Ni/NiF2 reference electrode used for molten fluoride, and making method thereof

Abstract

The invention discloses a Ni / NiF2 reference electrode used for molten fluoride, and a making method thereof. The Ni / NiF2 reference electrode comprises a nickel wire electrode, an insulation sleeve and a sealing plug used for sealing the insulation sleeve; the bottom of the insulation sleeve is provided with a reference salt; the nickel wire electrode is fixed to the sealing plug, and one end of the nickel wire electrode traverses through the sealing plug, extends into the insulation sleeve and is immersed in the reference salt; the outer sidewall of the insulation sleeve is provided with an arc-shaped groove, and the bottom of the arc-shaped groove is provided with a through hole; the surface roughness Ra of the arc-shaped groove is less than 12.5[mu]m, and the radius of curvature of the arc-shaped groove is not less than 2mm; and the diameter of the through hole is 0.05-0.3mm, and the depth of the through hole is 0.3-2.0mm. The Ni / NiF2 reference electrode has the advantages of short ion conduction time, and good reappearance and stability of the electrode potential.

Description

technical field

[0001] The invention relates to a kind of Ni / NiF used in high temperature fluoride molten salt system 2 Reference electrode and its manufacturing method. Background technique

[0002] Electrochemical research in high-temperature molten salt system is of great significance in both basic research and industrial production, and the reference electrode plays a vital role in the accurate measurement of electrochemical parameters. In the electrochemical research and production of fluoride molten salt system, a bottleneck problem is how to prepare a reference electrode with stable performance, good reproducibility and long service life. The commonly used reference electrode in fluoride molten salt is Ni / NiF with hot-pressed boron nitride as the sleeve. 2 Reference electrode, Ni / NiF with lanthanum fluoride single crystal as diaphragm material 2 Reference electrode, or insert Pt, W and other inert metals directly into the molten salt as a quasi-reference electrode....

Examples

Embodiment 1

[0042] Such as Figure 1 ~ Figure 3 As shown, the present embodiment provides a kind of Ni / NiF for high temperature fluoride molten salt system 2 The reference electrode comprises a nickel wire electrode 1, an insulating sleeve 2 and a sealing plug 3; the nickel wire electrode is fixedly connected to the sealing plug, and the insulating sleeve 2 is equipped with a reference salt 6 for the sealing plug. To seal the insulating sleeve, the bottom end of the nickel wire electrode is immersed in the reference salt in the insulating sleeve; the outer wall of the insulating sleeve is provided with an arc groove 4, and the bottom of the arc groove is provided with a Through hole 5; through hole 5 is used as a salt bridge, so that the reference salt in the insulating casing and the high-temperature fluoride molten salt outside the insulating casing realize ion conduction; the surface roughness of the arc-shaped groove is 4 μm, The curvature radius R of the arc-shaped groove is 10mm; t...

Embodiment 2

[0051] In this example Ni / NiF 2 The Ni / NiF of embodiment 1 on the reference electrode structure 2 The reference electrode is similar, the difference lies in the parameters of each component.

[0052] A kind of mixed reference salt composed of FLINAK molten salt and nickel fluoride, nickel wire, zirconia doped boron nitride composite material as basic raw materials to prepare Ni / NiF 2 The method of reference electrode, comprises the following steps:

[0053] (1) Accurately weigh 10 grams of lithium fluoride, sodium fluoride, potassium fluoride, and nickel fluoride with a molar ratio of 37.2:9.2:33.6:20, put the above four fluorides into an agate mortar and grind them Mix well, put into graphite crucible, heat up from room temperature to 350°C at 5°C / min, dry under reduced pressure at 350°C for 10 hours, cool naturally, then grind into powder in agate mortar and put into reagent bottle spare;

[0054] (2) Take 7cm of nickel wire (99.98% purity) with a diameter of 1mm, heat i...

Embodiment 3

[0060] In this example Ni / NiF 2 The Ni / NiF of embodiment 1 on the reference electrode structure 2 The reference electrode is similar, the difference lies in the parameters of each component.

[0061] A kind of mixed reference salt composed of FLINAK molten salt and nickel fluoride, nickel wire, zirconia doped boron nitride composite material as basic raw materials to prepare Ni / NiF 2 The method of reference electrode, comprises the following steps:

[0062] (1) Accurately weigh 10 grams of lithium fluoride, sodium fluoride, potassium fluoride, and nickel fluoride with a molar ratio of 44.175:10.925:39.9:5, put the above four fluorides into an agate mortar and grind them Mix well, put into graphite crucible, heat up from room temperature to 350°C at 5°C / min, dry under reduced pressure at 350°C for 10 hours, cool naturally, then grind into powder in agate mortar and put into reagent bottle spare;

[0063] (2) Take 7cm of nickel wire (99.98% purity) with a diameter of 1mm, he...

technical field

[0001] The invention relates to a kind of Ni / NiF used in high temperature fluoride molten salt system 2 Reference electrode and its manufacturing method. Background technique

[0002] Electrochemical research in high-temperature molten salt system is of great significance in both basic research and industrial production, and the reference electrode plays a vital role in the accurate measurement of electrochemical parameters. In the electrochemical research and production of fluoride molten salt system, a bottleneck problem is how to prepare a reference electrode with stable performance, good reproducibility and long service life. The commonly used reference electrode in fluoride molten salt is Ni / NiF with hot-pressed boron nitride as the sleeve. 2 Reference electrode, Ni / NiF with lanthanum fluoride single crystal as diaphragm material 2 Reference electrode, or insert Pt, W and other inert metals directly into the molten salt as a quasi-reference electrode....

Examples

Embodiment 1

[0042] Such as Figure 1 ~ Figure 3 As shown, the present embodiment provides a kind of Ni / NiF for high temperature fluoride molten salt system 2 The reference electrode comprises a nickel wire electrode 1, an insulating sleeve 2 and a sealing plug 3; the nickel wire electrode is fixedly connected to the sealing plug, and the insulating sleeve 2 is equipped with a reference salt 6 for the sealing plug. To seal the insulating sleeve, the bottom end of the nickel wire electrode is immersed in the reference salt in the insulating sleeve; the outer wall of the insulating sleeve is provided with an arc groove 4, and the bottom of the arc groove is provided with a Through hole 5; through hole 5 is used as a salt bridge, so that the reference salt in the insulating casing and the high-temperature fluoride molten salt outside the insulating casing realize ion conduction; the surface roughness of the arc-shaped groove is 4 μm, The curvature radius R of the arc-shaped groove is 10mm; t...

Embodiment 2

[0051] In this example Ni / NiF 2 The Ni / NiF of embodiment 1 on the reference electrode structure 2 The reference electrode is similar, the difference lies in the parameters of each component.

[0052] A kind of mixed reference salt composed of FLINAK molten salt and nickel fluoride, nickel wire, zirconia doped boron nitride composite material as basic raw materials to prepare Ni / NiF 2 The method of reference electrode, comprises the following steps:

[0053] (1) Accurately weigh 10 grams of lithium fluoride, sodium fluoride, potassium fluoride, and nickel fluoride with a molar ratio of 37.2:9.2:33.6:20, put the above four fluorides into an agate mortar and grind them Mix well, put into graphite crucible, heat up from room temperature to 350°C at 5°C / min, dry under reduced pressure at 350°C for 10 hours, cool naturally, then grind into powder in agate mortar and put into reagent bottle spare;

[0054] (2) Take 7cm of nickel wire (99.98% purity) with a diameter of 1mm, heat i...

Embodiment 3

[0060] In this example Ni / NiF 2 The Ni / NiF of embodiment 1 on the reference electrode structure 2 The reference electrode is similar, the difference lies in the parameters of each component.

[0061] A kind of mixed reference salt composed of FLINAK molten salt and nickel fluoride, nickel wire, zirconia doped boron nitride composite material as basic raw materials to prepare Ni / NiF 2 The method of reference electrode, comprises the following steps:

[0062] (1) Accurately weigh 10 grams of lithium fluoride, sodium fluoride, potassium fluoride, and nickel fluoride with a molar ratio of 44.175:10.925:39.9:5, put the above four fluorides into an agate mortar and grind them Mix well, put into graphite crucible, heat up from room temperature to 350°C at 5°C / min, dry under reduced pressure at 350°C for 10 hours, cool naturally, then grind into powder in agate mortar and put into reagent bottle spare;

[0063] (2) Take 7cm of nickel wire (99.98% purity) with a diameter of 1mm, he...

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