Large Area Mesoporous Silica Thin Film with Perpendicular Nanochannels on a Substrate and Process of forming the same

Patent metadata

Field	Value
Publication number	US-2016282274-A1
Application number	US-201615059526-A
Country	US
Kind code	A1
Filing date	Mar 3, 2016
Priority date	Mar 23, 2015
Publication date	Sep 29, 2016
Grant date	—

Abstract

The present invention disclosed a mesoporous silica thin film with perpendicular nanochannels on a substrate, a process of forming the same and the application in surface-enhanced Raman spectroscopy. Furthermore, a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels and the process of forming the same is also present in the invention.

First claim

What is claimed is:

1 . A process of forming a mesoporous silica thin film with perpendicular nanochannels on a substrate, said process comprising:
(1). Providing a substrate; (2). Providing an ammonia solution which comprises a tertiary alkyl ammonium halide, alcohol, and an additive; (3). Immersing the substrate into the ammonia solution; (4). Introducing a silica precursor into the ammonia solution; and (5). Performing a heating step to form a mesoporous silica thin film with perpendicular nanochannels on the substrate, wherein the mesoporous silica thin film with perpendicular nanochannels having a film thickness between 20 nm and 100 nm, a pore diameter of the perpendicular nanochannels which is between 2 nm and 10 nm and a area more than 500 um×500 um in SEM analysis.

2 . The process according to claim 1 , said process further comprising a washing step, wherein the washing step is to stabilize the mesoporous silica thin film with perpendicular nanochannels on the substrate by using a buffer which comprises HF/NH 4 F.

3 . The process according to claim 1 , wherein the additive is selected from one of the group consisting of decane, ethyl acetate, petroleum ether, hexadecane, pentyl ether and the combination thereof and a concentration of the additive is between 0.001M and 0.3M.

4 . The process according to claim 1 , wherein the substrate comprises a silicon wafer, a polystyrene-coated silicon wafer, a ceramic, aluminum oxide, tert-butyltrichlorosilane-functionalized Si wafer, indium tin oxide (ITO), fluorine doped tin oxide (FTO), sapphire surfaces and a conducting glass.

5 . The process according to claim 1 , wherein the ammonia concentration of the ammonia solution is between 0.05 M and 1.5M.

6 . The process according to claim 1 , wherein the tertiary alkyl ammonium halide is cetyltrimethylammonium bromide.

7 . The process according to claim 1 , wherein the silica precursor comprises tetraethyl orthosilicate, fumed silica, and zeolite beta seeds.

8 . A mesoporous silica thin film with perpendicular nanochannels, said mesoporous silica thin film with perpendicular nanochannels having a film thickness between 20 nm and 100 nm, a pore diameter of the perpendicular nanochannels which is between 2 nm and 10 nm, and a 2D hexagonal packing diffraction pattern with the space group of p6mm in FFT-SEM analysis.

9 . The mesoporous silica thin film with perpendicular nanochannels according to claim 8 , said mesoporous silica thin film with perpendicular nanochannels having a out-of-plane (q z ) and in-plane (q y ) converted line diagram as shown in FIG. 9( b ) , wherein the out-of-plane (q z ) and in-plane (q y ) converted line diagram is derived from GISAXS image patterns.

10 . The mesoporous silica thin film with perpendicular nanochannels according to claim 8 , wherein the pore diameter of the perpendicular nanochannels is between 5 nm and 10 nm.

11 . The mesoporous silica thin film with perpendicular nanochannels according to claim 8 , being on part or all of surfaces of at least one selected from a membrane, a semiconductor, a catalyst, a sensor and an energy conversion device.

12 . A process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels, said process comprising
(1). Providing a mesoporous silica material with perpendicular nanochannels selected from one of the groups consisting of a mesoporous silica thin film and a mesoporous silica nanoparticle; (2). Performing a reaction to have the mesoporous silica material with perpendicular nanochannels react with an amino functional group introducing agent to give an amino functionalized mesoporous silica material with perpendicular nanochannels; (3). Immersing the amino functionalized mesoporous silica material with perpendicular nanochannels into a gold precursor solution to coat gold ions onto the amino functionalized mesoporous silica material with perpendicular nanochannels; and (4). Performing a reduction reaction to reduce the gold ions to gold nanoparticles, so as to form the gold nanoparticle array on the mesoporous silica material with perpendicular nanochannels, wherein the gold nanoparticles directly anchored on the perpendicular nanochannels, wherein a pore diameter of the perpendicular nanochannels is between 2 nm and 10 nm.

13 . The process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels according to claim 12 , wherein the gold nanoparticle having a diameter between 3 nm and 30 nm.

14 . The process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels according to claim 12 , wherein gap distances between the gold nanoparticles on the mesoporous silica material with perpendicular nanochannels is less than 3 nm.

15 . The process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels according to claim 12 , wherein the amino functional group introducing agent comprises (3-aminopropyl)trimethoxysilane.

16 . The process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels according to claim 12 , wherein the gold precursor solution comprises 0.01 mM-5 mM of HAuCl 4 .

17 . The process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels according to claim 12 , wherein the reduction reaction is performed with 0.1 mM-10 mM of sodium borohydride.

18 . The process of making a gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels according to claim 12 , wherein the gold nanoparticle array on a mesoporous silica material with perpendicular nanochannels is applied in label-free chemical sensing and biosensing.

Assignees

• Univ Nat Taiwan

Inventors

• Mou Chung-Yuan
• Kao Kun-Che
• Chen Tzu-Ying
• Wang Yi-Wen
• Liu Yi-Hsin

Classifications

• C01P2002/80

  defined by measured data other than those specified in group C01P2002/70 · CPC title

• C01P2006/16

  Pore diameter · CPC title

• C01B33/124

  Preparation of adsorbing porous silica not in gel form and not finely divided, i.e. silicon skeletons, by acidic treatment of siliceous materials · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title