An electrochemical sensor for monitoring nitrogen content in molten iron and its preparation method

An electrochemical and sensor technology, applied in the field of electrochemical sensors for monitoring nitrogen content and their preparation, can solve the problems of single phase number of compounds, poor compatibility and mutual repulsion, and achieve precise control of thickness, small interface internal resistance, interface The effect of low resistance

Active Publication Date: 2019-09-24
NORTHEASTERN UNIV LIAONING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the above-mentioned technical problems, the object of the present invention is to provide an electrochemical sensor for monitoring the nitrogen content in molten iron, which not only has excellent thermal shock resistance and high temperature resistance, but also has good conductivity of the auxiliary electrode in the electrochemical sensor, and is compatible with Solid electrolytes have excellent chemical compatibility; the number of compound phases is relatively single, which avoids the problem of poor compatibility and mutual exclusion. At the same time, the battery reaction process is simpler and the working performance is more stable, so it is a nitrogen with better performance. Sensor, especially suitable for on-line monitoring of nitrogen content in iron and steel metallurgy process

Method used

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  • An electrochemical sensor for monitoring nitrogen content in molten iron and its preparation method
  • An electrochemical sensor for monitoring nitrogen content in molten iron and its preparation method
  • An electrochemical sensor for monitoring nitrogen content in molten iron and its preparation method

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preparation example Construction

[0049] See figure 2 Shown is a flow chart of the preparation method of an electrochemical sensor for monitoring nitrogen content of the present invention. Basically include the steps: S1: preparing a YSZ solid electrolyte layer; S2: high temperature surface nitriding treatment: using a high temperature surface nitriding method to make one side surface of the YSZ solid electrolyte layer contact with metal nitride powder, baking and nitrogen at high temperature Under the protection of the atmosphere, the side surface of the YSZ solid electrolyte layer is nitridated, and a layer of zirconia layer (YNSZ) co-doped with nitrogen ions and oxygen ions is formed by substituting nitrogen ions for part of the oxygen ions in YSZYSZ. Auxiliary electrode layer); S3: Coating NiO and Ni mixed powder on the other side of the YSZ solid electrolyte layer to prepare a reference electrode layer. Preferably, step S3 is to spray the mixed powder of NiO and Ni onto the surface of the YSZ solid electr...

Embodiment 1

[0076] Step 1. Prepare YSZ solid electrolyte powder: Weigh 7.82g YCl 3 , 148.24g of ZrOCl 2 ·8H 2 O, dissolved in 1L of deionized water to obtain Zr 4+ The concentration is about 0.46mol / L. Under the stirring of a magnetic stirrer, at a constant temperature of 25°C, add ammonia water dropwise for co-precipitation. When the PH=9-10, stop the titration, filter the precipitate, and wash with distilled water and ethanol three times to remove Cl - Plasma impurity ions. Dry the precipitate at a temperature of 75~85℃, dry at a constant temperature for 24h, grind it in an agate mortar for 0.5h, and then roast it in a high-temperature furnace for 10h at a roasting temperature of 600℃ to obtain Y 2 O 3 Stable zirconia solid electrolyte powder YSZ.

[0077] Step 2. Making YSZ solid electrolyte layer: Weigh 30g of solid YSZ powder into a 5cm diameter press mold, apply 300Mpa axial pressure to form a sheet-shaped body, and place it in a high-temperature furnace for sintering. The sintering tem...

Embodiment 2

[0081] The difference between this embodiment and Embodiment 1 is that in step 3, the heating temperature in the furnace 40 is controlled to 1600° C. for 8 hours to obtain the YNSZ auxiliary electrode layer 12 with a thickness of 0.8 mm.

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Abstract

The invention relates to an electrochemical sensor for monitoring the nitrogen content. The sensor comprises a solid electrolyte layer which takes Y2O3-doped zirconia (YSZ) as a matrix material, and an auxiliary electrode layer which takes nitrogen-doped Y2O3 stabilized zirconia (YNSZ) formed by replacing partial oxygen ions in the YSZ with nitrogen ions as a matrix material. The invention furtherprovides a manufacturing method for the electrochemical sensor. A high-temperature surface nitriding treatment method is used for generating the YNSZ auxiliary electrode layer with a certain thickness in situ on the surface of the prepared YSZ solid electrolyte, so that the process is rapid and simple, the YNSZ auxiliary electrode layer is compact and pore-free and is tightly and firmly combinedwith the matrix of the YSZ solid electrolyte, the compatibility is good, and the interface resistance is small; and therefore, the nitrogen content electrochemical sensor with the excellent performance can be further obtained by means of the manufacturing method.

Description

Technical field [0001] The invention relates to the technical field of electrochemical sensors, in particular to an electrochemical sensor for monitoring nitrogen content and a preparation method thereof. Background technique [0002] Online accurate measurement of nitrogen content in molten steel is a vital task in the steel metallurgy process. Some researchers have used AlN as a solid electrolyte to prepare nitrogen sensors, but because of its high electronic conductivity at high temperatures (solid electrolytes should have high ionic conductivity rather than electronic conductivity) and easy oxidation. Successfully used in actual production. Hong Yanruo et al. used the three-phase compound β-Al 2 O 3 +α-Al 2 O 3 +AlN is used as solid electrolyte and metal-metal compounds are used as reference electrodes. Nitrogen sensors have been developed to monitor the nitrogen activity in Fe-Mn-N and Fe-Mn-V-N alloys. The experimental results show good regularity. However, the prior art ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/30
Inventor 刘涛莫扬成温天朋王相南易茂义张震
Owner NORTHEASTERN UNIV LIAONING
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