CN112858582B

CN112858582B - Electrical measurement sample rod for piston type pressure bag

Info

Publication number: CN112858582B
Application number: CN202011639417.4A
Authority: CN
Inventors: 张勇; 张警蕾; 屈哲; 韩慧; 皮雳
Original assignee: Hefei Institutes of Physical Science of CAS
Current assignee: Hefei Institutes of Physical Science of CAS
Priority date: 2020-12-31
Filing date: 2020-12-31
Publication date: 2022-08-26
Anticipated expiration: 2040-12-31
Also published as: CN112858582A

Abstract

The invention discloses an electrical measurement sample rod for a piston type pressure bag, which comprises a connecting pipe fixedly connected with the pressure bag, wherein one end of the connecting pipe, which is far away from the pressure bag, is fixedly connected with a test switching part, and the test switching part is connected with an adjusting part; the test switching part comprises an adapter, and a connecting seat and an external connector are arranged on the adapter; the adjusting part comprises a sliding sleeve connected with the connecting seat; the connecting pipe comprises a hollow pipe and a lead arranged along the axial direction of the hollow pipe, and two ends of the lead are respectively communicated with the pressure bag and the external connector. And the air tightness of the sample rod is very good.

Description

Electrical measurement sample rod for piston type pressure bag

Technical Field

The invention relates to the field of electrical measurement, in particular to an electrical measurement sample rod for a piston type pressure bag.

Background

The piston type pressure bag is of a cylindrical structure, two ends of the piston type pressure bag are fixed by screws, a sample is sealed in a Teflon pipe filled with high-pressure oil and then placed in the cylinder, and a strip line is led out from one end of the sample and fixed by screws; and the other end of the pressure transmission device pressurizes the Teflon pipe in a pressure transmission mode of screwing the screw, high pressure oil is squeezed to obtain pressure, and the more the screw is screwed inwards, the higher the obtained pressure is. So that the length of the piston pressure packs at different pressures is different. Therefore, when a comprehensive Property Measurement System (PPMS) designed by Quantum Design corporation is used for electrical Measurement under pressure, there is a problem that the lengths of pressure packets are different and the length of a sample rod is also changed. Causing the measurement to have two main problems: thermal coupling and sample chamber vacuum. Mainly be sample pole length can not be fixed, and sample pole beginning length must be the longest, can guarantee sample chamber and sample pole heat exchange's normal this moment, but along with the increase of pressure, the increase screw of pressure package is constantly twisted into, and the whole length of pole is shorter and shorter, and the pressure point at the back just can hardly guarantee the normal of heat exchange like this, arouses very big measuring error. The latter uses general sealing mode and can appear leaking gas when meetting this kind of special circumstances, leads to sample chamber temperature not to fall, long-time operation, and the vapor gets into in the air and can lead to the sample chamber to freeze, and the refrigerator cold head gradually worsens, can aggravate the worsening of heat exchange simultaneously, and then leads to the damage of instrument and the failure of measurement. At present, the solution of Quantum Design company is to use a mode without a sample rod, directly utilize a clamp to clamp a piston type pressure bag, put the piston type pressure bag into a sample cavity, use a built-in measurement system of PPMS to measure, and reuse the clamp to clamp the piston type pressure bag after the measurement is finished. Its main existence has two problems, its two, piston pressure package dead weight is itself compared general sample and is held in the palm, very heavy, PPMS sample chamber just can put down the pressure package, and operating space is very limited, and this presss from both sides the power requirement to anchor clamps very high, often operates carelessly, and the pressure package slips in the sample chamber, and this is very big to PPMS sample intracavity set measuring stitch injury, in case askedly pounding, the stitch is pounded, and the repair expense is very expensive, and whole set of measurement system repairs more than half a month, has very big risk. Secondly, the built-in measurement system measures the samples in the pressure bag, only one sample can be measured at a time, the measurement efficiency is lower than that of an external system, the measurement efficiency is limited by the built-in measurement system, a user needs some special measurement requirements sometimes, and the PPMS cannot meet the requirements. At present, the measuring machine is tense in colleges and research institutes, which is undoubtedly a great disadvantage.

Disclosure of Invention

The present invention aims to provide an electrical measuring sample rod for a piston-type pressure cell to solve the problems set forth in the background art.

In order to achieve the purpose, the invention provides the following technical scheme:

an electrical measurement sample rod for a piston type pressure bag comprises a connecting pipe fixedly connected with the pressure bag, wherein one end, far away from the pressure bag, of the connecting pipe is fixedly connected with a test switching part, and an adjusting part is connected onto the test switching part;

the test switching part comprises an adapter, and a connecting seat and an external connector are arranged on the adapter;

the adjusting part comprises a sliding sleeve connected with the connecting seat;

the connecting pipe comprises a hollow pipe and a lead arranged along the axis direction of the hollow pipe, and two ends of the lead are respectively communicated with the pressure bag and the external connector.

As a further scheme of the invention: the adapter is hollow square structure, square opening has been seted up to adapter one side, the connector is connected to adapter square opening internal seal, external joint fixed connection be in the connector outside.

As a further scheme of the invention: the connecting seat is a hollow cylinder, the connecting seat is fixedly connected with the hollow pipe, and the connecting seat is provided with a avoiding hole for a lead to pass through when in use.

As a further scheme of the invention: the external connector is a Raymond male connector, and the external connector is connected with a measuring instrument.

As a further scheme of the invention: one end that sliding sleeve is close to the adapter is equipped with the casing head, the connecting seat is close to sliding sleeve's one end fixedly connected with gasket, the gasket lower extreme is equipped with the packing ring, gasket, packing ring are located the sliding sleeve upper end, gasket, packing ring are located in the casing head.

As a further scheme of the invention: the hollow pipe is provided with at least one heat resistant sheet along the axis direction, and the hollow pipe is provided with at least one vent hole.

As a further scheme of the invention: the hollow pipe is fixedly connected with the pressure bag through a connecting part.

As a further scheme of the invention: the connecting part comprises a coupler fixedly connected with the hollow pipe, and the coupler is fixedly connected with the pressure bag through a connector.

As a further scheme of the invention: the connector outside parcel has the heat-conducting ring, connector one side is equipped with the thermometer, the thermometer with the wire intercommunication.

As a further scheme of the invention: the pressure cell includes the sample chamber, sample chamber lower extreme threaded connection has the pressurization bolt, pressurization bolt lower extreme fixedly connected with sample end socket.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, the sample rod with adjustable length is arranged, so that when the length of the pressure package is changed, the sample bottom bracket at the bottom of the sample rod is ensured to be in close contact with the bottom end of the inner wall of the measuring system by adjusting the vertical positions of the test switching part and the sliding sleeve, and good heat conduction performance is ensured, so that the measuring precision is high, and the efficiency is high. The gas tightness of the sample rod is good, 182mbar can be achieved at 2K, and the lowest temperature of the system can be achieved at 1.6K by the sample rod at low temperature.

2. The invention is connected with the pressure bag through the lead, so that the measuring device is arranged externally, an external measuring system is used, the measuring means are various, a plurality of samples can be measured simultaneously, and the sample rod has no risk of damaging the instrument.

Drawings

FIG. 1 is a schematic view of a sample rod according to the present embodiment;

FIG. 2 is a cross-sectional view of a sample rod according to the present embodiment;

fig. 3 is a schematic structural view of the sample rod adapter of the present embodiment;

FIG. 4 is a schematic view of the test portion of the sample rod of the present embodiment;

FIG. 5 is a graph showing the time-air pressure variation when the sample chamber is cooled;

fig. 6 is a time-temperature variation graph of the sample chamber of the present embodiment when it is cooled.

In the figure: 1-test switching part, 11-adapter, 12-connector, 13-connecting seat, 14-external connector, 2-regulating part, 21-sliding sleeve, 22-gasket, 23-gasket, 24-sleeve head, 3-connecting pipe, 31-lead, 32-heat-resisting sheet, 33-hollow pipe, 4-connecting part, 41-coupler, 42-connector, 43-heat-conducting ring, 44-thermometer, 5-pressure bag, 51-sample cavity, 52-pressurizing screw and 6-sample bottom bracket.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1-5, in an embodiment of the present invention, an electrical measurement sample rod for a piston-type pressure bag includes a connection pipe 3 fixedly connected to a pressure bag 5, one end of the connection pipe 3 far from the pressure bag 5 is fixedly connected to a test switching portion 1, the test switching portion 1 is connected to an adjustment portion 2, the test switching portion 1 includes an adapter 11, a connector 12, a connection seat 13, and an external connector 14, the adjustment portion 2 includes a sliding sleeve 21, a gasket 22, a washer 23, and a sleeve head 24, the connection pipe 3 includes a lead 31, a heat blocking sheet 32, and a hollow pipe 33, and the connection portion 4 includes a coupler 41, a connection head 42, a heat conducting ring 43, and a thermometer 44.

Test switching portion 1 includes adapter 11, be equipped with connecting seat 13 on adapter 11, external joint 14, adapter 11 is hollow square structure, the square opening has been seted up to adapter 11 one side, sealing connection has connector 12 in the adapter square opening, external joint 14 fixed connection is in the connector 12 outside, connecting seat 13 is hollow cylinder, connecting seat 13 and hollow tube 33 fixed connection, be used for making the hole of dodging that wire 31 passed when using on connecting seat 13, external joint 14 is the thunder public head, external joint 14 is connected with measuring instrument.

Regulating part 2 includes the sliding sleeve 21 of being connected with connecting seat 13, sliding sleeve 21 is close to the one end of adapter 11 and is equipped with casing head 24, connecting seat 13 is close to the one end fixedly connected with gasket 22 of sliding sleeve 21, gasket 22 lower extreme is equipped with packing ring 23, gasket 22, packing ring 23 is located sliding sleeve 21 upper end, gasket 22, packing ring 23 is located casing head 24, sliding sleeve 21 can slide at upper and lower certain distance relative connecting seat 13, when screwing up casing head 24, gasket 22 extrusion rubber packing ring 23, seal the sliding gap between connecting seat 13 and the sliding sleeve 21, obtain the vacuum. At the moment, the sliding sleeve and the connecting seat can slide mutually, and the air pressure in the cavity can reach 182mbar at the temperature of 1.66K, so that good sealing performance is achieved.

The connecting pipe 3 comprises a hollow pipe 33 and a lead 31 arranged along the axial direction of the hollow pipe 33, two ends of the lead 31 are respectively communicated with the pressure packet 5 and the external connector 14, the lead is a woven copper lead, every two leads are twisted, at least three heat resisting sheets 32 are arranged on the hollow pipe 33 along the axial direction after the two leads are twisted, at least one vent hole is formed in the hollow pipe 33, and in the embodiment, the hollow pipe is made of stainless steel, so that the magnetic heat conduction is poor, and the heat sink is facilitated. And 3 small holes are formed in the hollow pipe, so that when the vacuum pumping is convenient, air in the rod is not pumped, and the temperature of the sample rod is influenced.

Hollow tube 33 passes through connecting

portion

4 and 5 fixed connection of pressure package, connecting portion 4 include with hollow tube 33 fixed connection's shaft coupling 41, through connector 42 fixed connection between shaft coupling 41 and the pressure package 5, the outside parcel of connector 42 has heat conduction ring 43, heat conduction ring and sample chamber wall contact for the cooling of sample in the pressure package, be equipped with the notch on the connector 42, be equipped with thermometer 44 in the notch, thermometer 44 and wire 31 intercommunication, the temperature that utilizes the thermometer to reflect is as the temperature on the sample.

The pressure bag 5 comprises a sample cavity 51, a pressurizing bolt 52 is in threaded connection with the lower end of the sample cavity 51, a sample bottom bracket 6 is fixedly connected with the lower end of the pressurizing bolt 52, a sample support base in the special comprehensive physical property measuring system cavity is fixed behind the pressure bag, the base is matched with a notch for sample measurement in the sample cavity, and after a sample rod is inserted into the sample support base, the sample rod and the notch are matched, so that the sample rod is ensured to be in contact with the base in the cavity, thermal connection is facilitated, the sample support base and a connecting piece are all made of oxygen-free copper, and the heat conducting property is good and magnetism is avoided; the coupling is made of stainless steel, has poor heat conduction and no magnetism, and is convenient for heat sink.

Piston pressure package pressure is different, and the length of pressure package is also different, injects synthetic rerum natura measurement system intracavity when the sample pole, and the sample pole contacts with sample intracavity base, during the cooling, because expend with heat and contract with cold, the sample pole can be disjointed mutually with chamber base measurement notch, when leading to falling to the low temperature, the sample pole does not have direct contact chamber base, and cold volume is not enough, and the temperature hardly reaches minimumly.

The test cable adapter of this embodiment and its supporting sliding sleeve, a gasket, the casing head combination, when using, the sample that will await measuring is placed in the sample intracavity of pressure package 5, then insert the sample intracavity with the sample pole of this embodiment, at this moment, the sample end socket of 5 lower extremes of pressure package and the inside notch phase-match of sample chamber of comprehensive rerum natura measurement system, and then guarantee zonulae occludens, improve the hot connection, furthermore, when inserting the sample pole and getting into the sample chamber, vacuum flange meets on sliding sleeve 21 and the sample chamber, sliding sleeve 21 and casing head 24 thereof this moment, gasket 22, rubber packing ring 23 is all fixed. When normal sample chamber cooling, intracavity atmospheric pressure is less than atmospheric pressure far away, under the effect of atmospheric pressure, test switching portion can receive atmospheric pressure down always, and then connecting seat 13 can the relative slip sleeve pipe lapse, compensaties piston pressure package length change and expend with heat and contract with cold's influence, through adjusting the position of test switching portion and slip sleeve pipe from top to bottom, compensaties the inconsistent problem of sample pole length. Through the cooperation between gliding sleeve pipe and the test switching portion, when the temperature descends, atmospheric pressure descends, utilizes atmospheric pressure directly to tightly press the sample pole on intracavity sample measurement notch, guarantees the firm of hot-link. Meanwhile, a heat conduction ring on the connecting piece is in contact with the wall of the sample cavity, and a constant temperature area is arranged at the bottom of the PPMS sample cavity, so that the upper and lower sample cavities of the piston type pressure packet are in contact, the temperature difference between the upper and lower pressure packets is reduced, and the measurement accuracy is improved.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims

1. The electrical measurement sample rod for the piston type pressure bag is characterized by comprising a connecting pipe (3) fixedly connected with the pressure bag (5), wherein one end, far away from the pressure bag (5), of the connecting pipe (3) is fixedly connected with a test switching part (1), and the test switching part (1) is connected with an adjusting part (2);

the test switching part (1) comprises a switching head (11), and a connecting seat (13) and an external connector (14) are arranged on the switching head (11);

the adjusting part (2) comprises a sliding sleeve (21) connected with the connecting seat (13), a sleeve head (24) is arranged at one end, close to the adapter (11), of the sliding sleeve (21), a gasket (22) is fixedly connected to one end, close to the sliding sleeve (21), of the connecting seat (13), a gasket (23) is arranged at the lower end of the gasket (22), the gasket (22) and the gasket (23) are located at the upper end of the sliding sleeve (21), and the gasket (22) and the gasket (23) are located in the sleeve head (24);

the connecting pipe (3) comprises a hollow pipe (33) and a lead (31) arranged along the axial direction of the hollow pipe (33), and two ends of the lead (31) are respectively communicated with the pressure packet (5) and the external connector (14).

2. The electrical measurement sample rod for the piston type pressure bag as claimed in claim 1, wherein the adapter (11) is a hollow square structure, a square opening is formed in one side of the adapter (11), a connector (12) is hermetically connected in the square opening of the adapter, and the external connector (14) is fixedly connected to the outer side of the connector (12).

3. An electrical measuring sample rod for a piston type pressure bag according to claim 1, characterized in that the connecting base (13) is a hollow cylinder, the connecting base (13) is fixedly connected with the hollow tube (33), and an avoiding hole for a lead wire (31) to pass through is arranged on the connecting base (13) when in use.

4. An electrical measuring sample rod for a piston-type pressure bag according to claim 1, characterized in that the external connector (14) is a Raymond head, the external connector (14) being connected to a measuring instrument.

5. An electrical measurement sample rod for a piston type pressure bag according to claim 1, characterized in that the hollow tube (33) is provided with at least three heat resistant sheets (32) along the axial direction, and the hollow tube (33) is provided with at least one vent hole.

6. Electrical measuring sample rod for piston-type pressure packs according to claim 1, characterised in that the hollow tube (33) is fixedly connected with the pressure pack (5) by means of a connection (4).

7. Electrical measuring sample rod for piston type pressure bag according to claim 6 characterized in that the connection part (4) comprises a coupling (41) fixedly connected with a hollow tube (33), the coupling (41) and the pressure bag (5) are fixedly connected through a connector (42).

8. An electrical measuring sample rod for a piston type pressure bag according to claim 7, characterized in that the connector (42) is externally wrapped with a heat conducting ring (43), a thermometer (44) is arranged on one side of the connector (42), and the thermometer (44) is communicated with the lead (31).

9. An electrical measurement sample rod for a piston type pressure bag according to claim 1, characterized in that the pressure bag (5) comprises a sample cavity (51), a pressurizing bolt (52) is connected with the lower end of the sample cavity (51) in a threaded manner, and a sample bottom holder (6) is fixedly connected with the lower end of the pressurizing bolt (52).