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Embedded NASICON-based H2 sensor with compound metal oxide as passivation reference electrode and manufacturing method of embedded NASICON-based H2 sensor

A reference electrode and composite metal technology, applied in the direction of material electrochemical variables, etc., can solve the problems of shortened sensor life, reduced catalyst specific surface area, catalyst agglomeration, etc., achieve good electrical conductivity and chemical stability, improve heat utilization, and prepare The effect of simple process

Active Publication Date: 2013-08-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this sensor has the following disadvantages: First, compared with the electrical signal, the output intensity of the optical signal is weaker, and the output needs to be amplified; second, after repeated use, the Pd film is easy to delaminate, bubbles appear, and the service life is limited
In addition, the hydrogen-sensitive material of the fiber-optic hydrogen sensor is noble metal Pd. At the same time, the use of the amplifier circuit not only increases the volume and weight of the device, but also increases the cost.
The contact combustion sensor has the advantages of simple structure and low cost, but there are still some problems to be solved during the use of this type of sensor. For example, the agglomeration phenomenon will occur when the catalyst is used for a long time, which will reduce the specific surface area of ​​the catalyst and reduce the performance of the sensor. Sensitivity; In addition, the sensitive signal generated by this sensor during use is relatively weak, and generally requires an external amplifier circuit to amplify
Electrochemical sensor is another widely used sensor. The advantages of this type of sensor are good linearity and high precision, but the liquid electrolyte is easy to dry up, which shortens the life of the sensor. Once the acidic electrolyte leaks, it will cause corrosion. The liquid electrolyte makes this The sensor can only be used at room temperature, not suitable for high temperature or cold environment

Method used

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  • Embedded NASICON-based H2 sensor with compound metal oxide as passivation reference electrode and manufacturing method of embedded NASICON-based H2 sensor
  • Embedded NASICON-based H2 sensor with compound metal oxide as passivation reference electrode and manufacturing method of embedded NASICON-based H2 sensor
  • Embedded NASICON-based H2 sensor with compound metal oxide as passivation reference electrode and manufacturing method of embedded NASICON-based H2 sensor

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Using spinel-type composite metal oxide CoCr 0.8 mn 1.2 o 4 As a passivation electrode material, Au is used as a sensitive electrode to make a mixed potential type H 2 Sensor, its specific production process:

[0035] 1. Preparation of NASICON powder by sol-gel method

[0036] Specific material preparation process:

[0037] (1) Take 19.3366g of ZrOCl 2 , 7.6484 g NaNO 3 , 3.9634g (NH 4 ) 2 HPO 4 Dissolve in 300ml, 200ml and 100ml of deionized water respectively, and set aside;

[0038] (2) Slowly drip ammonia water with a volume fraction of 20% into ZrOCl 2 solution until pH = 10, at this time white flocculent ZrO(OH) 2 Precipitation, related chemical reactions are as follows:

[0039] ZrOCl 2 +2NH 4 OH=ZrO(OH) 2 ↓+2NH 4 Cl...................................(2-1)

[0040] (3) The product obtained in (2) is centrifugally cleaned with a high-speed centrifuge to remove the Cl - to obtain pure ZrO(OH) 2 precipitation;

[0041] (4) with concentrated HNO ...

Embodiment 2

[0060] spinel composite metal oxide CoCr 1.2 mn 0.8 o 4 As a passivation electrode material, Au is used as a sensitive electrode to make a mixed potential type H 2 Sensor, its specific production process:

[0061] With Cr(NO 3 ) 3 , Co(NO 3 ) 2 and Mn(NO 3 ) 3 As a raw material, weigh 21.6g, 13g and 12.9g to prepare the solution respectively. The specific preparation process is as described above to obtain CoCr 1.2 mn 0.8 o 4 . The fabrication process of the device is the same as above.

Embodiment 3

[0063] spinel composite metal oxide CoCrMnO 4 As a passivation electrode material, Au is used as a sensitive electrode to make a mixed potential type H 2 Sensor, its specific production process:

[0064] With Cr(NO 3 ) 3 , Co(NO 3 ) 2 and Mn(NO 3 ) 3 As the raw material, weigh 21.6g, 13g and 12.9g to prepare the solution respectively. The specific preparation process is as described above. Finally, the material is sintered in a high-temperature sintering furnace at 600°C to obtain CoCrMnO 4 . The fabrication process of the device is the same as above.

[0065] The test method of the device adopts the traditional static test method:

[0066] 1. Place the device in a static test bottle A with a volume of 1L to achieve stability, that is, the electromotive force value of the device in the air (EMF 空气 )constant.

[0067] 2. In the static test bottle with the same volume of 1L, configure the atmosphere to be tested with the corresponding concentration (100ppm, 500ppm, 10...

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Abstract

The invention discloses an embedded NASICON-based H2 sensor with a compound metal oxide as a passivation reference electrode, and a preparation method of the embedded NASICON-based H2 sensor, belonging to the technical field of gas sensors. The sensor is composed of an Al2O3 ceramic tube used as an insulating layer, a nickel-cadmium alloy heating wire arranged inside the Al2O3 ceramic tube, a first NASICON ion conducting layer coated on the surface of the Al2O3 ceramic tube, a sensitive electrode prepared on the surface of the NASICON ion conducting layer, a second NASICON ion conducting layer coated on the sensitive electrode and the surface of the first NASICON ion conducting layer, and a passivation reference electrode prepared on the surface of the second NASICON ion conducting layer, wherein the sensitive electrode is made of a ring-shaped netted Au material, and the passivation reference electrode is composed of the ring-shaped netted Au material and a compound metal oxide electrode material CoCrxMn2-xO4 layer coated on the Au material. The sensor can be used for detecting the hydrogen concentration in atmosphere.

Description

technical field [0001] The invention belongs to the technical field of gas sensors, and in particular relates to a buried type NASICON-based mixed potential type H sensor with a novel composite metal oxide as a passivation reference electrode. 2 The sensor can be used to detect the concentration of hydrogen in the atmosphere. Background technique [0002] Hydrogen is a colorless, odorless, flammable gas. It is an important reducing agent in chemical production. It is also considered to be the most ideal alternative energy source. It is widely used in industrial production processes and new energy exploration. However, since hydrogen is an extremely flammable gas, it can burn when the volume fraction in air is 4% to 75%. If hydrogen reaches the above concentration in a limited space, it will be very dangerous. 2 It is very important to quickly, timely and accurately check and monitor the concentration of hydrogen, so it is necessary to develop a hydrogen sensor with high sen...

Claims

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Application Information

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IPC IPC(8): G01N27/26G01N27/30
Inventor 梁喜双张含卢革宇
Owner JILIN UNIV
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