JPH09222402A - Method for surface analysis of insulator - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain an analytical method, for the surface of an insulator, which prevents the insulator from being charged with electricity and in which a precise analysis can be performed. SOLUTION: An insulator 3 is installed on a sample base 17 inside a surface analyzer, and the surface of the insulator 3 is analyzed by an electron spectroscopic method. At this time, a part 3a, to be analyzed, at the insulator 3 is covered with a mask piece 5 which is attached at the upper part of the sample base 17, and a metal vapor-deposited film 4 is formed on an uncovered face 3b at the insulator 3 by using a vapor deposition device 6 installed inside the surface analyzer. Thereby, since the insulator 3 is not exposed to the air, the metal vapor-deposited film 4 is not oxidized, and the removal effect of electrification of the insulator 3 can be maintained in a good state.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing the surface of an insulator, and more particularly to a method for analyzing the surface of an insulator using an Auger electron spectroscopy analyzer or an X-ray photoelectron spectroscopy analyzer.

[0002]

2. Description of the Related Art Auger electron spectroscopy analyzers (AES) and X-ray photoelectron spectroscopy analyzers (EES) that require electron beams and X-rays are used as devices for analyzing the surface composition of materials by electron spectroscopy.
SCA) is known. When the substance to be analyzed is an insulator when the substance is analyzed using the analyzer, the insulator is easily charged. The charging may distort the spectrum shape of the measurement or shift the peak.

[0003]

Therefore, in the Auger electron spectroscopic analyzer, the insulator to be measured is tilted to reduce the incident angle of the electron beam so that the charge can easily escape, but the shape of the region to be analyzed is It becomes an ellipse and is not suitable for analysis of minute areas. Further, the X-ray photoelectron spectroscopy analyzer irradiates an electron shower having a negative charge to neutralize the positive charge due to X-ray irradiation, but the charge has not been sufficiently removed. Therefore, there has been attempted a method of forming a metal vapor deposition film and then installing the metal vapor deposition film in the above-mentioned analysis device, but the removal of the charge varies. It is speculated that this is because the insulator is exposed to the atmosphere and the metal vapor deposition film is oxidized.

The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a surface analysis method for an insulator, which prevents electrification of the insulator and enables accurate analysis. It is in.

[0005]

According to a first aspect of the present invention, there is provided a surface analysis method for an insulator, wherein the insulator is placed on a sample table in a surface analyzer and the surface of the insulator is analyzed by electron spectroscopy. In this case, a mask piece mounted above the sample table covers the analysis portion of the insulator, and a vapor deposition device installed in the surface analyzer forms a metal vapor deposition film on the non-covered surface of the insulator. Is characterized by. According to the above method, the insulator is not exposed to the atmosphere, so that the metal vapor deposition film is not oxidized.

According to a second aspect of the present invention, there is provided an insulator surface analysis method according to the first aspect, wherein the insulator surface control method is the same kind as the insulator on the mask piece. And depositing a metal vapor deposition film while analyzing the surface of the film thickness control insulator. By the above method, the film thickness of the metal vapor deposition film can be easily controlled.

According to a third aspect of the present invention, there is provided an insulator surface analysis method according to the first or second aspect of the present invention, wherein the sample stage is provided with a pipe through which liquid nitrogen vapor is passed. It is characterized in that the metal vapor deposition film is formed in a state in which the insulator is cooled. The above method prevents the composition and the bonding state of the insulator from changing during vapor deposition.

A surface analysis method for an insulator according to a fourth aspect of the present invention is the surface analysis method for an insulator according to any one of the first to third aspects, wherein the mask piece has an axis perpendicular to the base end. Then, by rotating this shaft, the mask piece is set on the insulating material or is removed from the insulating material.

A surface analysis method for an insulator according to a fifth aspect of the present invention is the method for surface analysis for an insulator according to any one of the first to fourth aspects, wherein the insulator on which the metal vapor deposition film is formed is It is characterized in that the surface of the insulator is analyzed after the electron shower is irradiated from the neutralizing electron gun installed in the surface analyzer.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below.
FIG. 1 is a schematic view of a surface analysis apparatus used for carrying out the analysis method of the present invention.

The present invention analyzes the surface of an insulator 3 such as ceramic by electron spectroscopy. The surface analysis apparatus used for carrying out the present invention includes an electron gun 8 for generating an electron beam, an X-ray source 9 for generating X-rays, and a sample table 17 on which the insulator 3 is placed in the analysis chamber 1. Prepare for The sample table 17 has a sample holder 7 made of stainless steel or copper on the irradiation surface, and the insulator 3 is left standing on the sample holder 7 for analysis. At the time of surface analysis, a beam generated from the electron gun 8 and the X-ray source 9 is applied to the analysis point 3a of the insulator 3 and secondary electrons generated from this analysis point 3a are detected in the analyzer 2. Detector to measure the spectrum of the energy distribution. The above surface analysis device is used in the analysis room 1.
And the vacuum pump 11 is provided connected to and operate the vacuum pump 11, the inside of the surface analysis apparatus 10 ^-9
The measurement is performed in an ultrahigh vacuum state of Torr or lower.

The surface analysis apparatus has a shaft 10 perpendicular to the sample table 17, and the shaft 10 has a horizontal support piece 1 at the upper end.
2 is provided, and the mask piece 5 is attached to the tip of this support piece. The shaft 10 has a rotatable structure,
By the rotation of the shaft 10, the mask piece 5 supported by the support piece 12 moves on the horizontal plane about the axis 10 by 180 degrees. By this rotation of the shaft 10, the mask piece 5 can be moved to a position covering the analysis place 3a of the insulator 3. Further, the vapor deposition device 6 is installed in the surface analysis device, and vaporized metal particles can be generated from the vapor deposition device 6.

A feature of the present invention is that the mask piece 5 mounted above the sample stage 17 covers the analysis place 3a of the insulator 3 and the vapor deposition device 6 installed in the surface analysis device. This is to form the metal vapor deposition film 4 on the non-covered surface 3b of the insulator 3. As the metal vapor deposition film 4,
For example, an aluminum film having a high vapor deposition rate can be given. The material of the mask piece 5 and the shaft 10 is preferably the same stainless steel or copper as the sample holder 7. The distance between the mask piece 5 and the analysis portion 3a of the insulator 3 is preferably about 2 mm. If the mask piece 5 has a disk shape with a diameter of about 3 mm, the metal deposition film 4 can be formed on the non-covered surface 3b other than the analysis site 3a without depositing the analysis site 3a. After the metal vapor deposition film 4 is formed, the mask piece 5 is removed from the insulator 3 by rotating the shaft 10, and the surface analysis is performed. As described above, according to the present invention, since the metal vapor deposition film 4 is formed in the surface analysis device, the insulator 3 is not exposed to the atmosphere. Therefore, since the metal vapor deposition film 4 is not oxidized, the charge removing effect can be maintained in a good state. As a result, the surface analysis of the present invention has good accuracy.

When forming the vapor-deposited metal film 4, as shown in FIG. 2, it is preferable to install a film thickness controlling insulator 13 of the same kind as the insulator 3 on the mask piece 5. If this film thickness control insulator 13 is installed, the film thickness control insulator 1
Since the vapor deposition can be performed while analyzing the state of the metal vapor deposition film 14 formed on the metal 3, the thickness of the metal vapor deposition film 4 of the insulator 3 can be easily controlled. The film thickness control insulator 13 may be installed by screwing it on the mask piece 5.

Further, with the insulator 3 cooled,
It is preferable to form the metal vapor deposition film 4 on the insulator 3. An analysis chamber 1 for cooling the insulator 3 is shown in FIG. As shown in the figure, a container 14 filled with liquid nitrogen is provided adjacent to the analysis chamber 1 of the surface analysis device, and vapor generated from liquid nitrogen flows through a pipe 16 connected to the container 14. The pipe 16 is in contact with the sample table 17 in the analysis chamber 1 so as to surround the sample table 17 and is connected to the pump 15. This pump 15
And the liquid nitrogen vapor is passed through the pipe 16 to move the sample stage 17 to the liquid nitrogen vapor at about −100 ° C.
Then, the insulator 3 is cooled. When the insulator 3 is cooled, it is possible to prevent the composition and bonding state of the surface of the insulator 3 from changing due to radiation heat of the insulator 3 or condensation heat of metal particles that evaporate during vapor deposition.

Further, in the X-ray photoelectron spectroscopy analyzer, it is preferable to irradiate the insulator on which the metal vapor deposition film 4 is formed after vapor deposition with an electron shower. When the electron shower is irradiated, the charge is neutralized and alleviated, so that the charge removal efficiency can be improved even if the metal vapor deposition film 4 is too thin.

[0017]

According to the surface analysis method for an insulator according to the first aspect of the present invention, since the metal vapor deposition film is formed in the surface analyzer, the insulator is not exposed to the atmosphere. Therefore, since the metal vapor deposition film is not oxidized, it is possible to maintain the charge removing effect in a good state. As a result, the surface analysis has good accuracy.

According to the insulator surface analysis method of the second aspect of the present invention, in addition to the above effects, the metal vapor deposition film is formed while analyzing the surface of the insulator for controlling the film thickness. It is possible to easily control the film thickness of the metal vapor deposition film formed on.

According to the surface analysis method for an insulator of the present invention, in addition to the above effects, since the metal vapor deposition film is formed in a state where the insulator is cooled, the insulator is vapor-deposited. It is possible to prevent the composition and the bonding state from changing, and further improve the accuracy of the surface analysis.

According to the surface analysis method of the insulator of the fifth aspect of the present invention, in addition to the above effects, particularly in the case of the X-ray photoelectron spectroscopy analyzer, the charge removal efficiency is improved even if the metal deposition film is too thin. be able to.

[Brief description of drawings]

FIG. 1 is a schematic view of a surface analysis apparatus used for carrying out the analysis method of the present invention.

FIG. 2 is a cross-sectional view showing a main part of an insulator and a mask piece.

FIG. 3 is a schematic view of an analysis room used for carrying out the analysis method of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Analysis room 2 Analyzer 3 Insulator 3a Analysis point 3b Uncoated surface 4 Metal deposition film 5 Mask piece 6 Deposition apparatus 7 Sample holder 8 Electron gun 9 X-ray source 10 Axis 11 Vacuum pump 12 Support piece 17 Sample stage

Claims (5)

[Claims] 1. When the insulator is installed on a sample stage in a surface analysis apparatus and the surface of the insulator is analyzed by electron spectroscopy, the insulator is analyzed with a mask piece mounted above the sample stage. A method for analyzing a surface of an insulating material, comprising forming a metal vapor-deposited film on a non-coated surface of the insulating material by a vapor deposition device which covers a portion and is installed in the surface analyzing device. 2. A metal vapor deposition film is formed while a film thickness controlling insulator of the same type as the said insulator is placed on the mask piece, and the surface of the film thickness controlling insulator is analyzed. The surface analysis method for an insulator according to claim 1. 3. The metal vapor deposition film is formed while the sample stage is cooled through a pipe through which liquid nitrogen vapor is passed, and the insulator is cooled.
A method for analyzing the surface of an insulating material as described above. 4. The mask piece has an axis perpendicular to the base end,
4. The surface analysis method for an insulator according to claim 1, wherein the mask piece is installed on or removed from the insulator by rotating the shaft. . 5. The surface analysis of the insulator is performed after irradiating the insulator having the vapor deposited metal film with an electron shower from a neutralizing electron gun installed in the surface analyzer. The surface analysis method for an insulator according to any one of claims 1 to 4.