassium antimony tartrate were dissolved in deionized water to prepare a mixed metal salt solution with a total metal ion concentration of 0.5 mol / L. The molar ratio of aluminum nitrate, cerium nitrate and potassium antimony tartrate was 5:3:2.3.

[0068] The mixed metal salt solution was heated to 80°C, stirred at a rate of 300 rpm, and ammonia water was added dropwise while stirring to adjust the pH value of the solution to 10.5; after the addition was completed, the stirring reaction was continued for 2 hours; after the reaction was completed, the solution was allowed to stand for aging at 80°C for 2 hours; after the aging was completed, the solution was washed alternately with deionized water and anhydrous ethanol 5 times; the washed precipitate was dried at 120°C for 12 hours to obtain a precursor; the precursor was calcined, the temperature was raised to 700°C, the heating rate was 10°C / min, the holding time was 3 hours, and the Al2O3-CeO2-Sb2O3 complex was obtained after cooling.

[0069] Step 2: Prepare high temperature resistant filler

[0070] Aluminum phenylphosphinate and ammonium polyphosphate were added to a high-speed mixer at a speed of 900 rpm and stirred for 30 minutes, with a mass ratio of aluminum phenylphosphinate to ammonium polyphosphate of 3:1, to obtain a mixed powder. γ-Aminopropyltriethoxysilane was added to the mixed powder and stirred, with the γ-Aminopropyltriethoxysilane accounting for 4% of the mixed powder mass. The mixture was heated to 90°C, the speed was set to 600 rpm, and the stirring time was 40 minutes. The mixture was then vacuum dried at a temperature of 100°C, a vacuum degree of -0.095 MPa, and a drying time of 2 hours to obtain a high-temperature resistant filler.

[0071] Step 3: Dispersion of basic fillers

[0072] Vinyl-terminated polysiloxane and phenyl vinyl silicone oil were added to a planetary mixer at 200 rpm and stirred for 10 minutes to obtain a base gum matrix. Fumed silica and phenyltrimethoxysilane were added to the base gum matrix, and the mixture was heated to 120°C, vacuumed to -0.09 MPa, and stirred at 100 rpm for 2 hours. After stirring, the mixture was cooled to 60°C, and a high-temperature resistant filler and an Al2O3-CeO2-Sb2O3 composite were added at 150 rpm and stirred for 30 minutes to obtain a basic mixed filler.

[0073] Step 4: Add additives

[0074] The hydrogenated silicone oil and the platinum-alkyne complex are mixed uniformly to obtain a catalyst mother solution. An inhibitor and an antioxidant are added to the base mixed filler and stirred uniformly. The catalyst mother solution is added dropwise while stirring at a speed of 150 rpm to obtain a mixed material. The inhibitor is diallyl maleate, and the antioxidant is triphenyl phosphite.

[0075] Step 5: Prepare silicone rubber

[0076] The mixed material is transferred to a vacuum degassing kettle, the vacuum degree is set to -0.098 MPa, and the degassing time is 30 minutes; after the degassing is completed, it is filtered through a 200-mesh stainless steel filter and packaged in an aluminum-plastic composite tube or a vacuum sealed barrel to obtain silicone rubber.

[0077] Comparative Example 1

[0078] A silicone rubber for electronic packaging, comprising the following raw materials, measured in parts by weight: 35 parts of vinyl-terminated polysiloxane, 25 parts of phenyl vinyl silicone oil, 30 parts of fumed silica, 8 parts of phenyltrimethoxysilane, 5 parts of Al2O3-CeO2-Sb2O3 complex, 10 parts of hydrogenated silicone oil, 0.5 parts of platinum-alkyne complex, 0.15 parts of inhibitor, and 1 part of antioxidant.

[0079] A method for preparing a high-temperature resistant addition-type single-component silicone rubber for electronic packaging, comprising the following steps:

[0080] Step 1: Synthesis of Al2O3-CeO2-Sb2O3 composite

[0081] This step is the same as the step of “Synthesis of Al2O3-CeO2-Sb2O3 composite” in Example 2.

[0082] Step 2: Dispersion of basic fillers

[0083] Vinyl-terminated polysiloxane and phenyl vinyl silicone oil were added to a planetary mixer at 200 rpm and stirred for 15 minutes to obtain a base gum matrix. Fumed silica and phenyltrimethoxysilane were added to the base gum matrix, and the mixture was heated to 100°C, set to a vacuum of -0.095 MPa, and stirred at 100 rpm for 4 hours. After stirring, the mixture was cooled to 50°C, and an Al2O3-CeO2-Sb2O3 complex was added at 150 rpm and stirred for 60 minutes to obtain a basic mixed filler.

[0084] Step 3: Add additives

[0085] This step is the same as the "additive addition" step in Example 2.

[0086] Step 4: Prepare silicone rubber

[0087] This step is the same as the step of "preparing silicone rubber" in Example 2.

[0088] Comparative Example 2

[0089] A high-temperature resistant, addition-type, one-component silicone rubber for electronic packaging comprises the following raw materials, measured in parts by weight: 35 parts of vinyl-terminated polysiloxane, 25 parts of phenyl vinyl silicone oil, 30 parts of fumed silica, 8 parts of phenyltrimethoxysilane, 15 parts of high-temperature resistant filler, 10 parts of hydrogenated silicone oil, 0.5 parts of platinum-alkyne complex, 0.15 parts of inhibitor, and 1 part of antioxidant.

[0090] A method for preparing a high-temperature resistant addition-type single-component silicone rubber for electronic packaging, comprising the following steps:

[0091] Step 1: Prepare high temperature resistant filler

[0092] This step is the same as the step of “preparing high temperature resistant filler” in Example 2.

[0093] Step 2: Dispersion of basic fillers

[0094] Vinyl-terminated polysiloxane and phenyl vinyl silicone oil were added to a planetary mixer at 200 rpm and stirred for 15 minutes to obtain a gum base. Fumed silica and phenyltrimethoxysilane were added to the gum base, and the mixture was heated to 100°C, set to a vacuum of -0.095 MPa, and stirred at 100 rpm for 4 hours. After stirring, the mixture was cooled to 50°C, and a high-temperature resistant filler was added at 150 rpm and stirred for 60 minutes to obtain a basic mixed filler.

[0095] Step 3: Add additives

[0096] This step is the same as the "additive addition" step in Example 2.

[0097] Step 4: Prepare silicone rubber

[0098] This step is the same as the step of "preparing silicone rubber" in Example 2.

[0099] Example 4 Performance Test

[0100] (I) The silicone rubbers prepared in Examples 1-3 and Comparative Examples 1-2 were tested for Shore hardness according to the test method provided in GB / T 531.1-2008, and for tensile strength and elongation at break according to the test method provided in GB / T 528-2009. The specific test results are shown in Table 1.

[0101] Table 1

[0102]

[0103] As can be seen from the test results in Table 1, the Shore hardness of the silicone rubber prepared in Examples 1-3 is 69-74 Shore A, the tensile strength is 4.68-4.79 MPa, and the elongation at break is 382-395%, which are significantly improved compared with the comparative example, proving that the silicone rubber prepared in the present invention has excellent mechanical strength.

[0104] (2) The silicone rubbers prepared in Examples 1-3 and Comparative Examples 1-2 were subjected to a high-temperature treatment at 300°C for 24 hours. Shore hardness and tensile strength were then measured according to the test methods specified in GB / T 531.1-2008 and GB / T 528-2009. The specific test results are shown in Table 2.

[0105] Table 2

[0106]

[0107] As can be seen from the test results in Table 2, the silicone rubber prepared in Examples 1-3 has a Shore hardness of 73-79 Shore A after high-temperature treatment. As the temperature increases, the hardness increases slightly; the tensile strength still reaches 4.32-4.41 MPa. Compared with the comparative example, the tensile strength retention rate is higher, which proves that the silicone rubber prepared in the present invention has excellent high-temperature resistance.

[0108] (III) Test specimens were prepared from the silicone rubber prepared in Examples 1-3 and Comparative Examples 1-2 according to the test method specified in GB / T 1410-2006. The specimens were placed in a 250°C oven for 30 minutes, and a DC voltage of 100 V was applied. The volume resistivity was measured. The specific test results are shown in Table 3.

[0109] Table 3

[0110]

[0111] From the test results in Table 3, it can be seen that the high-temperature volume resistivity of the silicone rubber prepared in Examples 1-3 reaches 1.9×10 14 -3.1×10 14 Ω·cm, which proves that the silicone rubber prepared by the present invention has excellent high temperature resistance and electrical insulation stability.

[0112] The specific parameters of the raw materials used in the present invention are as follows:

[0113] The viscosity of the vinyl terminated polysiloxane is 5000-10000 cSt, and the vinyl content is 0.15-0.35%.

[0114] The phenyl content of the phenyl vinyl silicone oil is 15-25%, and the vinyl content is 0.2-0.5%.

[0115] The particle size of the fumed silica is 7-16 nm.

[0116] The purity of the phenyltrimethoxysilane is ≥98%.

[0117] The Si—H content of the hydrogen-containing silicone oil is 0.8-1.6%.

[0118] The platinum-alkyne complex is Wacker CATALYST OL catalyst.

[0119] Obviously, there are many specific implementation methods that can be changed under the concept of the present invention. Here, it should be stated that any changes made under the inventive concept of the present invention will fall within the scope of protection of the present invention.

Claims

1. A high-temperature resistant, addition-type, one-component silicone rubber for electronic packaging, characterized by: The silicone rubber raw materials include vinyl-terminated polysiloxane, phenyl vinyl silicone oil, fumed silica, phenyltrimethoxysilane, high-temperature resistant filler, Al2O3-CeO2-Sb2O3 compound, hydrogen-containing silicone oil, platinum-alkyne complex, inhibitor, and antioxidant; The high-temperature resistant filler is prepared by the following method: adding aluminum phenylphosphinate and ammonium polyphosphate into a high-speed mixer and stirring to obtain a mixed powder; adding γ-aminopropyltriethoxysilane into the mixed powder and stirring for 40-60 minutes; and then vacuum drying to obtain the high-temperature resistant filler; The Al2O3-CeO2-Sb2O3 composite is prepared by the following method: aluminum nitrate, cerium nitrate, and potassium antimony tartrate are dissolved in deionized water to prepare a mixed metal salt solution, the mixed metal salt solution is heated to 60-80°C, the pH value of the solution is adjusted, and the solution is stirred for reaction for 1-2 hours; after the reaction, the solution is allowed to stand for aging at a temperature of 60-80°C and an aging time of 2-4 hours; after the aging, the solution is washed, dried, and calcined to obtain the Al2O3-CeO2-Sb2O3 composite.

2. The high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 1, characterized in that: The weight ratio of the raw materials is: 30-40 parts of vinyl-terminated polysiloxane, 20-30 parts of phenyl vinyl silicone oil, 25-40 parts of fumed silica, 3-8 parts of phenyltrimethoxysilane, 10-15 parts of high-temperature resistant filler, 3-5 parts of Al2O3-CeO2-Sb2O3 complex, 8-12 parts of hydrogen-containing silicone oil, 0.3-0.5 parts of platinum-alkyne complex, 0.1-0.15 parts of inhibitor, and 0.5-1 parts of antioxidant.

3. The high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 1, characterized in that: The molar ratio of the aluminum nitrate, cerium nitrate and potassium antimony tartrate is 5:(2.8-3):(2-2.3).

4. The high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 1, characterized in that: The mass ratio of the phenyl phosphinate aluminum to the ammonium polyphosphate is (2-3):1; the gamma-aminopropyltriethoxysilane accounts for 3-4% of the mass of the mixed powder.

5. The method for preparing a high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to any one of claims 1 to 4, characterized in that: The method includes the steps of synthesizing Al2O3-CeO2-Sb2O3 compound, preparing high temperature resistant filler, dispersing basic filler, adding auxiliary agent and preparing silicone rubber.

6. The method for preparing a high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 5, characterized in that: The basic filler dispersion comprises the following steps: adding vinyl-terminated polysiloxane and phenyl vinyl silicone oil into a planetary mixer and stirring for 10-15 minutes to obtain a base gum matrix; adding fumed silica and phenyl trimethoxysilane into the base gum matrix, heating the mixture to 80-120° C. and performing vacuum stirring; after the stirring is completed, cooling the mixture to 50-60° C., adding a high-temperature resistant filler and an Al2O3-CeO2-Sb2O3 complex, and stirring the mixture for 30-60 minutes to obtain a basic mixed filler.

7. The method for preparing a high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 6, characterized in that: The auxiliary agent addition comprises the following steps: mixing hydrogen-containing silicone oil and platinum-alkyne complex uniformly to obtain a catalyst mother solution; adding an inhibitor and an antioxidant to a basic mixed filler and stirring uniformly; adding the catalyst mother solution dropwise while stirring at a rotation speed of 100-150 rpm to obtain a mixed material after the addition is completed.

8. The method for preparing a high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 7, characterized in that: The method for preparing the silicone rubber comprises: vacuum degassing the mixed material, filtering the mixed material through a 200-mesh stainless steel filter screen after the degassing is completed, and packaging the mixed material in an aluminum-plastic composite tube or a vacuum sealed barrel to obtain the silicone rubber.

9. The method for preparing a high-temperature resistant addition-type one-component silicone rubber for electronic packaging according to claim 8, characterized in that: The vacuum degassing: the mixed material is transferred to a vacuum degassing kettle, the vacuum degree is set to -0.095MPa to -0.098MPa, and the degassing time is 30-45min.

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