JPH0623718B2 - Oxygen ion conductivity measurement device - Google Patents

Description

TECHNICAL FIELD The present invention relates to an apparatus for measuring oxygen ion conductivity characteristics.

Substances exhibiting oxygen ion conductive properties have been developed as oxygen concentration measuring devices and solid-state batteries, and are widely used in the automobile industry and the like. However, new oxygen ion conductive materials are being researched and developed, and measurement of oxygen ion conductive properties is important for research and development.

2. Description of the Related Art A conventional device for measuring oxygen ion conductivity has a structure in which the circumference of a disk-shaped sample and the end of a ceramic pipe are glass-welded to be airtight. Therefore, a step of connecting the sample to the ceramic pipe is required before measuring the characteristics, and the sample once used for measurement is difficult to use for other measurements. Furthermore, since the welded portion is glass, it is not possible to measure the temperature above the softening point of the glass. Further, there is a problem that lead wires must be drawn out from the electrodes coated on both sides of the disk-shaped sample.

The present invention has been made to solve the problems in the conventional device, without the step of connecting the sample and the ceramic pipe or the operation of pulling the lead wire from the electrodes provided on both sides of the disk-shaped sample, It is to provide a device that can be measured immediately.

Constitution of the invention The present invention has a difficulty in connecting a disc-shaped oxygen ion conductive sample and a ceramic pipe by using a metal ring as a packing, and a metal coated on the inside and outside of the ceramic pipe. Has been solved by using as a circuit for measuring electromotive force.

The gist of the present invention is, in an apparatus for measuring an oxygen ion conductive property by energizing a disc-shaped sample, a disc-shaped sample and metal rings arranged on both sides thereof are ceramic nuts and ceramic pipes that can be fitted to each other. The disc-shaped sample is clamped by the metal ring and the space is formed on both sides of the disc-shaped sample by tightening the pipe and the nut while being arranged so as to fit in the concave part of the nut. In addition, the disk-shaped sample is electrically connected to the electric path coated on the inner and outer surfaces of the pipe and the nut through the metal ring, and the measuring apparatus for the oxygen ion conductivity characteristic is provided.

Since the present invention has the above-mentioned configuration, the disk-shaped sample can be exchanged only by rotating the ceramic nut. Further, by sandwiching both sides of the disc-shaped sample with metal rings, a space is formed on both sides, so that the oxygen partial pressure on each side of the disc-shaped sample can be changed independently.
Further, since the metal coated on the inner and outer surfaces of the ceramic pipe and the ceramic nut is used as the electric path, no lead wire for measurement is required.

The oxygen ion conductivity characteristic measuring apparatus of the present invention will be described with reference to the drawings. FIG. 1 is a schematic cross-sectional view of the apparatus, in which 1 is a ceramic pipe with a male thread at its end, and 2 is a female inside. A nut made of ceramics with a screw, 3 is an O-ring made of metal, 4 is a disk-shaped sample having oxygen ion conductivity, and 5 is an electric furnace. Fig. 2 is an assembly drawing for sample insertion.
The dotted line shows the part coated with metal.
Both sides of the sample are clamped by metal O-rings 3 and strongly clamped by a ceramic pipe 1 and a ceramic nut 2. Therefore, the airtightness inside and outside the pipe is maintained by the O-ring. The oxygen pressure inside and outside the pipe can be set independently by changing the oxygen partial pressure in the gas supplied from the left and right sides of the device. The potential on the right side surface of the sample is transmitted to the metal coated inside the ceramic pipe 1 through the right metal O-ring, and is guided to the outside of the furnace. The potential on the left side of the sample is
Ceramic nut 2 through the left metal O-ring
Is transmitted to the metal coated on the outside of the ceramic pipe, further passes through the threaded portion, is transmitted to the metal coated on the outside of the ceramic pipe 1, and is guided outside the furnace. Therefore, the electric wire for measuring the electromotive force is unnecessary for the present apparatus, and the step of connecting the electric wire to the sample is also unnecessary.

EFFECTS OF THE INVENTION According to the device of the present invention, the oxygen ion conductivity characteristics can be quickly measured with a simple device, the sample used for the measurement can be used for other measurements, and the measurement can be performed up to a temperature higher than the conventional measurement temperature. It will be possible. Moreover, the electric wire for measuring the electromotive force is unnecessary, and therefore the connection between the sample and the electric wire is also unnecessary.

Example Alumina was selected as the ceramic, and gold was used as the O-ring and the electric circuit material. Stabilized bismuth oxide was used as a sample, and the apparatus shown in FIG. 1 was used.

The temperature of the sample was 200 ° C. to 750 ° C., and the temperature was raised at 2 ° C./min. When the right side of the sample is 1 atm oxygen and the left side is 1 atm high purity argon, the left side oxygen pressure is
It was less than .1 ppm and it was found that the airtightness between the sample and the ceramic pipe was sufficiently maintained.

[Brief description of drawings]

FIG. 1 is a schematic diagram of the device of the present invention, and FIG. 2 is an assembly diagram for inserting a sample. 1: Ceramic pipe, 2: Ceramic nut, 3: Metal O-ring, 4: Disc-shaped sample, 5: Electric furnace.

Claims (1)

[Claims] 1. A device for measuring oxygen ion conductivity by energizing a disc-shaped sample, wherein a disc-shaped sample and metal rings arranged on both sides of the disc-shaped sample are made of ceramic nuts and ceramic pipes. In between, the disc-shaped sample is clamped by the metal ring by tightening the pipe and the nut so that the disc-shaped sample is placed in the recess of the nut, and a space is formed on both sides of the disc-shaped sample. An apparatus for measuring oxygen ion conductivity characteristics, characterized in that the disk-shaped sample is electrically connected through a metal ring to an electric path coated on the inner and outer surfaces of the pipe and the nut.