Ppb-level hydrogen sensor for detecting lower limit and preparation method thereof

A sensor and hydrogen technology, applied in the field of sensors, can solve the problems of limiting the test range of sensors, sudden changes in electrical properties, damage to Pd films, etc., and achieve the effects of humidity stability and selective application, room temperature environment application, and wide test range

Active Publication Date: 2020-11-20
UNIV OF ELECTRONIC SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when H 2 When the concentration of Pd increases to more than 2%, the α-phase palladium hydride will transform into the β-phase palladium hydride, which means that the Pd lattice will produce a violent lattice expansion that is not fully reversible, and cause a sudden change in its electrical properties.
For the commonly used Pd-based thin-film resistive sensors, the β-phase change will even cause damage to the Pd film and short-circuit the circuit, thus limiting the test range of the sensor.

Method used

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  • Ppb-level hydrogen sensor for detecting lower limit and preparation method thereof
  • Ppb-level hydrogen sensor for detecting lower limit and preparation method thereof
  • Ppb-level hydrogen sensor for detecting lower limit and preparation method thereof

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preparation example Construction

[0036] A method for preparing a hydrogen sensor with a ppb level detection lower limit, characterized in that it comprises the following steps:

[0037] Step 1, cutting the metal foam to a suitable size, cleaning with deionized water, absolute ethanol and acetone in turn, and drying; the metal foam is nickel foam, copper foam, zinc foam, aluminum foam, cobalt foam, etc., the foam The thickness of the metal is 0.1mm ~ 1mm, and the porosity is above 98%;

[0038] Step 2. Heat-treat the metal foam after cleaning and drying in step 1 in an air atmosphere. The heat treatment temperature is 500-1000° C., and the heat-treatment time is 3-6 hours. After completion, naturally cool to room temperature and take it out to obtain oxidized metal foam;

[0039] Step 3, using the DC magnetron sputtering method, sputtering the surface of the oxidized metal foam obtained in step 2 to obtain Pd nanoparticles with a particle size of 5nm to 10nm, wherein the sputtering rate is 8nm / min, and the spu...

Embodiment 1

[0047] A preparation and activation method of a ppb-level detection lower limit hydrogen sensor, the specific steps are:

[0048] Step 1. Select nickel foam with a thickness of 0.3mm and a porosity of 98%, cut the nickel foam into small squares of 3mm×8mm, and then ultrasonically clean it in deionized water, absolute ethanol and acetone for 15 minutes;

[0049] Step 2. Heat-treat the nickel foam after step 1 has been cleaned and dried in an air atmosphere. The heat-treatment temperature is 800° C. and the heat-treatment time is 3 hours. After completion, naturally cool to room temperature and take it out to obtain oxidized nickel foam;

[0050] Step 3, adopting DC magnetron sputtering, sputtering on the surface of oxidized nickel foam obtained in step 2 to obtain Pd nanoparticles with a particle size of about 8nm, wherein the sputtering rate is 8nm / min, and the sputtering time is 180s. The shooting target is pure Pd (99.9995wt%) target;

[0051] Step 4, the two ends of the ox...

Embodiment 2

[0058] A preparation and activation method of a ppb-level detection lower limit hydrogen sensor, the specific steps are:

[0059] Step 1. Select foamed copper with a thickness of 0.5mm and a porosity of 98%, cut the foamed copper into small squares of 3mm×8mm, and then ultrasonically clean it in deionized water, absolute ethanol and acetone for 15 minutes;

[0060] Step 2. Heat-treat the copper foam after cleaning and drying in step 1 in an air atmosphere. The heat-treatment temperature is 650° C. and the heat-treatment time is 6 hours. After completion, naturally cool to room temperature and take it out to obtain oxidized copper foam;

[0061] Step 3, adopting DC magnetron sputtering, sputtering the surface of the oxidized copper foam obtained in step 2 to obtain Pd nanoparticles with a particle size of about 8nm, wherein the sputtering rate is 8nm / min, and the sputtering time is 180s. The shooting target is pure Pd (99.9995wt%) target;

[0062] Step 4, the two ends of the o...

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Abstract

The invention discloses a ppb-level hydrogen sensor for detecting a lower limit, and belongs to the technical field of sensors. The hydrogen sensor comprises oxidized foam metal and palladium nanoparticles loaded on the oxidized foam metal, wherein the particle size of the palladium nanoparticles is 5-10 nm, the oxidized foam metal is obtained by carrying out high-temperature heat treatment on foam metal in an air atmosphere, the heat treatment temperature is 500-1000 DEG C, and the time is 3-6 h. Foam metal is fully oxidized at a certain temperature, a large number of insulating metal oxide nano wrinkles are obtained on the surface of the foam metal, and the oxidized foam metal substrate has a large surface area so as to adhere Pd nano particles; by utilizing the phenomenon that Pd reactswith high-concentration hydrogen to generate an incompletely reversible beta-phase Pd-H compound, a method for activating the hydrogen sensor through the high-concentration hydrogen is provided for the first time, and stable ppb-level hydrogen sensing performance of the hydrogen sensor is achieved.

Description

technical field [0001] The invention belongs to the technical field of sensors, and in particular relates to a highly sensitive hydrogen sensor with a lower detection limit of ppb level and a preparation method thereof. Background technique [0002] Due to the advantages of high combustion efficiency and non-polluting products, hydrogen energy, together with solar energy and nuclear energy, is called the three major new energy sources. As one of the key technologies to realize the safe and effective utilization of hydrogen energy, the hydrogen sensor has also received widespread attention. In addition, hydrogen, as the most abundant substance in the universe, accounts for 75% of the total mass of matter and more than 90% of the total number of atoms. Therefore, hydrogen detection plays a pivotal role in exploring the mysteries of outer space and the origin of the universe, detecting the state of the earth, and searching for extraterrestrial life. Nowadays, more and more co...

Claims

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Application Information

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IPC IPC(8): G01N27/12
CPCG01N27/127
Inventor 蒋洪川田佳蔚邓新武师港伟赵晓辉张万里
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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