JPS634997Y2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sample processing device for an electron microscope, etc., which can coat a sample surface immediately after treatment with a reactive gas.

When performing morphological observation or elemental analysis of a sample using an electron microscope, especially a scanning electron microscope or an Coating with a thin film is often necessary. Conventional processing equipment includes etching equipment, ashing equipment, etc., and the sample processed in these equipment is once removed from the equipment, inserted into a vacuum evaporation equipment, and the surface is coated. This method of once removing the sample from the processing apparatus and inserting it into the vapor deposition apparatus results in the etched or cleaned sample becoming contaminated when it is taken out into the atmosphere. In particular, in the case of incineration treatment, the incinerated biological sample is very fragile, so deformation of the sample during movement is a major problem.

The purpose of the present invention is to solve these drawbacks, by placing a sample in an airtight chamber, introducing an arbitrary gas into the airtight chamber, ionizing it and reacting with the sample, and etching or etching the sample. In an apparatus for performing ashing, an auxiliary chamber is provided through a rotatable partition wall, a coating material particle generation means is provided in the partition wall, and the coating material particle generation means is sealed in the auxiliary chamber by rotation of the partition wall. The sample processing apparatus for an electron microscope or the like is characterized in that it can be switched between the position of the sample and the position facing the sample.

An embodiment of the present invention will be described below with reference to the accompanying drawings. In the figure, reference numeral 1 denotes an airtight chamber, which is connected to a vacuum pump 4 via a pipe 2 and a valve 3, so that the interior can be evacuated to a high vacuum. In addition, there is a pipe 5 in this airtight room.
A gas cylinder 7 is connected through a valve 6, and a gas necessary for processing, for example, oxygen gas in the case of ashing processing, is introduced into the airtight chamber at a predetermined flow rate. The exhaust pipe 2 is installed at the center of the bottom plate of the airtight chamber 1, and the gas introduction pipe 5 is installed at the end of the bottom plate or the side of the airtight chamber. A shield tube 8 having a slit is provided. A sample stage 9 is placed inside the shield tube, and a sample 10 is placed on it.
Reference numeral 11 denotes a high frequency coil, which is wound around the outer periphery of the lower part of the airtight chamber 1 and is connected to a high frequency oscillator 12. 13 is adjacent to the airtight chamber and sample 10
An auxiliary room located opposite the pipe 14,
connected to a vacuum pump 16 via a valve 15;
The gas inside can be discharged. Reference numeral 17 denotes a partition wall provided between the airtight chamber and the auxiliary chamber, which is plate-shaped and has a shaft 18.
It is configured to be able to rotate at least 180 degrees around , as shown by the arrow. A heater 19 is provided on one side of the partition wall to heat and evaporate the coating material 20.

In such a configuration, the partition wall 17 is first aligned with the arrow A.
The evaporation source (heater 19) is sealed in the auxiliary chamber 13, the valve 3 is opened with the sample 10 placed on the sample stage 9, and the inside of the airtight chamber 1 is evacuated by the vacuum pump 4. While maintaining this exhaust state, the valve 6 is opened and oxygen gas is introduced into the airtight chamber from the cylinder 7. Next, when high-frequency power is supplied from the high-frequency oscillator 12 to the high-frequency coil 11, the electromagnetic field generated by the coil ionizes the oxygen gas introduced into the airtight chamber, forming a plasma atmosphere. This plasma generation region is a cylindrical region between the shield tube 8 and the side wall of the airtight chamber because the shield tube 8 is provided and the gas introduction port is outside the shield tube. Oxygen ions in this plasma enter the inside of the shield cylinder 8 through the slit by being evacuated by the vacuum pump 4, come into contact with the sample 10, and cause a reaction. Gases that did not contribute to the reaction and gases newly generated by the reaction are discharged to the outside by the pump 4. Due to the reaction with the oxygen ions, the biological sample is incinerated while maintaining its original shape, and elements such as metals remain intact. When the ashing process is completed, close the valve 6 to stop the gas introduction and let the inside of the airtight chamber 1 clear.
Evacuate to high vacuum of 10 ^-3 Torr or higher. At the same time, the valve 15 is opened to exhaust the inside of the auxiliary chamber 13 as well. When both chambers reach a predetermined degree of vacuum, the partition 17 is rotated in the direction of arrow B, the heater 19 and the coating material 20 are made to face the sample 10, and then the heater is energized to heat the coating material 20. Let it evaporate. These evaporated particles were scattered and turned into ashes in sample 10.
It adheres to the surface and forms a thin coating film. Once the film has been formed to a predetermined thickness, the power supply to the heater 19 is stopped, the valves 3 and 15 are closed, and the atmosphere is further leaked inside to take out the sample. The extracted sample is immediately mounted on a sample stage of a scanning electron microscope, etc., and morphological observation and elemental analysis are performed.

Note that the sample can be cleaned by using hydrogen gas instead of oxygen gas, and the sample can be etched by using Freon gas. Which of these is used is appropriately selected depending on the processing purpose.

With the configuration described in detail above, processing such as ashing and etching and coating of a thin film on the surface of the sample can be performed while the sample is placed in a fixed position. This prevents damage to the sample.

Furthermore, since the coating material is sealed in the auxiliary chamber during the ashing process, it is not exposed to the low vacuum state or reaction gas atmosphere during the ashing process, and thus remains clean. That is, the purity of the coating material is maintained. Furthermore, by rotating the partition wall during vapor deposition so that the heater and coating material face each other, the evaporation source and the sample can be brought closer together, making it possible to shorten the vapor deposition time and prevent the sample from being destroyed by the radiant heat of the heater. It can be prevented.

[Brief explanation of the drawing]

The accompanying drawings are schematic diagrams showing one embodiment of the present invention. 1: Airtight chamber, 4: Vacuum pump, 7: Gas cylinder, 8: Shield cylinder, 10: Sample, 11: High frequency coil, 12: High frequency oscillator, 13: Auxiliary room, 1
7: Partition wall, 19: Heater, 20: Coating material.

Claims (1)

[Scope of utility model registration request] an airtight chamber, a sample placed in the airtight chamber, and means for introducing a desired gas into the airtight chamber;
An apparatus for processing the sample by collision or reaction of the ionized gas, comprising a pump for evacuating the airtight chamber and a means for ionizing the gas in the airtight chamber, the auxiliary chamber being connected to the auxiliary chamber via a rotatable partition wall. A coating material particle generating means is provided on the partition wall, and by rotation of the partition wall, the coating material particle generating means can be switched between a state in which it is enclosed in the auxiliary chamber and a state in which it is placed in a position facing the sample. A sample processing device for an electron microscope, etc., characterized by: