JPH0711565B2 - Cryostat - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cryostat for use in a vibrating sample magnetometer for measuring the magnetization characteristics in the extremely low temperature to room temperature region.

[0002]

2. Description of the Related Art As shown in FIG. 4, a cryostat used in a conventional vibrating sample magnetometer accommodates an annular liquid nitrogen tank (51) in a casing (50) and the liquid nitrogen tank (51). Place a liquid helium tank (52) in the internal space of
Inside this liquid helium tank (52) is a double quartz glass tube (5
3) The guide tube (54) of the sample rod formed in (53) is inserted and arranged, and the inside of the casing (50) is maintained in a vacuum state between the casing (50) and the liquid nitrogen tank (51), and between the liquid nitrogen. The tank (51) and the liquid helium tank (52) are vacuum-insulated, and the vibrating rod (55) is arranged inside the inner quartz glass tube (53) so that it can vibrate back and forth. A sample mounting holder (56) is formed at the tip of the rush, and the vibrating rod (55) is connected to a vibrating device to vibrate along the axis, and the inner and outer quartz glass tubes (53) (53) It is formed such that the inside of the inner quartz glass tube (53) is filled with the heat transfer gas while switching between the vacuum heat insulating state and the heat transfer state filled with the heat transfer gas.

[0003]

However, in the conventional cryostat, the quartz glass tube, which is a heat-defective conductor, is not used.
Since the cold heat of liquid helium was transferred to the sample part through the layer, there is a problem that heat transfer occurs through the adiabatic layer and it takes a long time for the sample to reach the cryogenic region. There is also a problem that helium evaporates and the running cost increases.

Further, in the conventional cryostat, since the vibrating rod formed in the sample mounting holder is vibrated along the axis inside the quartz glass tube formed in the hermetically sealed structure, the quartz rod is moved up and down. There is also a problem that the pressure inside the glass tube fluctuates and the temperature environment in the holder for mounting the sample becomes uneven. The present invention has been made paying attention to such a point, and an object thereof is to provide a cryostat capable of cooling a sample to an extremely low temperature region in a short time and having a low running cost.

[0005]

In order to achieve the above object, the present invention arranges a metal guide tube of a sample holder in a casing formed in an airtight structure so as to project from the outside of the casing. A sample holder that is interlockingly connected to a vibrating device is mounted in the guide cylinder, and the cold heat generating portion of the cryogenic refrigerator is inserted inside the casing to form a vacuum between the casing and the guide cylinder. The guide tube and the sample holder are filled with a heat transfer medium, and the guide tube and the cold heat generating part of the cryogenic refrigerator are connected by a heat transfer body formed of a flexible and highly heat-conductive material. I am trying.

[0006]

According to the present invention, a metal guide cylinder is disposed inside a casing formed in an airtight structure in a state of protruding from the outside of the casing, and a sample holder linked to an oscillating device is mounted in the guide cylinder. , The cold heat generating part of the cryogenic refrigerator is placed inside the casing to form a vacuum between the casing and the guide cylinder, and the space between the guide cylinder and the sample holder is filled with the heat transfer medium, Since the cold heat generation part of the cryogenic refrigerator is connected by a heat transfer body made of a flexible and highly heat-conductive material, the guide tube that is thermally connected to the sample holder is connected to the cryogenic refrigerator. Since it will be directly cooled by, the sample rapidly drops to the cryogenic temperature range. Further, since the cold heat is directly obtained by the cryogenic refrigerator and the liquefied gas is not used as the cold heat source, the liquefied gas is not evaporated and the running cost can be reduced.

[0007]

1 to 3 show an embodiment of the present invention, FIG. 1 is an enlarged view of a main portion, FIG. 2 is a schematic configuration diagram of a cryostat,
FIG. 3 is a longitudinal sectional view of the cryostat. In this cryostat, a cold head (3) of a cryogenic refrigerator (2) and a metal guide tube (4) are arranged so as to protrude from the upper wall of a casing (1) formed in an airtight structure, and the cold head is arranged.
(3) and the compressor unit (5) of the cryogenic refrigerator (2) are connected by a pair of flexible tubes (6) and an electric cord (7), and the sample holder (8) is placed inside the guide tube (4). )
Is inserted so that it can be vibrated up and down, and the upper end of the sample holder (8) is interlockingly connected to the vibrating device (9) in a removable state.

The metal guide tube (4) is inserted into the casing (1) and comprises a bottomed cylinder (10) made of a non-magnetic material having good thermal conductivity such as copper and a heat-defective conductor such as stainless steel. Formed by brazing and joining a tubular body (11) made of a non-magnetic material, the bottomed tubular body (10) is located in the plunge inner part, and the joint part is located in the casing (1) It is located at. Also,
The cold head (3) has two cold heat generating parts (12), and the tube body (11) of the guide cylinder (4) is transferred to the tropical zone (13) at the first stage cold heat generating part (high temperature side) (12a). ) And the second,
The bottomed cylindrical body of the guide cylinder (4) on the stage cold heat generation part (low temperature side) (12b)
The (10) part is thermally connected to the tropical zone (13). And
The heat transfer zone (13) connecting the cold heat generating part of the cold head (3) and the guide tube (4) is formed by weaving a thin copper wire into a strip shape and has flexibility and high thermal conductivity. Is formed.

In the guide cylinder (4), the tubular body (11) is the casing.
A heat transfer medium supply / discharge block (15) is arranged so as to project above (1) and has a passage opening / closing valve (14) formed of a ball valve at the upper end thereof. This heat transfer medium supply / discharge block (1
In (5), an exhaust port (17) communicating with the vacuum pump (16),
An air supply port (19) communicating with a helium gas cylinder (18) storing helium gas as a heat transfer medium, and a supply / discharge port (19) communicating with a balloon serving as a pressure fluctuation buffer (20) in the guide cylinder space (20). 21) has been formed.

The sample holder (8), the upper end of which is detachably linked to the vibrating device (9), has a heat transfer medium supply / discharge block.
It penetrates the ceiling wall of (15) and projects into the inside of the guide tube (4), and the sample holder (22) is attached to the lower end of the sample holder (8).
Are formed. A thermometer for measurement (23) formed of a thermocouple of gold-iron vs. normal silver is arranged in the vicinity of the sample holder (22) of the sample holder (8). ) Is connected to a temperature display device (24) arranged outside the casing (1).

Further, a gas refrigerant heat exchanger formed by winding a copper pipe (25) having a liquefied gas passage formed inside is closely fixed to the outer periphery of the guide cylinder (4). tube
One end of (25) is connected to a liquefied gas storage container (26) arranged outside the casing (1), and the other end is connected to a vacuum pump (16) via a warmer (27). . In addition, the temperature adjustment heater (28) is located at the place where the influence of the magnetic field is the smallest when set in the vibrating sample magnetometer near the joint in the bottomed cylindrical body (10) located on the rush tip side of the joint. In addition to the temperature adjustment heater (28), a temperature adjustment thermometer (29) formed of a gold-iron vs. chromel thermocouple is placed near the temperature adjustment heater (28). (1) Each is connected to the temperature control device (30) arranged outside.

The inside of the casing (1) is communicatively connected to a vacuum pump (16) through a vacuuming line (32) connected to a vacuum port (31) formed on the peripheral side wall of the casing (1). The casing (1) is formed so as to be vacuum-insulated. Reference numeral (33) in the figure denotes a flow path opening / closing valve arranged in the vacuum line (32).

In the cryostat thus formed, the guide cylinder (4) accommodating the sample holder (8) so that the sample holder (8) can be moved forward and backward is directly cooled by the cryogenic refrigerator (2), and the guide cylinder (4) is also cooled. Since the heat transfer medium such as helium gas is sealed inside, the cold heat generated in the cryogenic refrigerator (2) can be efficiently transferred to the sample. Moreover, the guide tube
(8) has a copper tube (25) inside which a liquefied gas passage is formed on the outer peripheral surface, and a heater (28) for temperature adjustment is arranged, so that the sample can be heated from 4.2 K to room temperature. Can be cooled to a temperature of.

Further, in the cryostat of this embodiment,
A bottomed cylindrical body (10) in which the guide cylinder (4) is made of a good heat conductive material such as copper, and a pipe body (stainless steel) continuous with the bottomed cylindrical body (10) such as stainless steel ( By exposing the tube body (11) made of the low heat conductive material to the outside of the casing (1), heat penetration into the cryostat is suppressed.

Further, a heat transfer medium supply / discharge block (15) is provided at the upper end of the pipe body (11) of the guide cylinder (4) to open and close the passage valve (1).
Since it is connected via 4), it can be used as a guide
By closing the passage opening / closing ball valve (14) when the sample holder (8) is pulled out from (4), the inside of the guide cylinder (4) becomes a closed space. As a result, the sample can be exchanged while the cryostat is kept at a low temperature.

Further, since the heat transfer medium in the guide tube (4) does not escape to the outside when the sample is exchanged, the volume inside the heat transfer medium supply / discharge block (15) is evacuated to fill the heat transfer medium. Since this can be done, wasteful consumption of the heat transfer medium can be reduced.

Further, since the pressure fluctuation cushioning tool (20) such as a balloon is connected to the heat transfer medium supply / discharge block (15), the sample holder (8) is vibrated when the measurement is performed.
The pressure fluctuation in the guide cylinder (4) due to the movement of (8) in and out can be buffered by the pressure fluctuation cushioning tool (20) to maintain a constant pressure in the guide cylinder (4). This makes it possible to suppress temperature variations due to pressure fluctuations and perform stable measurements.

[0018]

According to the present invention, the guide cylinder is arranged inside the casing formed in an airtight structure so as to protrude from the outside of the casing, and the sample holder which is interlockingly connected to the vibrating device is mounted in the guide cylinder. , The cold heat generating part of the cryogenic refrigerator is placed inside the casing to form a vacuum between the casing and the guide cylinder, and the space between the guide cylinder and the sample holder is filled with the heat transfer medium, Since the cold heat generation part of the cryogenic refrigerator is connected by a heat transfer body made of a flexible and highly heat-conductive material, the guide tube that is thermally connected to the sample holder is connected to the cryogenic refrigerator. Since it will be directly cooled by, the sample can be quickly lowered to the cryogenic temperature range.

Further, since the cold heat is directly obtained by the cryogenic refrigerator and the liquefied gas is not used as the cold heat source, the liquefied gas is not evaporated and the running cost can be reduced.

[Brief description of drawings]

FIG. 1 is an enlarged view of a main part of a cryostat used for a vibrating sample magnetometer.

FIG. 2 is a schematic configuration diagram of a cryostat used in a vibrating sample magnetometer.

FIG. 3 is a vertical sectional view of a cryostat used for a vibrating sample magnetometer.

FIG. 4 is a vertical cross-sectional view showing a conventional example of a cryostat used for a vibrating sample magnetometer.

[Explanation of symbols]

1 ... Casing, 2 ... Cryogenic refrigerator, 4 ... Guide tube, 8 ... Sample holder, 9 ... Vibrating device,
10 ... Tube with bottom, 11 ... Tube,
12… Cold heat generation part of cryogenic refrigerator, 13… heat transfer body,
14 ... Ball valve for passage opening / closing, 20 ... Pressure buffer, 23 ... Thermometer for measurement,
28 ... Heater, 29 ... Thermometer for temperature adjustment.

Continuation of front page (56) Reference JP-A-1-170882 (JP, A) Special Table 2-501592 (JP, A) Satoshi Konnokaku "Experimental Physics Course 17 Magnetics" PP. 196-209 Kyoritsu Publishing, issued June 1, 1968

Claims (4)

[Claims] 1. A cryostat used for a vibrating sample magnetometer, wherein a metal guide tube (4) of a sample holder (8) is provided inside a casing (1) formed in an airtight structure from outside the casing (1). It is placed in a state of plunging into the guide cylinder (4)
The sample holder (8) linked with the (9) is mounted so that it can move back and forth, and the cold heat generating part (12) of the cryogenic refrigerator (2) is inserted into the inside of the casing (1) so that the casing (1) ) And guide tube
A vacuum is formed between the guide tube (4) and the sample holder (8) and a heat transfer medium is filled between the guide tube (4) and the sample holder (8) to cool the guide tube (4) and the cryogenic refrigerator (2). A cryostat in which the generating portion (12) is connected by a heat transfer body (13) made of a flexible and highly heat-conductive material. 2. A tube body (1) made of a metal material having low thermal conductivity.
A guide cylinder (4) is formed by joining a bottomed cylinder (10) made of a non-magnetic metal material having good heat conductivity to the tip of (1).
The joint between (11) and the bottomed cylinder (10) is arranged so that the bottomed cylinder (10) is located inside the casing (1), and the influence of the magnetic field in the bottomed cylinder (10) is maximized. A heater (28) for temperature adjustment and a thermometer (29) for temperature adjustment are arranged in a small number of parts, and it is made of a material that is not affected by the magnetic field in the vicinity of the sample placement part of the sample holder (8) or the sample. The cryostat according to claim 1, wherein a thermometer (23) for measurement is arranged. 3. A pressure damper (20) communicating with the inside of the guide cylinder (4) is arranged outside the casing (1), and the guide cylinder closer to the casing (1) than the pressure damper (20).
The cryostat according to claim 1 or 2, wherein a ball valve (14) for opening and closing a passage is provided in (4) so that a sample holder (8) can be inserted therein. 4. The cryostat according to any one of claims 1 to 3, wherein a gas refrigerant heat exchanger (25) is arranged on the outer periphery of the guide cylinder (4) corresponding to a portion near the sample mounting portion.