JPS60189853A - Device for replacing the sample - Google Patents

Abstract

PURPOSE:To improve the operation efficiency of a device for replacing the sample by equipping the device with a replacement pipe and a sample bar so that attachment, preliminary exhaustion, installation at the analysis position, aeration and removement of several samples can be performed parallel and continuously. CONSTITUTION:A device for replacing the sample is constituted of a sample replacement pipe 5 and a sample bar 12 which slides in the pipe 5 to replace the sample. The sample pipe 5 has an opeing corresponding to the analysis position located in the vacuum case of the analyzer. The sample bar 12 is equipped with sample attachment sections 13 located at given intervals. The figure indicates the stage when sample (A) is undergoing analysis, sample (B) is undergoing aeration before being removed, sample (C) is undergoing preliminary exhaustion and sample (D) is being attached to the sample bar 12. When the sample bar 12 is moved by one pitch after analysis of sample (A) is finished, sample (C) already undergoing preliminary exhaustion moves to the analysis position, sample (D) undergoes preliminary exhaustion and sample (A) is subjected to aeration and removed. Therefore, it is possible to make only time for moving the sample necessary, thereby improving the operation efficiency of the device.

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-exhausted, in which the sample stage and other analyzers are exchanged. A method is used in which the sample loaded into the main body and analyzed is temporarily stored, 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 main body of the analyzer. ing. 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 installation of a large number of samples, preliminary evacuation, setting to analysis positions, suction, and removal of multiple samples to be performed continuously and in parallel, thereby eliminating the need for any time other than the time for moving the samples. The object of the present invention is to provide a sample exchange device that improves the operating rate of the system and improves the efficiency of analysis.

(Tsunari) 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.

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.
An electron beam irradiation system 4 that irradiates an electron beam 3 to the sample 2, an electron beam detector that detects secondary electron beams from the sample 2, and an X-ray spectroscopic detector that detects characteristic X-rays (not shown in the figure) A system is set up.

5 is a sample exchange pipe, which exchanges X, Y,
It is fixed to a sample stage 6 that can move in the Z direction, and there is a bellows 7 between the outer periphery of the sample exchange pipe 5 and the vacuum container 1.
Vacuum sealing is performed movably. An opening 8 is provided in the sample exchange pipe 5 at an 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 extracted. 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 a sample 2 is set in each sample attachment portion 13. It is supposed to be done.

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. The sample mounting part 13 in front of the sample mounting part 13 is set to be at the exhaust port 9.

Additionally, an O-ring groove 14 is provided between adjacent sample mounting parts 13.
is provided, 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 inhaled/removing the sample, sample C is being analyzed.
is in the process of preliminary evacuation, and the sample holder is in the process of mounting the sample, and operations at each stage are being carried out in parallel.

Next, when the analysis of sample A is completed, by moving the sample rod 12 by one pitch in the direction of the arrow, sample C, which has completed preliminary evacuation, moves to the analysis position, the sample chamber is preliminarily evacuated, and sample A It becomes inhaled and taken out.

Thereafter, in the same manner, every 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 l. 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) In the sample exchange device of the present invention, analysis, preliminary evacuation, sample attachment, and removal are performed in parallel, and the time required for sample exchange is only the time required to move the sample rod one pitch. This has the effect of improving the operating efficiency of the device and significantly improving analysis efficiency.

[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
...0 ring. Agent Patent Attorney Shigeo Noguchi

Claims (1)

[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 a preliminary exhaust means at a position a predetermined distance from the opening; Sample mounting sections are provided at intervals corresponding to a predetermined distance,
A sample exchange device 6 comprising: a sample rod that slides in the sample exchange pipe in an airtight manner;