JPH07234184A - Glow discharge emission spectrophotometer - Google Patents

Abstract

PURPOSE:To provide a glow discharge emission spectrophotometer which can accurately analyze even a sample where the entire surface containing an analysis surface is a thin recessed and projecting surface and a porous surface with a simple configuration. CONSTITUTION:A liquid-shaped resin 7 is applied to a surface including a contact surface with at least a seal member 6 and is cured at the outer periphery of an analysis surface 5c of a sample 5. The sample 5 is pressed against the lower part of the glow discharge space of a glow discharge tube 10 by allowing the resin 7 to contact the seal member 6. The resin 7 which is in a completely smooth surface in a liquid-shaped application positively contacts the seal member 6 in airtight state and positively closes the inner glow discharge space by the sample 5.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a glow discharge optical emission spectrometer for analyzing generated light while sputtering a sample.

[0002]

2. Description of the Related Art In an argon (Ar) atmosphere having a gas pressure of about 4 to 10 Torr, when a high voltage of direct current or high frequency is applied between two electrodes, glow discharge occurs and Ar ions are generated. The generated Ar ions are accelerated by a high electric field, collide with the cathode surface, and knock out the substances present therein. This phenomenon is called sputtering. Sputtered particles (atoms, molecules, ions) are excited in plasma and emit light of a wavelength peculiar to the element when returning to the ground state. An analysis method of spectrally analyzing the emitted light with a spectroscope to identify an element is called a glow discharge emission spectral analysis method.

As a glow discharge tube in an analyzer that embodies the glow discharge emission spectral analysis method described above, a hollow anode type grim glow discharge tube 1 as shown in FIG. 5 is generally used. In this grim glow discharge tube 1, a support block 2 serving as a cathode and an anode block 3 are joined via a Teflon washer 4 which is an insulator. The anode block 3 has an argon gas supply hole 3a and first and second vacuum exhaust holes 3b and 3c, and the inside V of the tube is a rare gas atmosphere of argon (4 to 10 Torr). A hollow anode tube 3d is formed integrally with the anode block 3, and the anode tube 3d penetrates the Teflon washer 4 and is close to the surface 5a of the sample 5. This sample 5
An annular O surrounding the analysis surface on the surface 5a
It is pressed against the support block 2 in an airtight state via a seal member 6 such as a ring.

In this Grimm glow discharge tube 1, a high voltage is applied between an anode block 3 and a support block 2 by a power source section 9 to generate a glow discharge, and a sample 5 is passed through a support block 2 generally made of copper. Apply a negative voltage,
Argon cations generated by the generation of glow discharge collide with the surface 5a of the sample 5 to sputter the sample 5. Further, the cooling liquid K is introduced from the cooling liquid introduction passage 2a of the support block 2 into the jacket 2b and fed to the cooling liquid discharge passage 2c, thereby cooling the sample 5 and the hollow anode tube 3d through the support block 2. are doing.

[0005]

By the way, in the above-mentioned glow discharge emission spectroscopy analyzer, the surface 5a of the sample 5 is vacuum-sealed by the seal member 6 embedded in the support block 2 to make the support block 2 airtight. The sample 5 is pressed to close the inner space (glow discharge space) of the support block 2 that houses the hollow anode tube 3d, and the inner space is evacuated. Therefore, the sample 5 to be analyzed needs to have a flat surface 5a including the analysis surface facing the inner space, and the surface 5a needs to have a roughness that allows airtight contact with the annular seal member 6. There is.

However, even if the sample 5 has a flat surface 5a, normal analysis becomes impossible if the surface 5a is as follows. That is, as shown in FIG. 6, for example, the surface condition is such that fine irregularities 5b are present at a cycle of a micron unit, or the surface 5a is porous, or a surface treatment having poor airtightness is applied. For the sample 5 as shown in FIG.
It is not possible to bring a into contact with the support block 2 via the O-ring 6 in a completely airtight state. Therefore, when the inner space is evacuated, as shown by the arrow in FIG.
Vacuum leakage occurs from a slight gap between the surface 5a of the and the O-ring 6, and normal analysis cannot be performed.

Therefore, the present invention provides a glow discharge emission spectroscopic analyzer capable of accurately performing analysis with a simple structure even for a sample having a fine uneven surface or a porous surface on the entire surface including the analysis surface. That is the purpose.

[0008]

In order to achieve the above object, in the glow discharge emission spectroscopy analyzer according to the present invention, a sample is pressed against the lower part of the glow discharge space of a glow discharge tube via a seal member. In such a glow discharge emission spectroscopic analyzer, a liquid resin is applied and cured on a surface including at least a contact surface with the seal member on the outer periphery of the analysis surface of the sample.

[0009]

For example, when the sealing member is an O-ring having a diameter larger than the outer circumference of the analysis surface of the sample, the liquid resin is applied to the surface of the sample along the outer circumference of the analysis surface corresponding to the shape of the O-ring. The ring-shaped resin, which is surrounded and applied in a ring shape, is brought into contact with the O-ring, and the surface of the sample is pressed against the lower portion of the glow discharge tube. Therefore, even in the case of a sample in which the entire surface including the analysis surface is a fine uneven surface or a porous surface, the resin, which is a completely smooth surface due to being applied in a liquid state, can be reliably attached to the O-ring. Since they contact each other in an airtight state, the sample is pressed against the lower part of the glow discharge tube via the resin and the O-ring to reliably seal the inner glow discharge space. Further, the analysis surface on the inner side of the annular resin on the surface of the sample faces the glow discharge space as it is without being covered with the resin, so that the analysis of this sample can be performed without any trouble.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT A preferred embodiment of the present invention will be described below with reference to the drawings. As shown in FIG. 1, a glow discharge emission spectroscopic analyzer according to an embodiment of the present invention emits light of a wavelength peculiar to an element by sputtering using glow discharge, and is emitted from a grim glow discharge tube 10.
The light L transmitted through the window plate 13 enters the spectroscope 15. The spectroscope 15 measures the incident slit 14, the diffraction grating 16 that diffracts the light L incident from the incident slit 14 at different diffraction angles according to the wavelength, the exit slit 17 that allows the diffracted light to pass, and the intensity of the diffracted light. Photomultiplier tube 1
Eight.

FIG. 2 shows an example of the Grim glow discharge tube 10 in the analyzer of FIG. 2, the same parts as those in FIG. 5 are designated by the same reference numerals. The difference is that, as clearly shown in FIG. 3 which is an enlarged view of an essential part of FIG. 2 and FIG. 4 which is a perspective view of the sample 5, the analysis surface 5c of the surface 5a of the sample 5 on which the fine unevenness 5b exists is present. The liquid resin 7 is applied and cured on the annular surface surrounding the outer periphery of the sample 5
However, only the structure in which the resin 7 is brought into contact with the seal member 6 of FIG. 2 and pressed against the support block 2.

As the resin 7, a resin which does not have tackiness after being hardened, for example, an adhesive such as an epoxy type or Aron Alpha (trademark), or polyethylene which is heated and melted is used. 2 to 4
As shown in FIG. 4, in this embodiment, in order to save the usage amount of the resin 7, the resin 7 is applied in an annular shape so as to correspond to the shape of the seal member 6 in a precise manner. Therefore, when it is difficult or troublesome to apply the resin 7 in such a shape, the resin 7 may be applied to almost the entire outer portion of the outer periphery of the analysis surface 5c of the surface 5a of the sample 5. That is, the resin 7 may be applied to the surface of the surface 5a of the sample 5 excluding the analysis surface 5c, including at least the entire contact surface with the seal member 6.

Since the resin 7 is applied to the sample 5 in a liquid state, as shown in FIG. 3, it enters the fine irregularities 5b of the sample 5 so as to fill it. Further, when the surface 5a of the sample 5 is porous, it enters so as to be embedded in the fine pores. If the sample 5 is held in a horizontal state at the time of applying the resin 7, the applied resin 7 becomes an accurate smooth surface along the surface 5a due to its own property, and retains this shape and cures.

Therefore, as shown in FIG. 3, the smooth surface of the annular resin 7 is pressed against the seal member 6 and comes into contact with it in a reliable airtight state, so that the sample 5 passes through the resin 7 and the seal member 6. The inner space of the glow discharge tube 10 is pressed against the support block 2 with certainty.
The analysis surface 5c on the inner side of the annular resin 7 on the surface of the sample 5 faces the glow discharge space as it is.
Therefore, even if the analysis surface 5c is the sample 5 having an uneven surface or a porous surface, the analysis can be normally performed.

Next, the operation of the above configuration will be described. Figure 2
Between the support block 2 and the anode block 3 of the power source unit 9
When a high voltage of several hundred to several thousand volts is applied, a glow discharge is generated and argon cations are generated. The generated Ar ions collide with the analysis surface 5c of the sample 5, which is the cathode, and sputter the analysis surface 5c. As a result, the atoms knocked out from the analysis surface 5c of the sample 5 and peeled off are excited by Ar ions or electrons, and emit light specific to the element when returning to the ground state again. This light L
Passes through the window plate 13 and goes toward the diffraction grating 16 of the spectroscope 15 through the entrance slit 14 of FIG. The diffractive grating 16 diffracts light of a predetermined wavelength, and the exit slit 17
To enter the photomultiplier tube 18. The photomultiplier tube 18 measures the intensity of the incident light.

[0016]

As described above, according to the glow discharge emission spectroscopy analyzer of the present invention, the liquid resin is applied to the outer periphery of the analysis surface of the sample, at least the surface including the contact surface with the seal member. Since it has been hardened, the resin that has a completely smooth surface due to being applied in liquid form
Since it contacts the sealing member in a reliable airtight state, even if the sample including the analysis surface is a fine uneven surface or a porous surface, this sample is applied to the glow discharge tube through the resin and the sealing member. By pressing it to the lower part, it is possible to securely seal the inner glow discharge space with the sample, and since the analysis surface of the sample faces the glow discharge space as it is,
The above-mentioned sample analysis can be performed accurately without any trouble. Further, there is an advantage that the above analysis can be achieved with a simple and inexpensive structure in which a resin is applied to a sample and then cured.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram of an analyzer according to an embodiment of the present invention.

FIG. 2 is a cross-sectional view showing an example of a Grimm glow discharge tube according to the same analyzer.

FIG. 3 is an enlarged view of a main part of the above discharge tube.

FIG. 4 is a perspective view of a sample used in the same apparatus.

FIG. 5 is a cross-sectional view of a Grim glow discharge tube in a conventional analyzer.

FIG. 6 is a cross-sectional view showing a state in which a sample having fine irregularities on its surface is pressed against the same discharge tube.

[Explanation of symbols]

5 ... sample, 5c ... analysis surface of sample, 6 ... sealing member, 7 ...
Resin, 10 ... glow discharge tube.

Claims (1)

[Claims] 1. A glow discharge emission spectroscopic analyzer in which a sample is pressed under a glow discharge space of a glow discharge tube via a seal member, wherein at least the contact surface with the seal member at the outer periphery of the analysis surface of the sample. A glow discharge emission spectroscopic analyzer in which a liquid resin is applied and cured on the surface containing the resin.