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Preparation method of a double-layer composite self-assembled lubricating film

A self-assembly, lubricating film technology, applied in the directions of lubricating compositions, coatings, devices for coating liquids on surfaces, etc., can solve the problems of limited practical application, cannot be maintained for a long time, low bearing capacity, etc., and is easy to implement and popularize. , the effect of low energy consumption and cost, low friction coefficient

Inactive Publication Date: 2018-06-15
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although self-assembled monolayers can effectively reduce the friction coefficient of silicon surfaces, most of the organic monolayers prepared so far still have the disadvantages of low load-carrying capacity and poor wear resistance, and cannot be maintained for a long time under repeated sliding conditions.
When some molecules are removed from the surface due to mechanical friction, the film will fail, which will greatly limit its practical application in the field of MEMS

Method used

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  • Preparation method of a double-layer composite self-assembled lubricating film
  • Preparation method of a double-layer composite self-assembled lubricating film

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preparation example Construction

[0025] The preparation method of the double-layer self-assembled lubricating film of the present invention uses 1,2-bis(triethoxysilyl)ethane and a low surface energy silane coupling agent as raw materials, and is prepared by conventional self-assembly technology with stable , uniform and orderly microstructured double-layer film surface; the preparation method comprises the following steps:

[0026] (1) After the monocrystalline silicon wafer is cut into regular sizes, it is sequentially washed with organic solvent and water ultrasonically;

[0027] (2) At a temperature of 90°C, 98% concentrated H with a volume ratio of 7:3 is used. 2 SO 4 and 30%H 2 o 2 Composed of Piranha solution, oxidize the surface of single crystal silicon for 30 minutes to make the surface hydroxylated, and finally fully wash with deionized water and dry carefully;

[0028] (3) Fully hydrolyze 1,2-bis(triethoxysilyl)ethane in methanol / water mixed solvent; The fully hydrolyzed concentration in the ...

Embodiment 1

[0031] Example 1: Cut the monocrystalline silicon wafer into small pieces of 1cm × 1cm size, then immerse in acetone, chloroform, and isopropanol in order to ultrasonically clean for 10 minutes, then fully clean with deionized water, take it out and dry it carefully; The final monocrystalline silicon wafer is immersed in a 90°C Piranha solution for oxidation treatment to make the surface hydroxylated. The Piranha solution is 98% concentrated H 2 SO 4 and 30%H 2 o 2 The mixed solution, the volume ratio is 7:3; the monocrystalline silicon wafer is taken out after 30min treatment, fully cleaned with deionized water and carefully blown dry. Take a certain amount of 1,2-bis(triethoxysilyl)ethane and add it to methanol / water mixed solvent (16 / 1 by volume), control the pH of the system to 4.5, and make it hydrolyze at room temperature for 2 day; immerse the oxidized monocrystalline silicon wafer in the hydrolyzed solution of 1,2-bis(triethoxysilyl)ethane for 2 minutes; take out t...

Embodiment 2

[0033]Embodiment 2: After cutting, cleaning and oxidizing the monocrystalline silicon wafer according to the steps of Embodiment 1, fully clean it with deionized water and dry it carefully; take a certain amount of 1,2-bis(triethoxy silicon Base) ethane is added in the methanol / water mixed solvent, the volume ratio of methanol / water mixed solvent is 9 / 1, the pH of the control system is 5.0, and it is hydrolyzed at normal temperature for 3 days; The slice was immersed in the hydrolyzed solution of 1,2-bis(triethoxysilyl)ethane for 1min; the sample was taken out to be cleaned and dried, and then immersed in 1mM 3-aminopropyltriethoxysilane Self-assembled in a toluene solution for 0.5 h under a nitrogen-protected environment; the silicon wafer was taken out, washed and dried to obtain a self-assembled lubricating film with a double-layer structure.

[0034] The oxidized single crystal silicon wafer was directly immersed in a toluene solution of 1mM 3-aminopropyltriethoxysilane, s...

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Abstract

The invention provides a preparation method of a double-layer self-assembly lubricating film and relates to a preparation method of a novel double-layer self-assembly film formed by 1,2-Bis(triethoxysilyl)ethane and a low-surface-energy silane coupling agent. The method comprises the steps that single crystal silicon wafers are cut and cleaned and then are subjected to oxidation treatment; and the processed silicon wafers are immersed into 1,2-Bis(triethoxysilyl)ethane hydrolysate, and a first-layer film is prepared; and the obtained film is immersed into a low-surface-energy silane coupling agent solution again after being cleaned and dried, and deposition of a second-layer film is carried out through active groups on the surface of the first-layer film. Instruments and equipment involved in the preparation method are simple, operation is easy during the process, and the obtained double-layer films are of a stable and ordered structure. Compared with a single-layer film of the low-surface-energy silane coupling agent, the double-layer films can maintain a low friction coefficient, and the adhesion resistance and abrasion resistance of the double-layer self-assembly lubricating film can be effectively improved. The double-layer film is expected to become an effective means of solving the problems of lubrication and protection of the surfaces of devices in micro electro-mechanical systems.

Description

technical field [0001] The invention relates to a method for preparing a solid lubricating material, in particular to a method for preparing 1,2-bis(triethoxysilyl)ethane / low surface energy silane coupling agent double-layer composite self-assembly on the surface of single crystal silicon Preparation method of lubricating film. Background technique [0002] Silicon is the most important building block material in microelectronics today. In microelectromechanical systems (MEMS), which have emerged in recent decades, most of the components are formed on the surface of silicon. Silicon material has the characteristics of high hardness, low cost, small surface roughness, and can realize integrated manufacturing and device miniaturization. However, silicon materials without surface treatment are highly brittle, and surface cracks can expand rapidly under low tensile stress, and are prone to delamination wear and brittle fracture, which is difficult to meet the use requirements....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B05D5/08B05D7/00C10M141/12C10M139/04C10N30/06
CPCB05D5/08B05D7/51B05D7/544B05D2203/30B05D2451/00C10M139/04C10M141/12C10M2201/105C10M2227/04C10N2030/06B05D2401/20
Inventor 王鹏滕淑华
Owner CHINA UNIV OF MINING & TECH
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