Preparation method of extra-thin silicon oil membrane
A silicone oil film and silicone oil technology, applied in the field of preparation of silicone oil ultra-thin films, can solve the problems of harsh film-forming substances and film-forming conditions, weak interaction, high price, etc. The effect of good solvent resistance
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Embodiment 1
[0043] Preparation of crosslinked vinyl silicone oil film:
[0044] 1. Pretreatment of the monocrystalline silicon substrate: soak the monocrystalline silicon wafer polished on one side with a certain volume of a mixture of 30% hydrogen peroxide and 98% concentrated sulfuric acid at 90°C for 2 hours, and then rinse with deionized water Ultrasonic cleaning, drying with high-purity nitrogen;
[0045] 2. Immerse the pretreated monocrystalline silicon substrate into 0.6% (w / w) vinyl-terminated silicone oil with a molecular weight of 600,000 (X=-CH=CH 2 ; 1 = R 2 = R 3 = R 4 =-CH 3) in n-pentane solution, the solution also contains 1% (by weight with vinyl silicone oil) of benzoyl peroxide as an initiator. The solvent was evaporated slowly under reduced pressure until the liquid level of the solution was lower than the surface of the sample.
[0046] 3. After taking out the sample, heat treatment at 300°C for 24 hours in a nitrogen atmosphere to obtain a cross-linked and end...
Embodiment 2
[0052] Preparation process of cross-linked and end-grafted vinyl silicone oil film:
[0053] 1. Single-sided polished single-crystal silicon wafers were first ultrasonically washed in acetone solvent for 5 minutes, dried with high-purity nitrogen, and placed in newly prepared concentrated H with a volume ratio of 70:30. 2 SO 4 and 30%H 2 o 2 , keep at 90°C for at least 2 hours. After taking out the single crystal silicon wafer, it was ultrasonically washed three times with 50 ml of twice-distilled water, and dried with high-purity nitrogen to obtain a hydroxylated silicon wafer.
[0054] 2. Immediately immerse the silicon wafer in 0.2% (v / v) vinyltriethoxysilane solution after hydroxylation, and react at 70°C for 24 hours to obtain a single crystal silicon wafer modified with a vinyl-terminated self-assembled film. Ultrasonic washing with methane to remove unbonded vinyltriethoxysilane, and drying with high-purity nitrogen;
[0055] 3. Immerse the pretreated monocrystalli...
Embodiment 3
[0061] The preparation process of cross-linked and end-grafted hydroxyl silicone oil film is as follows:
[0062] 1. The preparation of the silicon wafer of hydroxylation is with embodiment 2 step 1;
[0063] 2. Immediately immerse the hydroxylated silicon substrate in a concentration of 0.4% (w / w) silicone oil with a molecular weight of 600,000 terminal hydroxyl groups (X=OH, R 1 = R 2 = R 3 = R 4 =-CH 3 ) in the n-pentane solution, other operating steps are with embodiment 1 step 2;
[0064] 3. heat treatment is with embodiment 1 step 3;
[0065] 4. Washing is the same as Step 4 of Example 1.
[0066] When the film prepared by this method is under 0.5N load and 90mm / min reciprocating speed, the Si 3 N 4 The friction coefficient of the ceramic ball is stable at 0.03-0.05, and the service life exceeds 5000 times (the friction coefficient at this time is still maintained at 0.05).
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