JPS63145949A - Emission spectral analyzer - Google Patents

Abstract

PURPOSE:To achieve a depthwise composition analysis from the surface of a sample, by sputtering the sample surface with a glow discharge. CONSTITUTION:A sample 3 is mounted at the open end of a hollow anode 2 and an Ar gas is introduced into the anode 2 at an Ar gas supply port 9 while it is discharged through a gas discharge port 10 to create a low pressure Ar atmosphere. Then, a discharge is caused with a glow discharge circuit 5 in an abnormal glow discharge area between the anode 2 and the sample 3 to scrape off the surface of a sample 3 by Ar on sputtering. After the abnormal glow discharge is performed to a specified depth, an Ar gas is introduced into the anode 2 to develop an atmospheric pressure state in the anode 2. A spectroscope 1 receives emission attributed to elements at an analyzing point as generated by a spark discharge between an anode electrode rod 7 and the sample 3 thereby enabling depthwise composition analysis quickly at a high accuracy.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an optical emission spectrometer that performs compositional analysis in the depth direction from the surface of steel.

[Conventional technology]

For example, known techniques for CO concentration analysis of samples such as carburized steel, in which carbon 0 degrees (C0 degrees) changes in the depth direction from the surface of the steel, include (1) A technique in which samples of chips are sequentially collected mechanically and analyzed using a chemical analysis method, (2) a technique in which the sample is polished or cut using abrasive paper or a lathe, etc. from the surface of the sample at each step in the depth direction; (3) A technique for analyzing a sample in the depth direction using glow discharge emission spectroscopy, etc. are known.

In particular, when relatively thick objects are targeted, the analysis technique (3) based on glow discharge emission spectroscopy is used.

[Problem that the invention seeks to solve]

However, the above conventional analysis techniques have the following problems. In other words, in the analysis technique using the chemical analysis method described in (1) above, chips are collected at different depths from the surface of the sample, and the chips are analyzed using a wet method after being dissolved, which requires a large amount of man-hours and time. Even in the above-mentioned analysis technique using spark discharge optical emission spectroscopy (2), a considerable number of man-hours are still required because the sample is manually polished or cut. In addition, in the analysis technique using glow discharge optical emission spectroscopy described in (3) above, there is a particular problem in C analysis, which is thought to be caused by the generation of oil mist from the vacuum pump in the glow discharge lamp. There was a problem in that it was difficult to obtain stability in luminescence intensity and the reliability of analytical values was low.

[Means for solving problems]

The present invention solves the above-mentioned conventional problems, and aims to automate the compositional analysis in the depth direction from the surface of steel, especially the analysis of C,
The purpose is to provide a means for improving speed and analysis accuracy, and includes a cylindrical hollow anode, an argon (Ar) gas supply port into the hollow anode, and a hollow f
The Ia structure sputters the surface of the sample by applying a DC voltage between a flat sample mounted as a cathode to the open end of the g electrode and the anode, and The present invention relates to an emission spectroscopic analysis HC characterized by comprising an anode electrode rod provided to cause spark discharge between the sample and the sample as a cathode.

The present invention will be explained below based on the drawings.

FIG. 1 is an explanatory diagram showing the configuration of an example of a light emitting device of an optical emission spectrometer according to the present invention. In the same figure, the spectrometer (1)
A cylindrical hollow anode (2) is attached adjacent to the hollow anode (2), and a flat sample (3) as a cathode is attached to the open end of the hollow anode (2).
is attached via the holder (4), and the hollow anode (2
) is connected to the glow discharge circuit (9).

An insulating part (
6) completely insulated. The cylindrical hollow anode (2
) is provided with an anode electrode rod (2) at the center of the tube axis, and the anode electrode rod (2) and the sample (3) are connected to a spark discharge circuit (8). An Ar gas supply port (9) and a gas discharge port 0 are attached to the cylindrical hollow w4 (2).

Said l! The distance between the g-electrode and the surface of the sample (3) can be changed arbitrarily.

[For production]

For example, a sample (3
) To analyze C in the depth direction from the surface, first attach the sample (3) to the open end of the hollow anode (2).
While introducing Ar gas from the Ar gas supply port (9) into the hollow anode (2), the gas is discharged from the gas exhaust port using a vacuum pump (not shown), and a low pressure of 5 Torr is applied to the inside of the hollow anode (2).
Create an atmosphere. Next, the hollow anode (2) and the sample (3)
) with 50mA-1 by glow discharge circuit (5).
Discharge is caused under the condition of 200V.

This discharge is a discharge in the so-called abnormal glow discharge region, and is
The surface of the sample (3) is scraped off by sputtering using ions. The amount of sputtering in the depth direction, that is, the sample (3
) The depth from the surface is determined, for example, by measuring the emission intensity of iron (Fe) as a monitor. After performing abnormal glow discharge to a predetermined depth, Ar gas is introduced into the hollow anode (2) to bring the inside of the hollow anode (2) to atmospheric pressure, and the connection between the anode electrode rod ■ and the sample (3) is The spectrometer (1) detects the light emitted by element C at analysis point A caused by the spark discharge between
The Cci degree is determined. The distance between the anode electrode rod (2) and the surface of the sample (3) is approximately 50 seconds (2) during glow discharge, and the distance is brought close to the required distance during spark discharge.

By repeating the above sputtering of the sample surface due to abnormal glow discharge in a low-pressure Ar atmosphere and the spark discharge in an atmospheric-pressure Ar atmosphere, it is possible to analyze C at each stage in the depth direction from the surface of the sample (3). .

〔Example〕

The following will explain based on examples.

Using the apparatus of the present invention having the configuration shown in FIG. 1, a C analysis was conducted in the depth direction from the surface of a sample that had been carburized by gas carburization and then directly quenched at 930°C. Table 1 shows the chemical composition of the sample before carburizing.
Further, Table 2 shows the conditions for glow discharge and spark discharge.

The amount of sputtering in the depth direction of the sample can be detected using a wavelength of 37
This was done by measuring the Fe emission intensity of t9.9 people.

Further, Table 3 shows the analytical elements and the wavelengths of the analytical lines used. For comparison, an analysis using a conventional chemical analysis method was also conducted.

Table 1 Table 2 Table 3 Of the analysis results, C with large concentration changes in the surface layer
The results are shown in Figure 2. In the figure, the horizontal axis is the depth from the sample surface, the vertical axis is the C concentration, the solid line a is the analysis value by the apparatus of the present invention, and the broken line is the analysis value by the conventional chemical analysis method. From the figure, it can be seen that the conventional chemical analysis method requires a certain thickness in the depth direction to collect chips, and only average analytical values can be obtained, whereas the device of the present invention A large number of measurement points can be taken in the horizontal direction.
It can be seen that highly accurate analysis results can be obtained.

In addition, since sputtering on the sample surface is performed automatically,
The time and man-hours required for analysis are also much less than when using conventional techniques.

〔Effect of the invention〕

As explained above, by applying the apparatus of the present invention, which performs sputtering on the sample surface using glow discharge and performs elemental analysis using spark discharge, for composition analysis in the depth direction from the surface of steel, it is possible to analyze the composition in the depth direction from the surface of steel. Analysis can be performed quickly and with high precision without any problems. In particular, it is possible to accurately determine caIf in the depth direction of the surface layer of carburized material, which is extremely effective in improving quality control and operational management.

[Brief explanation of the drawing]

FIG. 1 is an explanatory diagram showing the configuration of an example of a light emitting device of an optical emission spectrometer of the present invention, and FIG. 2 is a diagram showing the relationship between the depth from the sample surface of a carburized material and the C concentration. 1... Spectrometer 2... Hollow anode 3...
Sample 4...Holder 5...Glow discharge circuit 6...Insulating part 7...Anode electrode rod
8...Spark discharge circuit 9...Ar gas supply port
IO...Gas exhaust port Figure 2 0 0.2 0. 'f O, f wiping tatsu or shi leaking 0 wet)

Claims (1)

[Claims] A DC voltage is applied between a cylindrical hollow anode, an argon gas supply hole into the hollow anode, a flat sample attached as a cathode to the open end of the hollow anode, and the anode. Luminescence spectroscopy characterized by comprising a mechanism for sputtering the surface of a sample, and an anode electrode rod provided at the center of the tube axis of the cylindrical hollow anode to cause spark discharge between the sample and the cathode. Analysis equipment.