JP3437400B2 - Sample stage with controllable sample temperature - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technical field of a sample stage for holding a sample to be measured, which is used in an electron spectroscope in an ultrahigh vacuum such as a photoelectron spectroscope and an Auger electron spectroscope. It belongs to the technical field of a sample stage capable of controlling a sample temperature, which is capable of cooling and heating to a predetermined temperature while holding a sample to be measured in a high vacuum.

[0002]

2. Description of the Related Art Conventionally, when a sample is irradiated with X-rays in an ultra-high vacuum, a photoelectric effect device for analyzing the elements of the sample by measuring the energy level of photoelectrons emitted from the sample by photoelectric effect and in an ultra-high vacuum. In an Auger electron spectrometer that measures the energy level of Auger electrons emitted from a sample when the sample is irradiated with an electron beam and analyzes the elements of the sample, the sample must be cooled to a predetermined temperature in an ultrahigh vacuum. Measurements are being made.

FIG. 2 is a diagram schematically showing an example of a conventional coolable sample stage for holding the sample in a cooled state when measuring the sample in a cooled state. In the figure, 1 is a coolable sample stage, 2 is a sample to be measured, 3 is a sample holder for holding the sample to be measured, 4 is integrally attached to the sample holder 3, and nitrogen gas is provided at the bottom. A refrigerant tank 5 into which a refrigerant such as is introduced is provided integrally with the refrigerant tank 4, and a heat transfer member that transfers the cold heat of the refrigerant in the refrigerant tank 4 to the measured sample 2 to cool the measured sample 2, 6 Is a stainless steel spiral tube for introducing and discharging the refrigerant in the refrigerant tank 4, and 7 is an in-plane rotation of the sample holder 3, the refrigerant tank 4, and the heat transfer body 5 integrally (rotation around the vertical axis in FIG. 2). ) The sample holder in-plane rotation gear, 8 is the in-plane rotation transmission gear that transmits in-plane rotation torque to the sample holder in-plane rotation gear 7, and 9 is the rotation that imparts rotation torque in the φ direction to the in-plane rotation transmission gear 8. Torque imparting axis, 10 The material holder in-plane rotating gear 7 is rotatably supported and the in-plane rotating torque imparting shaft 9 is rotatably supported, and can be further moved in the left-right direction (X direction) by a left-right direction moving operation member (not shown). It is a sample holder support.

Sample holder 3, heat transfer body 5, and refrigerant tank 4
Are integrally formed with each other, and the rotational torque is transmitted from the in-plane rotary gear 7 of the sample holder. Further, most of the refrigerant tank 4 and the heat transfer body 5 are arranged in the cylindrical rotary shaft 3 a of the sample holder 3 and the cylindrical rotary shaft 7 a of the sample holder in-plane rotary gear 7.

Then, the sample 2 to be measured is held on a coolable sample stage 1 in the electron spectroscope, the inside of the electron spectroscope is brought to an ultrahigh vacuum state, and it is cooled to a predetermined temperature in, for example, liquid nitrogen. A refrigerant such as nitrogen gas is introduced into the refrigerant tank 4 through the spiral tube 6. The sample 2 to be measured is cooled to a predetermined temperature via the heat transfer body 5 by the cold heat of the refrigerant in the refrigerant tank 4. In this state, by irradiating with an X-ray or an electron beam and measuring the energy level of electrons emitted from the sample to be measured 2 in a state of being cooled to a predetermined temperature in an ultrahigh vacuum, the elements of the sample to be measured 2 are measured. Is analyzed. In that case, the irradiation position of the X-ray, the electron beam, or the like on the measured sample 2, that is, the measurement point of the measured sample 2 is the movement of the sample holder support 10 in the X direction by the lateral movement operation member and the in-plane rotational torque imparting axis. It is changed and set by the in-plane rotation of the sample holder in-plane rotating gear 7 by 9. That is, the emission characteristics of the measured sample 2 such as photoelectrons and Auger electrons are measured with respect to the polar coordinates by the azimuth angle and the polar angle.

By using the spiral tube 6 as an introducing pipe for introducing the refrigerant into the refrigerant tank 4, the introducing pipe is made flexible to have a degree of freedom for in-plane rotation of the refrigerant tank 4. It is possible to rotate.

[0007]

By the way, in the conventional coolable sample stage 1, it is possible to rotate the sample 2 to be measured in-plane up to about 0 to 100 degrees by the degree of freedom based on the spiral tube 6. However, since the spiral tube 6 is connected to the refrigerant tank 4, it is impossible to endlessly rotate the sample 2 to be measured in-plane. Therefore, with the in-plane rotation of the sample 2 to be measured within this possible range, it is difficult to measure the emission spectral characteristics of photoelectrons, Auger electrons, etc. for all polar angles and all azimuth angles.

Therefore, it is desired that the sample 2 to be measured can be endlessly in-plane rotated so that all the measurement points of the sample 2 to be measured can be easily set to the irradiation positions of X-rays, electron beams, and the like. . In particular, the endless in-plane rotation is effective for the measurement of the sample 2 having a large diameter. However, the conventional coolable sample stage 1 cannot meet this demand.

Moreover, it is also desirable to change and set the irradiation angle of the X-ray, the electron beam, etc. by rotating the sample 2 to be measured about the axis in the left-right direction and tilting it in the T direction. In addition, it is more difficult to endlessly rotate the sample to be measured 2 in the plane and to incline the sample to be measured 2, and it is even more difficult to move the sample to be measured in the X direction, and even if it is possible,
The power transmission mechanism inevitably has a complicated structure.

The present invention has been made in view of the above circumstances, and an object thereof is to enable the temperature of a sample to be measured to be controlled and to rotate the sample to be measured endlessly in a plane. Another object of the present invention is to provide a sample stage having a simple structure that can be tilted to be substantially vertical with respect to the horizontal plane and has a sample temperature controllable.

[0011]

In order to solve the above-mentioned problems, the invention of claim 1 has a cylindrical rotary shaft, a sample holder for holding a sample to be measured, and a cylindrical rotary shaft. A sample holder in-plane rotating gear that rotates the sample holder in-plane, an in-plane rotation transmission mechanism that transmits in-plane rotation to the sample holder in-plane rotating gear, and the sample holder in-plane rotating gear in-plane A sample holder support that rotatably supports, an inclination introducing mechanism that inclines the sample holder support, and at least one of a cylindrical rotation shaft of the sample holder and a cylindrical rotation shaft of a sample holder in-plane rotating gear. A temperature control medium tank into which a temperature control medium arranged so as not to rotate in-plane is introduced, and a temperature control medium connected to the temperature control medium tank and for introducing the temperature control medium into the temperature control medium tank. An inlet tube and a heat transfer body provided integrally or integrally with the sample holder and capable of rotating relative to the temperature control medium tank while slidingly contacting with the temperature control medium tank, and the inclination introducing mechanism is provided. , Has a cylindrical tilt introduction shaft for introducing a rotation torque for tilting the sample holder support into the sample holder support, and the in-plane rotation transmission mechanism is coaxial with the cylinder tilt introduction shaft. It is characterized in that it has an in-plane rotational torque transmission shaft for transmitting a rotational torque for rotating the in-plane rotation gear of the sample holder in-plane to the in-plane rotation gear of the sample holder.

According to a second aspect of the present invention, when the sample to be measured is tilted by the tilt introducing mechanism, in-plane rotation of the sample to be measured does not occur in association with the tilt movement of the sample to be measured. It is characterized in that the sample to be measured is rotated in-plane in association with its tilting movement.

Further, the invention of claim 3 is characterized in that the inclination introducing mechanism is also an in-plane linear movement introducing mechanism for linearly moving the sample in the plane.

Further, in the invention of claim 4, the temperature control medium is a refrigerant, and the temperature control medium tank is a refrigerant tank, and the refrigerant is introduced into the refrigerant tank to measure the sample in a cooled state. It is characterized by doing.

[0015]

In the sample temperature controllable sample stage of the present invention having such a structure, the temperature control medium tank cannot rotate in-plane, and the heat transfer body integral with or integral with the sample holder is the temperature control medium. While sliding on the tank,
It rotates relative to the temperature control medium tank. Therefore, even if the temperature control medium introducing pipe is connected to the temperature control medium tank, the sample holder and the heat transfer body are not limited, and the in-plane rotation can be performed endlessly. As a result, an arbitrary azimuth angle can be set while the temperature of the measured sample is controlled to a predetermined temperature, and the emission from the measured sample for all azimuth angles with respect to any tilt angle of the measured sample. The electrons are measured depending on the angle.

Further, the inclined introduction shaft for inclining the sample to be measured and the in-plane rotational torque transmitting shaft for in-plane rotation of the sample to be measured are provided coaxially. As a result, twisting of the measured sample with respect to the in-plane rotational torque transmission shaft, which occurs when the measured sample is tilted, can be prevented.

Further, the tilt introduction shaft and the in-plane rotational torque transmission shaft are coaxially provided, and the sample to be measured is interlocked with the tilting movement of the sample to be measured so that in-plane rotation of the sample to be measured does not occur when the sample to be measured is tilted. Then it comes to rotate in the plane. As a result, in-plane rotation due to the tilt of the sample to be measured can be easily and automatically avoided, and the in-plane rotation transmission mechanism for in-plane rotation can be simplified.

[0018]

Embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is an example of an embodiment of a sample stage capable of controlling a sample temperature according to the present invention, and is a view similar to FIG. 2, schematically showing an example of cooling a sample. The same components as those of the coolable sample stage shown in FIG. 2 are designated by the same reference numerals, and detailed description thereof will be omitted.

As shown in FIG. 1, in a coolable sample stage 1 of this example, a coolant tank 4 and a heat transfer body 5 are separately formed, and a sample holder 3 and a heat transfer body 5 are provided. It is formed integrally. Further, the refrigerant tank 4 is fixed to the main body of the photoelectron spectroscopic device (not shown),
The heat transfer body 5 is in contact with the upper surface of the refrigerant tank 4 so as to be rotatable relative to the refrigerant tank 4. In that case, at least one of the upper surface of the refrigerant tank 4 and the lower surface of the heat transfer body 5 is coated with a substance having a good thermal conductor and a slip property. The rotation of the sample holder in-plane rotary gear 7 is transmitted to the sample holder 3, so that the heat transfer body 5 formed integrally with the sample holder 3 rotates together with the sample holder 3. The refrigerant tank 4 does not rotate. At this time, the heat transfer body 5 is attached to the sample holder 3
It keeps contact with the upper surface and rotates while sliding on the upper surface.

Further, the sample stage 1 of this example is provided with a tilt introducing mechanism 11 for tilting the sample holder support 10 in the T direction. This tilt introduction mechanism 11
Is composed of a cylindrical tilt torque imparting shaft 12, and one end of the tilt torque imparting shaft 12 is connected to the sample holder support 10. The tilt torque imparting shaft 12 extends through the vacuum partition 13 of the electron spectroscope to the outside of the atmosphere. The tilt torque applying shaft 12 is movable in the X direction. Therefore, by moving the tilt torque applying shaft 12 in the X direction, the sample holder support 10 is moved in the X direction.
It can be moved in any direction.

Further, the in-plane rotational torque imparting shaft 9 penetrates the tilt torque imparting shaft 12 and extends to the atmosphere,
In that case, the in-plane rotational torque imparting shaft 9 is supported in the inner hole of the tilt torque imparting shaft 12 via bearings 14 and 15 coaxially with the in-plane rotational torque imparting shaft 9 and rotatable relative to each other. Further, the in-plane rotational torque imparting shaft 9 penetrates through the tilt torque imparting shaft 12 and extends to the outside of the atmosphere. At this time, the outer peripheral surface of the in-plane rotational torque imparting shaft 9 and the inner periphery of the inclining torque imparting shaft 12 are extended. The sealing member is hermetically sealed from the surface. Therefore, the vacuum does not leak to the atmosphere side through the inner hole of the tilt torque imparting shaft 12. The atmosphere-side ends of the in-plane rotational torque imparting shaft 9 and the tilt torque imparting shaft 12 are connected to individual motor drive mechanisms (not shown). These motor drive mechanisms are electrically connected to a microcomputer (not shown). Therefore, the motor drive mechanisms are drive-controlled by the microcomputer,
The in-plane rotation torque applying shaft 9 and the tilt torque applying shaft 12 are each rotated.

By the way, when the tilt torque applying shaft 12 is rotated to tilt the sample holder support 10, that is, the sample 2 to be measured, the in-plane rotating torque applying shaft 9 does not rotate. Since the internal rotation transmission gear 8 meshes with the sample holder in-plane rotation gear 7, the sample holder in-plane rotation gear 7 rotates in-plane by an angle corresponding to the gear ratio of the gears 7 and 8. For example, when the gear ratio of both gears 7 and 8 is set to 1, the sample holder in-plane rotating gear 7 in-plane rotates by the same angle as the rotation angle of the tilt torque imparting shaft 12.

Therefore, in the sample stage 1 of this example, the sample holder support 1 by the rotation of the tilt torque imparting shaft 12 is used.
At the time of inclining 0, the microcomputer drives the motor drive mechanism so that the in-plane rotational torque imparting shaft 9 absorbs the rotation of the in-plane rotating gear 7 of the sample holder due to the inclining operation of the sample 2 to be measured. It is designed to rotate. As a result, when the sample holder support 10 is tilted, no in-plane rotation of the sample holder in-plane rotating gear 7 is performed, and the sample holder in-plane rotating gear 7 is easily held at the initial position in the in-plane rotating direction. It is like this.

The other structure of the sample stage 1 of this example thus constituted is the same as that of the conventional sample stage 1 shown in FIG.

In the sample stage 1 of this example configured as described above, the sample 2 to be measured is held on the sample stage 1 in the electron spectroscope, and the inside of the electron spectroscope is set to an ultrahigh vacuum state, and nitrogen gas is supplied. A coolant such as the above is introduced into the coolant tank 4 through the coolant introduction tube 6. The sample 2 to be measured is cooled to a predetermined temperature via the heat transfer body 5 by the cold heat of the refrigerant in the refrigerant tank 4. In this state, by irradiating X-rays, electron beams, etc., and measuring the energy level of electrons such as photoelectrons and Auger electrons emitted from the sample to be measured 2 while being cooled to a predetermined temperature in an ultrahigh vacuum. The element of the sample 2 to be measured is analyzed. In that case, the irradiation position of the X-ray, the electron beam, or the like on the measured sample 2, that is, the measurement point of the measured sample 2 is the sample holder support 1 by the tilt torque applying shaft 12.
It is changed and set by the movement of 0 in the X direction and the in-plane rotation of the sample holder in-plane rotating gear 7 due to the rotation of the in-plane rotating torque applying shaft 9 in the φ direction. As a result, the emission characteristics of the measured sample 2 such as photoelectrons and Auger electrons are measured with respect to the polar coordinates of all azimuth angles and all polar angles. At the time of in-plane rotation of the sample holder in-plane rotating gear 7, since the refrigerant tank 4 is separated from the sample holder in-plane rotating gear 7, even if the refrigerant tank 4 cannot rotate in-plane, the sample holder in-plane rotating The in-plane rotation of the gear 7 is not disturbed by the refrigerant tank 4.

On the other hand, the sample holder support 10 can be easily tilted by rotating the tilt torque imparting shaft 12 in the T direction. At this time, even if the sample holder support 10 is tilted, the sample holder in-plane rotating gear 7 does not rotate in-plane, and is held at the initial position in the in-plane rotating direction.

According to the sample stage 1 which can be cooled in this example, the sample 2 to be measured can be infinitely rotated in the plane without limitation, so that the sample 2 to be measured can be set at an arbitrary azimuth angle while being temperature-controlled. You will be able to set it. This makes it possible to measure the emitted electrons from the measured sample 2 with respect to all azimuth angles with respect to an arbitrary tilt angle of the measured sample 2 depending on the angle.

In addition, the tilt torque imparting shaft 12 for inclining the sample 2 to be measured and the in-plane rotating torque imparting shaft 9 for in-plane rotating the sample 2 to be measured are made coaxial, and when the sample 2 to be measured is tilted. Since the in-plane rotation of the measured sample 2 is interlocked with its tilting movement so that the in-plane rotation of the measured sample 2 does not occur, the in-plane rotation caused by the inclination of the measured sample 2 can be easily and automatically performed. It can be avoided. This simplifies the in-plane rotation transmission mechanism for in-plane rotation.

Further, by making the inclining torque applying shaft 12 and the in-plane rotating torque applying shaft 9 coaxial with each other, the sample 2 to be measured can be measured.
It is possible to prevent the twisting of the sample 2 to be measured with respect to the in-plane rotation torque imparting shaft 9 which is the in-plane rotation transmission mechanism when the sample is tilted.

It should be noted that when the sample 2 to be measured is measured at room temperature without introducing the refrigerant into the refrigerant tank or when the heating medium is introduced into the refrigerant tank and the sample 2 to be measured is heated, the measurement should be performed. The invention can be applied, and similarly, the emission characteristics of photoelectrons, Auger electrons, etc. of the sample to be measured 2 can be measured at normal temperature or in a heated state with respect to polar coordinates by all azimuth angles and all polar angles.

[0031]

As is apparent from the above description, according to the sample temperature controllable sample stage of the present invention, it is possible to prevent the temperature control medium tank from rotating in-plane and to provide a heat transfer member which rotates integrally with the sample holder. While sliding in contact with the temperature control medium tank,
Since the temperature control medium tank is rotated relative to the temperature control medium tank, the sample holder and the heat transfer member can be endlessly rotated in the plane. Thereby, it is possible to set an arbitrary azimuth angle while the temperature of the sample to be measured is controlled to a predetermined temperature, and with respect to an arbitrary tilt angle of the sample to be measured,
The emitted electrons from the sample to be measured with respect to all azimuth angles can be measured depending on the angle.

Further, since the inclination introducing shaft for inclining the sample to be measured and the in-plane rotational torque transmitting shaft for in-plane rotating the sample to be measured are provided coaxially, the in-plane rotating torque transmitting shaft which is generated when the sample to be measured is inclined is generated. It is possible to prevent the measurement sample from being twisted with respect to the in-plane rotational torque transmission shaft.

Further, the tilt introduction shaft and the in-plane rotational torque transmission shaft are provided coaxially, and the sample to be measured is interlocked with the tilting movement of the sample to be measured so that in-plane rotation of the sample to be measured does not occur when the sample to be measured is tilted. Since the in-plane rotation is performed by the in-plane rotation, it is possible to easily and automatically avoid the in-plane rotation due to the inclination of the sample to be measured, and to simplify the in-plane rotation transmission mechanism.

[Brief description of drawings]

FIG. 1 is a diagram schematically showing an example of a case where a sample is cooled in an example of an embodiment of a sample stage capable of controlling a sample temperature according to the present invention.

FIG. 2 is a diagram showing an example of a conventional cooling sample stage.

[Explanation of symbols]

1 ... Coolable sample stage, 2 ... Sample to be measured, 3 ... Sample holder, 4 ... Refrigerant tank, 5 ... Heat transfer body, 6 ... Spiral tube, 7 ... Sample holder in-plane rotating gear, 8 ... In-plane rotation transfer Gears, 9 ... Rotational torque imparting shaft, 10 ... Sample holder support, 11 ... Inclination introducing mechanism, 12 ... Inclination torque imparting shaft

─────────────────────────────────────────────────── ─── Continuation of the front page (58) Fields surveyed (Int.Cl. ⁷ , DB name) G01N 23/00-23/227 G01N 1/00-1/34 G01N 21/00-21/01 G01N 21 / 17-21/61 Practical file (PATOLIS) Patent file (PATOLIS)

Claims (4)

(57) [Claims] 1. A sample holder having a cylindrical rotary shaft for holding a sample to be measured, a sample holder in-plane rotary gear having a cylindrical rotary shaft and rotating the sample holder in-plane, In-plane rotation transmission mechanism that transmits in-plane rotation to the in-plane rotation gear of the sample holder, sample holder support that supports the in-plane rotation gear of the sample holder in-plane, and tilt introduction mechanism that inclines this sample holder support And a temperature control in which a temperature control medium arranged incapable of in-plane rotation is introduced into at least one of the cylindrical rotation shaft of the sample holder and the cylindrical rotation shaft of the sample holder in-plane rotating gear. A medium tank, a temperature control medium introducing pipe connected to the temperature control medium tank and for introducing a temperature control medium into the temperature control medium tank, and integrally or integrally with the sample holder and the temperature control A heat transfer member provided so as to be rotatable relative to the temperature control medium tank while slidingly contacting the medium tank, and the tilt introducing mechanism applies a rotation torque for tilting the sample holder support to the sample holder support. Has a cylindrical inclined introduction shaft for introducing into, the in-plane rotation transmission mechanism is coaxially arranged in the cylindrical inclined introduction shaft,
A sample stage capable of controlling a sample temperature, comprising an in-plane rotational torque transmitting shaft for transmitting a rotational torque for rotating the in-plane rotating gear of the sample holder to the in-plane rotating gear of the sample holder. 2. When the sample to be measured is tilted by the tilt introducing mechanism, the tilting mechanism interlocks with the tilting movement of the sample to be measured,
2. The sample stage capable of controlling the sample temperature according to claim 1, wherein the sample to be measured is rotated in-plane in association with its tilting movement so that in-plane rotation of the sample to be measured does not occur. 3. The sample stage according to claim 1, wherein the tilt introducing mechanism is also an in-plane linear movement introducing mechanism for linearly moving the sample in a plane. 4. The temperature control medium is a refrigerant, the temperature control medium tank is a refrigerant tank, and the refrigerant is introduced into the refrigerant tank to measure the sample in a cooled state. A sample stage according to claim 1, wherein the sample temperature can be controlled.