Titanium dioxide film hydrogen sensor and preparation method thereof

A titanium dioxide and sensor technology, applied in the field of hydrogen sensors, can solve the problems of small resistance change of hydrogen sensors, low detection limit of hydrogen, hidden safety hazards, etc., and achieve the effects of excellent detection sensitivity and stability, reducing leakage current and increasing density.

Active Publication Date: 2015-04-29
HUBEI UNIV
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Problems solved by technology

[0004] Existing oxide gas sensors have the following problems: First, the operating temperature is high, and the best working condition is generally reached at 200-300°C. Studies have shown that high temperature will reduce the activation of hydrogen adsorption and analysis on the sensor surface It is beneficial to the improvement of detection sensitivity, but it also brings great safety hazards and increases energy consumption; second, the low detection limit of hydrogen needs to be improved. It has been recorded in relevant literature that a rutile phase TiO 2 The minimum detection limit of the film for hydrogen can re

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  • Titanium dioxide film hydrogen sensor and preparation method thereof
  • Titanium dioxide film hydrogen sensor and preparation method thereof
  • Titanium dioxide film hydrogen sensor and preparation method thereof

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preparation example Construction

[0020] The present invention provides a kind of preparation method of titanium dioxide thin film hydrogen sensor on the other hand, it comprises the following steps:

[0021] A. Provide FTO conductive glass layer 1, and pre-deposit a layer of [002]-oriented TiO on the surface of FTO conductive glass layer 1 by magnetron sputtering method 2 seed layer 2;

[0022] B. Using the hydrothermal method, in the TiO 2 TiO grows on the surface of seed layer 2 2 Nano-array film layer 3;

[0023] C. On TiO 2 Interdigital electrodes 4 are arranged on the surface of the nano-array film layer 3 .

[0024] Preferably, said step B also includes, for TiO 2 The nano-array film layer 3 is annealed in an inert atmosphere. Further preferably, the annealing temperature is 380-420° C., and the annealing time is 20-30 min. Specifically, Ar gas is used as the inert atmosphere. By annealing, TiO can be optimized 2 The interface performance of the nano-array film layer 3 reduces the interface sta...

Embodiment 1

[0038] Clean the FTO conductive glass layer 1: put the FTO conductive glass layer 1 into acetone, absolute ethanol, and deionized water successively for 20 minutes, and dry it for later use;

[0039] Install Ti 2 o 3 Target and substrate: Ti 2 o 3 The target is installed at the cathode target position of the magnetron sputtering system, and the distance between the target and the substrate is adjusted to 60mm. The FTO conductive glass layer 1 is placed at the substrate position and water-cooled;

[0040] Clean Ti2 o 3 Target material: vacuum to 10 -4 In the Pa order of magnitude, 50sccm argon and 1sccm oxygen are introduced into the magnetron sputtering chamber, the deposition pressure of the chamber is controlled to be 1Pa, and the radio frequency Ti is adjusted. 2 o 3 The power of the target is 120W, and the target is glow-cleaned for 10 minutes;

[0041] Sputtering deposition and annealing: After cleaning, adjust the RF Ti 2 o 3 The power of the target is 120W, and...

Embodiment 2

[0047] Embodiment 2 of the present invention is basically the same as Embodiment 1, the difference is: through hydrothermal synthesis of TiO 2 After the nanoarray film layer 3, the TiO 2 The nano-array thin film layer 3 was annealed at 400° C. for 20 min under the protection of Ar atmosphere.

[0048] TiO at 25±5°C 2 Gas sensor for detection. The gas sensitivity test results show that the response time and recovery time of the sensor are both short. In the range of hydrogen concentration of 1-1000ppm, the response time of the sensor is about 10s, and the average recovery time of the sensor is 134s in the range of hydrogen concentration of 1-80ppm. , the hydrogen concentration is 100-1000ppm, and the sensor recovery time is faster, 36-66s. TiO 2 It exhibits very good gas-sensing characteristics at low concentrations. When the hydrogen concentration is 1ppm, the resistance value can drop by 4%. After the resistance value drops to the minimum, it can quickly stabilize at this...

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Abstract

The invention provides a titanium dioxide film hydrogen sensor and a preparation method thereof. The predeposited TiO2 seed crystal layer can isolate the FTO (fluorine-doped tin oxide) conducting layer and hydrothermal growth TiO2 layer, lower the drain current passing through the FTO conducting glass layer and enhance the detection sensitivity of the titanium dioxide film hydrogen sensor; the predeposited TiO2 seed crystal layer can be used as a buffer layer and seed crystal layer, provides a higher-density seed crystal layer for the next hydrothermal synthesis step of the TiO2 nano array film, and effectively increases the density of the film TiO2 nanorod array; and magnetron sputtering and hydrothermal synthesis are combined to enhance the grain orientation performance of the TiO2 nano array film, so that the finally prepared titanium dioxide film hydrogen sensor has excellent detection sensitivity and stability, and more importantly, can satisfy the requirements for hydrogen detection at 25+/-5 DEG C, and the method does not need any additional heating system and has the advantage of lower cost than other methods. The detection limit at 25+/-5 DEG C can reach 1 ppm, and the resistance change is up to 4% when a 1V voltage source is used as the drive.

Description

technical field [0001] The invention relates to a hydrogen sensor, in particular to a titanium dioxide thin film hydrogen sensor and a preparation method thereof. Background technique [0002] As an emerging important renewable energy carrier and the most important industrial gas and special gas, hydrogen has been widely used in petrochemical industry, electronics industry, metallurgical industry, food processing, float glass, fine organic synthesis, aerospace, etc., but when When the hydrogen content in the air reaches 4%, it is very easy to explode, which brings great safety hazards to the application and storage of hydrogen. Therefore, a sensor that can sensitively detect hydrogen, has stable performance and is cheap has become a must in today's industrial field. Urgent needs. [0003] At present, a variety of gas sensors have appeared on the market, mainly electrochemical, semiconductor, pyroelectric, metal and optical, among which TiO 2 Because of its stable surface p...

Claims

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Application Information

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IPC IPC(8): G01N27/12
Inventor 高云吴文希夏晓红
Owner HUBEI UNIV
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