JPH0574182B2 - - Google Patents

Description

Detailed Description of the Invention (Industrial Field of Application) The present invention relates to a sample exchange device for an analyzer that is equipped with a vacuum body and uses a charged particle beam, such as an X-ray microanalyzer, an ion microanalyzer, or a scanning electron microscope. It is related to.

(Prior art) Conventionally, sample exchange in the above-mentioned analyzers has been carried out by exposing the entire apparatus to the atmosphere, or by providing a single sample exchange chamber that is pre-evacuated. The sample that has been loaded into the analyzer and analyzed is stored once, the sample exchange chamber is exposed to the atmosphere, the sample is taken out, a new sample is loaded, preliminary evacuation is performed, and then the sample is loaded into the analyzer itself. There is. However, in either case, sample exchange is performed as a series of operations, so there is a problem in that sample exchange takes time and reduces analysis efficiency.

(Purpose) The present invention enables the mounting, preliminary evacuation, setting of analysis positions, suction, and removal of multiple samples to be performed continuously and in parallel, eliminating the need for any time other than the time required for moving the samples. improve the operating rate of the equipment,
The object of the present invention is to provide a sample exchange device that increases analysis efficiency.

(Structure) The present invention is a sample exchange device for an analyzer using a charged particle beam, and is composed of a sample exchange pipe and a sample rod that slides inside the pipe to exchange the sample. The sample exchange pipe has an opening at the analysis position within the vacuum container of the analyzer main body, and is provided with preliminary exhaust means at a predetermined distance from the opening. On the other hand, sample attachment portions are provided on the sample rod at intervals corresponding to the predetermined distance, and airtightness is maintained between the sample rod and the sample exchange pipe. The sample rod moves in one direction from the pre-evacuation means side toward the analysis position.

Hereinafter, the present invention will be explained in detail with reference to Examples.

(Example) The figure shows an example in which the present invention is applied to an analysis device such as an X-ray microanalyzer, and the vacuum vessel 1 of the device body includes an electron beam irradiation system 4 that irradiates a sample 2 with an electron beam 3. Although not shown, an electron beam detector for detecting secondary electron beams etc. from the sample 2 and an X-ray spectroscopic detection system for detecting characteristic X-rays are provided.

Reference numeral 5 denotes a sample exchange pipe, which is fixed to a sample stage 6 that can move in the X, Y, and Z directions with respect to the electron beam 3. A bellows 7 allows the pipe to move between the outer periphery of the sample exchange pipe 5 and the vacuum vessel 1. Vacuum sealed. An opening 8 is provided in the sample exchange pipe 5 at the analysis position where the electron beam is irradiated onto the sample 2 and the secondary electron beam and characteristic X-rays from the sample 2 are taken out. An exhaust port 9 for exhaust is opened, and this exhaust port 9 is constantly evacuated by a vacuum pump 11 via a vacuum pipe 10.

A sample rod 12 is slidably inserted inside the sample exchange pipe 5, and the sample rod 12 is provided with sample attachment portions 13 at regular intervals, and each sample attachment portion 13 has a sample 2 set therein. It is becoming more and more common.

The interval between the sample attachment parts 13 of the sample rod 12 corresponds to the interval between the opening 8 of the sample exchange pipe 5 and the preliminary exhaust outlet 9, and when one of the sample attachment parts 13 is at the position of the opening 8. Sample mounting part 13 in front of it
is set to be at the position of the exhaust port 9.
Further, an O-ring groove 14 is provided between adjacent sample mounting portions 13, and an O-ring 15 is fitted therein to vacuum-seal the inside and outside of the vacuum container 1.

To explain the operation of this embodiment, in the state shown in the figure, sample A is being analyzed, sample B is being sucked in and taken out, sample C is being pre-exhausted, and sample D is being attached. are being carried out in parallel.

Next, when the analysis of sample A is completed, the sample rod 12
By moving by one pitch in the direction of the arrow, sample C, which has been pre-evacuated, is moved to the analysis position, sample D is pre-evacuated, and sample A is taken out after being inhaled.

Thereafter, in the same manner, each time the analysis of the sample at the analysis position is completed, the sample is replaced by simply moving the sample rod 12 by one pitch. Therefore, the time required for sample exchange is only the time required to move the sample rod 12 by one pitch.

In this embodiment, the sample rod 12 is only moved unidirectionally in the direction of the arrow, so for example, if new sample rods 16 are added using the screwing means 17, several samples can be analyzed in succession. You will be able to do this.

Further, if the preliminary exhaust port 9 is also provided in the sample extraction direction (on the left side in the figure) and the sample rod 12 is moved back and forth, repeated analyzes can be continued using one sample rod 12.

The embodiment shown in the figure is equipped with a sample stage 6, and the sample position can be moved, so a bellows 7 is used to movably vacuum seal the space between the sample exchange pipe 5 and the vacuum container 1. There are also devices such as scanning electron microscopes that do not require moving the sample position. In such a case, the space between the sample exchange pipe 5 and the vacuum container 1 may be fixed and vacuum sealed.

(Effects) The sample exchange device of the present invention can perform analysis, preliminary evacuation,
The sample is installed and removed in parallel, and the time required to exchange the sample is only the time required to move the sample rod one pitch, which improves the efficiency of moving the analysis position and greatly improves the effectiveness of the analysis. There is.

[Brief explanation of the drawing]

The figure is a sectional view showing one embodiment of the present invention. 1... Vacuum container of the analyzer main body, 2... Sample,
5...Sample exchange pipe, 8...Opening, 9...Exhaust port for preliminary exhaust, 12...Sample rod, 13...Sample attachment part, 15...O ring.

Claims (1)

[Scope of Claims] 1. In an analyzer using a charged particle beam, a sample exchange pipe having an opening at an analysis position in a vacuum container of the analyzer main body and having preliminary exhaust means at a predetermined distance from the opening. and a plurality of sample attachment parts are provided at intervals corresponding to the predetermined distance to hold the analysis sample, and slide in the sample exchange pipe in an airtight manner from the preliminary exhaust means side toward the analysis position. a sample rod that can be moved in one direction, and analysis of a sample held in a sample holder positioned at the analysis position;
A sample exchange device characterized in that preliminary evacuation of a sample held in a sample mounting section positioned at the preliminary evacuation means position and mounting of the sample on the sample mounting section outside the sample exchange pipe are performed at the same time.