# US 9,040,126 B2 · Fabrication of zeolite composite film

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- Number: US 9,040,126 B2
- Document ID: US9040126B2
- Status: Granted
- Kind: B2
- Application number: 13/970,619
- Filed: 2013-08-20
- Published: 2014-06-19
- Granted: 2015-05-26
- Earliest claimed: 2012-12-14
- Assignees: I-Shou University
- Applicants: I-Shou University
- Inventors: Chiung-Fang Lin
- Web page: https://patentgrep.com/patent/US9040126B2

## CPC

- C01B 39/205: {using at least one organic template directing agent; Hexagonal faujasite; Intergrowth products of cubic and hexagonal faujasite}
- C01B 37/02: Crystalline silica-polymorphs, e.g. silicalites {dealuminated aluminosilicate zeolites}
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A fabrication of a zeolite composite film includes mixing a composition of water, aluminum isopropoxide, TMAOH, and TEOS according to a set ratio, followed by stirring and heating to obtain a mixture; performing a centrifugation on the mixture to obtain an upper layer suspension; preparing a mesoporous particle suspension that includes a plurality of mesoporous particles, and each mesoporous particle includes a plurality of templating agents; vaporizing a mixture suspension formed from both the upper layer suspension and the mesoporous particle suspension to form a plurality of vaporized droplets; depositing the vaporized droplets on a heated substrate while removing the templating agents to form the zeolite composite film with a plurality of macroporous, mesoporous and microporous structures.

## Claims

### Claim 1

A fabrication of a zeolite composite film, comprising:
mixing a composition of water, aluminum isopropoxide, TMAOH, and TEOS according to a set ratio to form a first mixture, and hydrolyzing the first mixture by stirring in room temperature, then heating to obtain a second mixture;
taking an upper layer suspension obtained from a centrifugation of the second mixture, wherein the upper layer suspension comprises a plurality of zeolite crystals and a plurality of silicon colloids, and particle sizes of the zeolite crystals are less than 50 nm;
preparing a mesoporous particle suspension, wherein the mesoporous particle suspension comprises a plurality of mesoporous particles, and each mesoporous particle comprises a plurality of pores and a plurality of templating agents inside the pores;
applying a heat treatment to a substrate;
mixing the upper layer suspension and the mesoporous particle suspension to form a mixture suspension, and vaporizing the mixture suspension to form a plurality of vaporized droplets; and depositing the vaporized droplets on the heated substrate to remove the templating agents in the mesoporous particles and to form a zeolite composite film, wherein the zeolite composite film comprises a plurality of macroporous, mesoporous and microporous structures.

### Claim 2 (depends on 1)

The method of claim 1, wherein the set ratio of the first mixture is expressed by a mole ratio 0.15 Na2O:5.5 (TMA)2O:2.3 Al2O3:10SiO2:570 H2O.

### Claim 3 (depends on 1)

The method of claim 1, wherein a temperature of the heat treatment applied to the substrate is between 250° C. and 400° C.

### Claim 4 (depends on 1)

The method of claim 1, further comprising performing a pretreatment to the substrate before applying the heat treatment to the substrate.

### Claim 5 (depends on 1)

The method of claim 1, wherein the step of vaporizing the mixture suspension comprises using a dispersant to vaporize the mixture suspension.

### Claim 6 (depends on 1)

The method of claim 1, wherein the step of depositing the vaporized droplets on the substrate comprises using an air as a carrier gas to deposit the vaporized droplets on the substrate.

### Claim 7 (depends on 1)

The method of claim 1, wherein the step of depositing the vaporized droplets on the substrate comprises:
using an inert gas to bring the vaporized droplets into a plasma to conduct a plasma reaction in order to obtain a plurality of plasma treated zeolite crystals, silicon colloids, and mesoporous particles; and
depositing the plasma treated zeolite crystals, silicon colloids, and mesoporous particles on the substrate.

### Claim 8 (depends on 7)

The method of claim 7, wherein the inert gas is argon, and the flow rate of the argon is 60 cc to 200 cc per minute.

### Claim 9 (depends on 7)

The method of claim 7, wherein the plasma is generated by applying a voltage of 60 V to 90 V.

### Claim 10 (depends on 1)

The method of claim 1, wherein pore sizes of the macroporous structures are between 2 μm and 3 μm.

### Claim 11 (depends on 1)

The method of claim 1, wherein pore sizes of the mesoporous structures are between 1.5 nm and 3 nm.

### Claim 12 (depends on 1)

The method of claim 1, wherein pore sizes of the microporous structures are between 0.5 nm and 0.7 nm.

### Claim 13 (depends on 1)

The method of claim 1, wherein a dielectric constant of the zeolite composite film is less than 2.3.

### Claim 14 (depends on 1)

The method of claim 1, wherein the set volume ratio of the mesoporous particle suspension to the upper layer suspension is 3.8:1 in the mixture suspension.