JPH0637315Y2 - Charged sample table for diffraction measurement - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial field of application) The present invention relates to a sample stage for diffraction measurement such as X-ray diffraction and neutron diffraction, and particularly to performing such diffraction measurement while applying an electric field to the sample. The present invention relates to a sample table that can be used.

(Prior Art) In the study of a substance whose crystal structure is changed by an external electric field, conventionally, after subjecting a sample to an electric field treatment, the sample is subjected to X-ray irradiation.
It was installed in a line diffractometer and used for X-ray diffraction measurement.

(Problems to be Solved by the Invention) In order to dynamically pursue such a mechanism of electric field-induced phase transition, it is desirable that the electric field treatment of the sample and the X-ray diffraction measurement be performed at the same time. Since the sample must be in line with X-ray diffraction techniques, the sample must be subjected to an electric field treatment while installed in the goniometer head. However, a device satisfying such a demand has not been known so far.

It is an object of the present invention to provide a sample stage that can perform diffraction measurement while applying an electric field to a sample in a diffracting apparatus such as X-ray diffraction and neutron diffraction.

(Means for Solving the Problems) The charged sample holder for diffraction measurement of the present invention will be described with reference to the drawings showing an embodiment, and it is fixed on the top of the goniometer head 6 for diffraction measurement and together with the goniometer head 6. The rotating base member 2 and the plate-shaped sample 14 fixed to the base member 2 and having the electrode layers 50 and 52 formed on the front and back surfaces are positioned on the central axis of rotation of the goniometer head 6 with at least one end sandwiched therebetween. Sample supporting members 10 and 12 to be supported by the sample supporting members 10 and 12 and a pair of electrode terminals 2 for contacting both electrode layers 50 and 52 of the sample 14 supported by the sample supporting members 10 and 12 and applying a voltage between both electrode layers 50 and 52
0, 24, 22, and 26 are provided.

(Example) The figure shows an example in which the present invention is applied to an X-ray diffraction sample stage.

Reference numeral 2 denotes a base member, which is made of an electrically insulating material such as polytetrafluoroethylene or α-alumina and has a dish-shaped upper portion. A fixing projection 4 is provided on the bottom surface of the base member 2, and the projection 4 is inserted into a goniometer head 6 of the X-ray diffraction apparatus and fixed by a screw 8.

Reference numerals 10 and 12 are a pair of sample fixing upper and lower chucks serving as sample support members, and the lower chuck 12 is fixed in the recess of the base member 2. Sample 14 is both chucks 10,1
It is held between two and fixed by screws 16 and 18. The upper chuck 10 can be moved in the vertical direction. For example, when the sample 14 is a thin film polymer,
14 can be extended.

A pair of electrodes 20, 22 are embedded in the side wall of the base member 2,
One end of each of the electrodes 20 and 22 projects into the recess of the base member 2, and internal leads 24 and 26 are connected to each by soldering. Film electrodes 50, 52 such as aluminum vapor-deposited films are formed on both surfaces of the sample 14 for applying an electric field, and the tips of the internal leads 24, 26 are formed by the film electrodes 5 of the sample 14.
It is designed to be fixed to 0,52 with silver paste.
Further, the other ends of the electrodes 20 and 22 project from the side wall of the base member 2 to the outside, the external leads 28 and 30 are connected to them, and a voltage is applied between the external leads 28 and 30. This electrode structure can apply a strong electric field of several tens to several tens of MV / cm to the sample 14.

The concave portion of the base member 2 is filled with insulating oil 32, and the inner lead 2
It is possible to immerse 4,26 and the fixed portions of them and the film electrodes 50, 52 on the surface of the sample 14 in the insulating oil 32.

Heater wires 34 and 36 are attached to the chucks 10 and 12 for fixing the sample, respectively.
Is wound, and the sample 14 is heated by heat conduction from the chucks 10 and 12 to the sample 14. 38,40
Is a thermocouple for controlling energization to the heater wires 34, 36, which are brought into contact with the upper chuck 10 and the lower chuck 12, respectively. Reference numeral 42 is a thermocouple for measuring the temperature of the sample 14, and a ceramic coating 44 is applied to the tip of the thermocouple to avoid air discharge with the film electrode of the sample.

To perform X-ray diffraction measurement using this sample table, the sample 14 is fixed between the chucks 10 and 12, and the internal leads 24 and 26 are attached to the sample 14.
After being fixed to the film-shaped electrodes 50 and 52, a predetermined voltage is applied between the external leads 28 and 30, the X-ray 46 is made incident on the sample 14, and the diffracted X-ray 48 is detected.

When a high electric field is applied to the sample 14, the insulating oil 32 is filled in the concave portion of the base member 2. As a result, it is possible to suppress the discharge in the air due to the high electric field.

When the sample 14 is further heated to measure the X-ray diffraction, the sample is controlled while controlling the amount of electricity to the heater wires 34 and 36 so that the temperature difference detected by the thermocouples 38 and 40 becomes zero. Heat 14 By heating the sample 14, the activation energy of the electric field-induced phase transition is lowered, and the electric field threshold value of the phase transition can be reduced.

In the above embodiment, the case where the present invention is used for the X-ray diffraction measurement is illustrated, but it can be applied to the case where it is used for the neutron diffraction measurement, for example.

(Effects of the Invention) By using the charged sample stage for diffraction measurement of the present invention, it becomes possible to simultaneously perform the electric field application and the diffraction measurement. It is particularly convenient for studying relaxation times of phase transitions, activation energies and kinetics such as multistage transitions.

[Brief description of drawings]

FIG. 1 is a sectional view showing an embodiment of the present invention. 2 ... Base member, 6 ... Goniometer head, 10, 12
…… Sample fixing chuck, 14 …… Sample, 20,22 …… Electrode, 24,26 …… Internal lead, 28,30 …… External lead.

Claims (1)

[Scope of utility model registration request] 1. A base member fixed to the top of a goniometer head for diffraction measurement and rotating together with the goniometer head, and at least a plate-shaped sample fixed to this base member and having electrode layers formed on the front and back surfaces thereof. A sample support member which holds one end portion of the sample and which is positioned and supported on the central axis of rotation of the goniometer head, and a pair of contacting both electrode layers of the sample supported by the sample support member and applying a voltage between both electrode layers A charged sample table for diffraction measurement, which includes an electrode terminal.