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Preparation method of mesoporous silicon oxide thin film material

A technology of mesoporous silicon oxide and thin film materials, which is applied in the preparation of low dielectric constant mesoporous silicon oxide thin film materials, in the field of divisional applications, and achieves the effects of good dielectric stability, uniform size distribution and good reproducibility

Inactive Publication Date: 2013-05-29
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pores of the film material prepared by the above sol-gel method can reach nanometer scale, but the following shortcomings are common: (1) The size of the pore size is difficult to control; (2) The pore size distribution of the material is wide and the uniformity is poor; (3) The pore size of the material is poor. poor reproducibility
However, silane monomers, water and acid are used in the process of preparing mesoporous films by the above-mentioned template method. This process is prone to hygroscopicity, so that the dielectric constant cannot be reduced to an ideal level or the stability of the dielectric constant is not good.
In addition, the quality of the film is unstable, and even drops sharply to the point where the dielectric constant cannot be measured

Method used

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  • Preparation method of mesoporous silicon oxide thin film material
  • Preparation method of mesoporous silicon oxide thin film material
  • Preparation method of mesoporous silicon oxide thin film material

Examples

Experimental program
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Embodiment 1

[0025] Example 1 A kind of preparation method of mesoporous silicon oxide film material

[0026] The P123 tri-block copolymer and PDMS-PEO di-block copolymer were added to the polymerized silica sol to form an oligomeric silicate precursor solution, and the silica sol was prepared by adding TEOS, water, hydrochloric acid (HCl) and ethanol ( ETOH) prepared by reflux at 60-80 ℃ for 80-100 min, the molar ratio of reactants is 1 TEOS: 0.008 P123: 0.017 PDMS-PEO: 72 H 2 O: 0.004 HCl: 33 ETOH; the precursor was aged at room temperature for 4-6 h. During the spin-coating process, the precursor solution was spin-coated onto the silicon wafer at a speed of 2500 rpm, and the spin-coating time was 25 s. The coating obtained after spin coating is baked at 100°C for 4-6 hours in an air atmosphere, and at 350°C for 1-2 hours to remove the template agent and obtain a silicon oxide film material with a mesoporous structure.

[0027] The triblock copolymer P123 in this example ( M w = ...

Embodiment 2

[0028] Example 2 Small-angle X-ray scattering (SAXS) measurement was carried out on the silicon oxide film material obtained in Example 1 by Nanostar U small-angle X-ray scattering instrument (CuKα) from Bruker, Germany. The tube pressure was 40 kV, the tube flow was 35 mA, and the recording time was 30 min. The resulting SAXS as figure 1 shown. Depend on figure 1 It can be seen that the SAXS spectra of As-made samples are at 0.46, 0.93 and 0.39 nm -1 3 clear diffraction peaks appear at , the three diffraction peaks q The value ratio is 1:2:3, which is assigned as the crystal plane diffraction peak of the layered mesoporous structure. After roasting under the protection of nitrogen at 350 °C, the clarity of the SAXS spectrum of the obtained sample decreased, and the diffraction peaks became wider, but two obvious diffraction peaks could also be observed, indicating that the layered structure after roasting at 350 °C still maintains the mesoporous structure. . The rel...

Embodiment 3

[0029] Example 3 The structure of the silicon oxide thin film material obtained in Example 1 was characterized by a Japanese JEOL JEM2011 high-resolution transmission electron microscope (TEM), and the accelerating voltage was 200 kV. The sample preparation process is as follows: the powdered silicon oxide thin film material obtained in Example 1 is dissolved in ethanol to form a slurry state, and the slurry is hanged on a copper net with a carbon film, and can be directly used for observation after drying. The TEM results of the resulting mesoporous silica coating are as follows figure 2 shown. Depend on figure 2 It can be seen that the layered structure remains after firing. It shows that the mesoporous silica thin layer with good skeleton stability can be successfully prepared by the co-template method. The average interlayer spacing is about 12.5 nm, which is comparable to figure 1 The SAXS spectrum characterization results are consistent.

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Abstract

The invention relates to a preparation method of a mesoporous silicon oxide thin film material. The method comprises the following steps of: adding P123 and PDMS-PEO (Polydimethylsiloxane-Poly Ethylene Oxide) into polymerized silicon oxide sol to form polysilicate precursor liquor; then, aging and spinning to a silicon wafer; and then, roasting to prepare the mesoporous silicon oxide thin film material with low dielectric constant. The polymerized silicon oxide sol is prepared by refluxing TEOS (Tetraethyl Orthosilicate), water, hydrochloric acid and ethanol which are mixed. The dielectric constant of the mesoporous silicon oxide thin film material prepared by the method provided by the invention is 1.9-2.8, and the dielectric stability is good. The shrinking percentage of the frame roasted is 8-16%, and the stability of the frame is excellent. Meanwhile, the material is good in high temperature thermal stability and hydrophobic stability. The mesoporous aperture of the thin film is smaller and is distributed uniformly. The specific surface area, the pore volume and the aperture respectively reach 600-1000m<2> / g, 0.35-0.65cm<3> / g and 4.5-6.2nm. Generally, the mesoporous silicon oxide thin film material prepared by the method provided by the invention is in particular suitable for the fields of coatings of low dielectric constant, film separation, sensors, optical materials and the like.

Description

[0001] The application of the present invention is a divisional application with the filing date of July 25, 2011 and the application number of 201110208143.8. technical field [0002] The invention relates to the technical field of new nanometer materials, in particular to a method for preparing a low dielectric constant mesoporous silicon oxide film material. Background technique [0003] At present, the low-dielectric constant film that has been studied more at home and abroad is porous silicon oxide film, and most of the preparation methods adopt the traditional sol-gel (sol-gel) method. For example, the U.S. Patent US 5194200 applied by Anderson Marc A et al. in 1993 adopts the sol-gel method to prepare silicon dioxide film, utilizes silicon alkoxide and ammonia water hydrolysis reaction to prepare sol, sol is dialyzed to a pH value of 8, and then acidified to The pH value is 3, and the sol is coated on the support. The disadvantage of this method is that the drying ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/50H10N30/857
Inventor 刘玉荣
Owner CHONGQING UNIV OF ARTS & SCI
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