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Sheet-like tungsten trioxide photoelectrode and preparation method thereof

A photoelectrode and sheet-like technology, applied in the direction of electrodes, electrolytic processes, electrolytic components, etc., can solve the problems of poor bonding between the film and the substrate, high film compactness, and small specific surface area, and achieve controllable morphology and low production costs. Low, repeatable effect

Inactive Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing a tungsten trioxide porous film photoelectrode composed of a sheet array, which uses a combination of magnetron reactive sputtering and chemical etching, and solves the problem of sputtering to prepare thin films. The shortcomings of high density and small specific surface area and the problem of poor bonding between the film and the substrate prepared by chemical methods

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  • Sheet-like tungsten trioxide photoelectrode and preparation method thereof
  • Sheet-like tungsten trioxide photoelectrode and preparation method thereof
  • Sheet-like tungsten trioxide photoelectrode and preparation method thereof

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Embodiment 1

[0038] (1) Place a clean FTO conductive glass substrate 170mm above the sputtering target, and control the background vacuum to be less than 7×10 -7 torr, the substrate is not heated. Using DC reactive sputtering, adjust the sputtering process parameters: working pressure is 10mtorr, reaction gas O 2 The air pressure is 2mtorr, sputtering 50nm tungsten oxide first, and then co-sputtering, the Al target sputtering power is 60W, the W target sputtering power is 150W, the pre-sputtering is 15 minutes, and the sputtering time is 1 hour, and the thickness is about 800nm ​​Al-W-O dense film, the morphology is as follows figure 1 shown.

[0039] (2) The obtained mixed-phase amorphous oxide film was exposed to 1M H 2 SO 4 Soaked in the solution for 10 hours, the appearance is as figure 2 shown. The flaky tungsten oxide thin film prepared in this embodiment is evenly distributed, with a thickness of about 30 nm and a size of 220 nm. And from image 3 It can be seen from the XR...

Embodiment 2

[0043] (1) Place a clean FTO conductive glass substrate 170mm above the sputtering target, and control the background vacuum to be less than 7×10 -7 torr, the substrate is not heated. Using DC reactive sputtering, adjust the sputtering process parameters: working pressure is 7.5mtorr, reaction gas O 2 The pressure is 2mtorr, first sputtering 30nm thick tungsten oxide, and then co-sputtering, the Cu target sputtering power is 80W, the W target sputtering power is 200W, the pre-sputtering is 15 minutes, and the sputtering time is 1 hour, and the thickness is about Cu-W-O dense film of 1000nm.

[0044] (2) The obtained mixed-phase amorphous oxide film was exposed to 1M H 2 SO 4 Etched in solution for 8 hours, Figure 8 It is a scanning electron microscope picture, the sheet thickness is about 45nm, and the size is about 670nm.

Embodiment 3

[0046] (1) Place a clean FTO conductive glass substrate above the sputtering target, and control the background vacuum to be less than 7×10 -7 torr, the substrate is not heated. Using DC reactive sputtering, adjust the sputtering process parameters: working pressure is 10mtorr, reaction gas O 2 The air pressure is 2mtorr, first sputtering 50nm thick tungsten oxide, and then co-sputtering, the distance between the W target and the substrate is kept at 150mm, the distance between the Zn target and the substrate is 170mm, the sputtering power of the Zn target is 60W, and the sputtering power of the W target is 150W , pre-sputtering for 15 minutes, and sputtering time for 1 hour, a dense Zn-W-O thin film with a thickness of about 710 nm was obtained.

[0047] (2) The obtained mixed-phase amorphous oxide film was exposed to 1M H 2 SO 4 Etched in solution for 4 hours, Figure 9 It is a scanning electron microscope picture, the sheet thickness is about 45nm, and the size is about...

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Abstract

The present invention relates to porous WO3 sheet-like array film preparation, which comprises: firstly utilizing a direct current reaction magnetron sputtering method, adopting Ar gas as sputtering gas, adopting O2 gas as reaction gas, and adopting double metal target co-sputtering to carry out sputtering so as to obtain an amorphous oxide film, wherein the one target is a tungsten target, and the other target is one selected from aluminum, copper and zinc; and immersing the prepared amorphous metal oxide film in a strong acid solution to selectively etch, obtaining a sheet-like porous structure on the substrate, and annealing at a temperature of 450-550 DEG C in air so as to form monoclinic crystal phase WO3, wherein the morphology is well preserved. According to the present invention, the porous tungsten oxide electrode obtained through the method has characteristics of specific surface increase, substantial light absorption property improving, and good adhesion between the material and the substrate; and the preparation method of the present invention has the following advantages that: the mass production can be achieved, the preparation process is simple, the saturated photocurrent of the prepared WO3 electrode is increased by 3 times compared with the saturated photocurrent of the unetched dense WO3 electrode, and the obtained sheet-like tungsten trioxide photoelectrode can further be used for dye-sensitized solar cells, electrochromic devices and the like.

Description

technical field [0001] The invention relates to a tungsten trioxide porous film photoelectrode composed of sheet arrays and a preparation method thereof. Background technique [0002] The environmental crisis and energy crisis are becoming more and more serious, which seriously restrict the development of social economy. Since Fujishima and Honda discovered the use of TiO in 1971 2 As an electrode, in the case of light, it can promote the photolysis of water, and the use of semiconductor catalysts for photocatalytic water splitting and photoelectrochemical splitting of water for hydrogen production has attracted more and more attention. [0003] In the early studies of photoelectrochemical water splitting, bulk thin films or single crystal materials were used as photoelectrodes. In recent years, nano-textured thin film electrodes have become the focus of research due to their large surface area and porous properties. WO 3 Due to its stability under acidic conditions and ...

Claims

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Application Information

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IPC IPC(8): C23C14/35C23C14/08C23C14/58C25B11/04
Inventor 李灿王楠施晶莹郑霄家
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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