CN110632956A - Ultralow temperature environment test device with inner vacuum - Google Patents
Ultralow temperature environment test device with inner vacuum Download PDFInfo
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- CN110632956A CN110632956A CN201910826381.1A CN201910826381A CN110632956A CN 110632956 A CN110632956 A CN 110632956A CN 201910826381 A CN201910826381 A CN 201910826381A CN 110632956 A CN110632956 A CN 110632956A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
- F25B9/14—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/20—Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature
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Abstract
The invention discloses an inner vacuum ultralow temperature environment test device which comprises a vacuum cavity, a refrigerating device, a sample insertion rod cavity, a sample insertion rod, a helium circulating device, a heater, a temperature sensor and a temperature controller. The ultra-low temperature environment test device provides an inner vacuum environment with lower temperature and accurate temperature control for sample test. The invention also discloses a sliding sealing device, which is internally provided with a sliding sealing cavity far away from one side of the sample insertion rod cavity and an air sealing cavity close to one side of the sample insertion rod cavity, wherein the sliding sealing cavity is provided with a sliding sealing cavity evacuation port, and the air sealing cavity is provided with an air sealing cavity evacuation port. The sliding seal device can conveniently replace the sample inserted rod and prevent air leakage.
Description
Technical Field
The invention belongs to the technical field of low-temperature refrigeration, and particularly relates to a test device for providing an ultralow-temperature environment.
Background
The low-temperature environment test device is a convenient and practical laboratory low-temperature system, can provide a temperature environment of 4K to 373K (-269 ℃ to +100 ℃), and can be used for research, test and experiment in the aspects of new materials, superconduction, electronic devices, condensed state physics, surface physics and the like. For example, chinese patent application CN107246741A discloses a cryostat including a vacuum chamber for placing a cooled sample and a cryocooler, the vacuum chamber and the cryocooler are independently fixed, the cryocooler and the vacuum chamber are connected by a rubber bellows, the cryocooler, the vacuum chamber and the rubber bellows form a sealed chamber filled with a heat-conducting medium, and a refrigerating head of the cryocooler is inserted into the sealed chamber. The sample to be tested is mounted inside the cryostat mostly by means of a sample rod.
It should be noted that, the ultra-low temperature environment testing device in the prior art has certain disadvantages, mainly including:
1. the working temperature range of the test equipment is narrow, and the temperature control precision is low;
2. when changing the sample pole, need shut down and return to the normal atmospheric temperature with the system, complex operation, consuming time are long, even some equipment need not return to the normal atmospheric temperature, also have the air leakage to the system, lead to the system to block up the problem.
Due to the above disadvantages, the existing low temperature environment testing device has limitations in application to testing of magnetic transmission performance (such as magnetic strength), electric transmission performance (such as alternating current sensitivity), and heat transmission performance (such as specific heat, thermal conductivity, and contact thermal resistance) of materials.
Disclosure of Invention
The invention aims at improving the prior technical problem, namely the invention aims to provide an inner vacuum ultralow temperature environment test device with lower temperature and accurate temperature control.
The technical scheme provided by the invention is as follows:
the utility model provides an ultra-low temperature environment test device of interior vacuum which characterized in that includes: the vacuum cavity is used for forming a vacuum area and is provided with a first helium injection hole; a refrigeration device having a primary cold head and a secondary cold head extending into the vacuum region; the sample inserting rod cavity is arranged on the vacuum cavity body and comprises an inserting part inserted into the vacuum area, the inserting part is provided with a second helium injection hole, and the sample inserting rod cavity is also provided with a helium outflow hole; the sample inserting rod is used for installing and placing a sample and is inserted into the cavity of the sample inserting rod during testing; the helium circulating device comprises a helium storage tank, an oil-free dry pump, an activated carbon filter element, a primary heat exchanger, a secondary heat exchanger, a liquid accumulation cavity, a low-temperature regulating valve and a sample cavity heat exchanger, wherein the stored helium tank and the oil-free dry pump are connected with each other, the activated carbon filter element, the liquid accumulation cavity, the low-temperature regulating valve and the sample cavity heat exchanger are positioned in the vacuum area, the primary heat exchanger is thermally connected with the primary cold head, the secondary heat exchanger is thermally connected with the secondary cold head, and helium flowing out of the helium storage tank under the driving of the oil-free dry pump flows back to the helium storage tank after sequentially passing through the first helium injection port, the activated carbon filter element, the primary heat exchanger, the secondary heat exchanger, the liquid accumulation cavity, the low-temperature regulating; a heater and a temperature sensor mounted adjacent to the secondary cold head, the sample chamber heat exchanger, and the sample; and the temperature controller is in communication connection with the heater and the temperature sensor.
Further, the above-mentioned ultralow temperature environment test device of interior vacuum still includes to be located vacuum region in the cold screen of second grade cold head thermal connection.
Further, a superconducting magnet is installed around the sample plunger cavity.
Further, the refrigerating device is a G-M refrigerator.
The invention further aims to solve the technical problem of providing an ultralow temperature environment test device which can conveniently replace a sample inserted rod and prevent air leakage, and the technical scheme is as follows:
the sample inserted bar is installed on the sample inserted bar cavity through a sealing connection device, a sliding seal cavity far away from one side of the sample inserted bar cavity and an air seal cavity close to one side of the sample inserted bar cavity are arranged in the sealing connection device, the sliding seal cavity is provided with a sliding seal cavity evacuation port, and the air seal cavity is provided with an air seal cavity evacuation port. The sample inserting rod is characterized in that a second channel is arranged between the sliding seal cavity and the air seal cavity, the sliding seal cavity is provided with a first channel communicated with the outside atmosphere, the air seal cavity is provided with a third channel communicated with the sample inserting rod cavity, and the sample inserting rod is inserted into the sample inserting rod cavity through the first channel, the second channel and the third channel in sequence during testing. The sample inserting rod is arranged in the first channel, the first channel is provided with a first sealing ring device matched with the outer diameter of the sample inserting rod, the second channel is provided with a second sealing ring device matched with the outer diameter of the sample inserting rod, and the third channel is provided with an isolating valve.
Further, be equipped with the sliding seal chamber valve on the mouth is managed to the sliding seal chamber, be equipped with the air seal chamber valve on the mouth is managed to the air seal chamber, the sliding seal chamber valve with be equipped with interface channel between the air seal chamber valve, be equipped with on this interface channel and take out the mouth by vacuum unit, this vacuum unit take out the mouth with be equipped with the bleed valve between the air seal chamber valve.
Compared with the prior art, the invention has the following effects:
1) the back ends of the first-stage heat exchanger and the second-stage heat exchanger are provided with the liquid accumulation cavity and the low-temperature regulating valve, and the low-temperature helium can be cooled to about 1.5K and enters the sample insertion rod cavity after being throttled and expanded by the temperature regulating valve, so that a lower low-temperature environment is provided for the sample.
2) The second-stage cold head, the sample cavity heat exchanger and the temperature adjusting device are arranged near the sample, so that the temperature can be adjusted more accurately.
3) The sample inserted rod is arranged in the cavity of the sample inserted rod through the sliding sealing device, and the external air can be effectively prevented from entering when the sample inserted rod is replaced.
Drawings
FIG. 1 is a block diagram showing the components and connections of the internal vacuum ultra-low temperature environment testing apparatus provided by the present invention.
FIG. 2 is a schematic diagram of a sample plunger and 4 ways in which a sample can be placed in the cavity of the sample plunger.
Fig. 3 is a schematic structural view of the sliding seal apparatus provided by the present invention.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
As shown in fig. 1 to 3, the internal vacuum ultra-low temperature environment test device provided by the embodiment of the present invention includes a vacuum chamber 10, a refrigerating device, a helium circulating device, a sample plunger 40, a sliding sealing device 70, and a sample plunger chamber 30.
The vacuum chamber 10 is used to provide an insulating environment with high vacuum inside. The surface of the vacuum chamber 10 is provided with a vacuum safety valve (not shown), a superconducting magnet current lead interface (not shown), a first helium injection port 13 and a vacuum pumping port (not shown), a vacuum region 19 is formed in the vacuum chamber 10, and the bottom of the vacuum chamber 10 is further provided with anti-skid support legs (not shown).
The refrigerating device provides a low-temperature cold source for the vacuum cavity 10, and is preferably a G-M refrigerator or a pulse tube refrigerator. The refrigeration unit 20 includes a compressor 21 and a coldhead assembly connected to each other. The coldhead assembly includes a coldhead base 221, and a primary coldhead 222 and a secondary coldhead 223 extending from the coldhead base 221. The cold head base 221 is mounted on the vacuum chamber 10, and the primary cold head 222 and the secondary cold head 223 extend into the vacuum region 19 inside the vacuum chamber 10. The compressor 21 is located outside the vacuum chamber 10.
The sample plunger cavity 30 is filled with flowing cryogenic helium for placement of the sample plunger 40. The sample plunger chamber 30 is mounted on the vacuum chamber body 10 and includes an insertion portion 31 that is inserted into the vacuum region 19 in the vacuum chamber body 10. The bottom of the insertion portion 31 is provided with a second helium injection port 31 a. The sample plunger chamber 30 is further provided with a helium outflow port 30 b. The insert 31 is thermally connected to the secondary cold head 223 by a pure copper cold conducting strip 32 to extract cold from the cold producing device 20. A superconducting magnet 33 is mounted around the sample plunger bore 30 to provide a magnetic field environment within the sample plunger bore 30.
The sample plunger 40 is used for mounting and placing the sample 50. For measurement, the sample plunger 40 and the sample 50 are inserted into the sample plunger cavity 30. The manner in which the sample plunger 40 and the sample 50 are placed in the sample plunger cavity 30 is flexible according to the testing requirements of different samples. As shown in fig. 2 a), b), c), d): mode 1: the sample plunger and sample are in the flowing helium in the sample plunger chamber 30; mode 2: the sample plunger is in flowing helium, and the sample is in a vacuum area; mode 3: the sample inserting rod and the sample are placed in static helium and are integrally placed in flowing helium; mode 4: the sample plunger and sample are placed in the vacuum region, and the whole is placed in flowing helium.
The cryogenic helium circulating device 60 comprises a helium storage tank 61, an oil-free dry pump 62 connected with the helium storage tank, an activated carbon filter element 63, a primary heat exchanger 64, a secondary heat exchanger 65, a liquid accumulation cavity 66, a cryogenic regulating valve 67 and a sample cavity heat exchanger 68. The activated carbon filter element 63, the primary heat exchanger 64, the secondary heat exchanger 65, the liquid accumulation cavity 66, the low-temperature regulating valve 67 and the sample cavity heat exchanger 68 are all arranged inside the vacuum cavity 10. A cold shield 70 is mounted within the vacuum chamber 10 in thermal communication with the primary cold head 222. The cold shield 70 is used to shield the insert 31 of the sample insert chamber 30 and the primary heat exchanger 64, secondary heat exchanger 65, cryoregulator 66, and sample chamber heat exchanger 67 of the cryogenic helium cycle device 60. The primary heat exchanger 64 is thermally connected to the cold shield 70, and the secondary heat exchanger 65 is thermally connected to the secondary cold head 223 by a pure copper strip or a pure copper plate.
The oil-free dry pump 62 is used for providing circulating power, and gas helium flowing out of the storage helium tank 61 flows into the vacuum cavity 10 through the first helium injection port 13 and then sequentially passes through: an activated carbon filter element 63 to filter and adsorb other impurity gases (nitrogen/oxygen/carbon dioxide, etc.) to avoid freezing and blocking the pipeline at a lower temperature region; a primary heat exchanger 64, and is cooled to about 40K; the secondary heat exchanger 65 is further cooled to about 4.2K; a liquid accumulation chamber 66 for containing helium which is cooled and condensed into liquid; the low-temperature regulating valve 66 is cooled to about 1.5K after throttling expansion; the sample chamber heat exchanger 68 performs sufficient heat exchange. Thereafter, the sample pin chamber 30 is filled through the second helium inlet 31a, and after sufficient heat exchange with the sample pin 40 in the sample pin chamber 30, the sample pin flows out through the helium outlet 31b and returns to the storage helium tank 61. From there, a cycle is completed, and then the cycle continues indefinitely according to the mode.
Further, in order to realize accurate temperature control of helium circulating in the vacuum chamber 10. A heater and a temperature sensor (not shown) are mounted in the vicinity of the secondary cold head 223, the sample chamber heat exchanger 67, and the sample 50 to be measured. The heater and the temperature sensor are connected with an external controller (not shown in the figure), so that the accurate control of the temperature can be realized. The use of heaters, temperature sensors, and controllers for local temperature control is prior art and will not be described in detail herein.
The invention further provides a technical scheme for flexibly and hermetically disassembling the sample inserting rod.
As shown in fig. 3, the sample plunger 40 is mounted to the sample plunger cavity 30 by a sealing connection 70, and the sample end of the sample 50 mounted on the end of the sample plunger 40 extends into the sample plunger cavity 30. The sealed connecting device 70 is provided with a sliding sealed cavity 71 and an air sealed cavity 72 which are adjacent to each other. The sliding seal cavity is close to one side of the sample plunger cavity, and the air seal cavity is far away from one side of the sample plunger cavity. The side of the sliding seal cavity 71 away from the isolation valve 73 is provided with a first passage 701 through which the sample insertion rod 40 passes and which can be communicated with the external atmosphere. The adjacent portion of the sliding seal chamber 71 and the air seal chamber 72 is provided with a second passage 712 through which the sample insert pin 40 passes. The side of the air-tight chamber 72 close to the isolation valve 73 is provided with a third channel 723 for the sample plunger 40 to pass through and communicate with the sample plunger chamber 30. A third channel communicates the air tight chamber 72 with the sample plunger chamber 30, and an isolation valve 73 is provided in the channel. During testing, the sample plunger 40 is inserted into the sample plunger cavity 30 from the external environment through the first channel 701, the second channel 712, and the third channel 723 in sequence.
To ensure effective isolation between the external environment and the sealing connection means 70, in particular the sliding sealing chamber 71, a first sealing ring means 701a is provided on the first channel 701 matching the outer diameter of the sample plunger 40. Since a perfect seal cannot be achieved, a small amount of outside air entering through the gap between the first sealing ring means and the sample plunger 40 enters the sliding seal chamber 71. Likewise, to ensure effective isolation between the sliding seal chamber 71 and the air seal chamber 72, a second sealing ring arrangement 712a matching the outer diameter of the sample plunger 40 is provided in the second passage 712. In addition, a sliding seal cavity evacuation port 71a is further provided in the sliding seal cavity 71, and an air seal cavity evacuation port 72a is further provided in the air seal cavity 72. The sliding seal cavity evacuation port 71a is connected to a vacuum unit evacuation port 73 through a sliding seal cavity valve 71b, and the air seal cavity evacuation port 72a is connected to a vacuum unit evacuation port 74 through an air seal cavity valve 72 b. An air release valve 75 is additionally arranged between the air sealing cavity evacuation port 72a and the air sealing cavity valve 72 b.
Based on the sliding seal device 70 having the above structure, the sample plunger 40 is mounted as follows:
1) connecting an external vacuum unit to a vacuum unit extraction port 74, opening a sliding seal cavity valve 71a and an air isolation cavity valve 72a, and confirming that an air release valve 75 is in a closed state;
2) starting a vacuum unit, and continuously vacuumizing for at least 5 minutes;
3) closing the air isolation cavity valve 72a, keeping the sliding seal cavity valve in an open state, and slowly moving the sample insert rod 4 downwards;
4) opening the isolation valve 73 and continuing to move the sample plunger 40 slowly downward to a working position in the sample plunger cavity 30;
5) the sliding seal chamber valve 71a is closed, and then the vacuum unit is closed, at which time the vacuum unit can be disconnected from the vacuum unit exhaust port.
The temperature-changing inserted bar device pulls out the sample inserted bar cavity, and when the sample inserted bar and the sample are replaced, the temperature-changing inserted bar device is carried out according to the following steps:
1) connecting an external vacuumizing unit to a vacuumizing unit vacuumizing port 74, starting the vacuum unit, then opening a sliding sealing cavity valve 71a, and confirming that an air isolation cavity valve 72a is in a closed state;
2) slowly raise the sample plunger 40 so that its bottom is clear of the sample plunger cavity 30, closing the isolation valve 73;
3) filling a little dry high-purity helium gas into the air isolation cavity 72a until the sample insert rod 40 is restored to the normal temperature;
4) the sliding seal chamber valve 71a is closed and the vent valve 75 is opened to place the air isolation chamber 72a in an atmospheric state, thereby completing the entire process of removing the sample rod from the sample chamber.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The utility model provides an ultra-low temperature environment test device of interior vacuum which characterized in that includes:
the vacuum cavity is used for forming a vacuum area and is provided with a first helium injection hole;
a refrigeration device having a primary cold head and a secondary cold head extending into the vacuum region;
the sample inserting rod cavity is arranged on the vacuum cavity body and comprises an inserting part inserted into the vacuum area, the inserting part is provided with a second helium injection hole, and the sample inserting rod cavity is also provided with a helium outflow hole;
the sample inserting rod is used for installing and placing a sample and is inserted into the cavity of the sample inserting rod during testing;
the helium circulating device comprises a helium storage tank, an oil-free dry pump, an activated carbon filter element, a primary heat exchanger, a secondary heat exchanger, a liquid accumulation cavity, a low-temperature regulating valve and a sample cavity heat exchanger, wherein the stored helium tank and the oil-free dry pump are connected with each other, the activated carbon filter element, the liquid accumulation cavity, the low-temperature regulating valve and the sample cavity heat exchanger are positioned in the vacuum area, the primary heat exchanger is thermally connected with the primary cold head, the secondary heat exchanger is thermally connected with the secondary cold head, and helium flowing out of the helium storage tank under the driving of the oil-free dry pump flows back to the helium storage tank after sequentially passing through the first helium injection port, the activated carbon filter element, the primary heat exchanger, the secondary heat exchanger, the liquid accumulation cavity, the low-temperature regulating;
a heater and a temperature sensor mounted adjacent to the secondary cold head, the sample chamber heat exchanger, and the sample; and
and the temperature controller is in communication connection with the heater and the temperature sensor.
2. The internal vacuum ultra-low temperature environment testing apparatus of claim 1, further comprising a cold shield located in said vacuum region in thermal communication with said primary cold head.
3. The in-vacuum ultra-low temperature environment testing apparatus according to claim 2, wherein a superconducting magnet is installed around the sample plunger cavity.
4. The internal-vacuum ultra-low-temperature environment testing apparatus as claimed in claim 3, wherein said refrigerating apparatus is a G-M refrigerator.
5. The internal vacuum ultra-low temperature environment testing device according to any one of claims 1 to 4, wherein the sample insertion rod is mounted on the sample insertion rod cavity through a sealing connection device, a sliding seal cavity away from one side of the sample insertion rod cavity and an air seal cavity close to one side of the sample insertion rod cavity are arranged in the sealing connection device, the sliding seal cavity is provided with a sliding seal cavity evacuation port, the air seal cavity is provided with an air seal cavity evacuation port,
a second channel is arranged between the sliding seal cavity and the air seal cavity, the sliding seal cavity is provided with a first channel communicated with the outside atmosphere, the air seal cavity is provided with a third channel communicated with the sample plunger cavity, the sample plunger is inserted into the sample plunger cavity through the first channel, the second channel and the third channel in sequence during the test,
the sample inserting rod is arranged in the first channel, the first channel is provided with a first sealing ring device matched with the outer diameter of the sample inserting rod, the second channel is provided with a second sealing ring device matched with the outer diameter of the sample inserting rod, and the third channel is provided with an isolating valve.
6. The ultra-low temperature environment testing device of the internal vacuum as claimed in claim 5, wherein a sliding seal cavity valve is disposed on the sliding seal cavity evacuation port, an air seal cavity valve is disposed on the air seal cavity evacuation port, a connection channel is disposed between the sliding seal cavity valve and the air seal cavity valve, a vacuum unit evacuation port is disposed on the connection channel, and a release valve is disposed between the vacuum unit evacuation port and the air seal cavity valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910826381.1A CN110632956A (en) | 2019-09-01 | 2019-09-01 | Ultralow temperature environment test device with inner vacuum |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910826381.1A CN110632956A (en) | 2019-09-01 | 2019-09-01 | Ultralow temperature environment test device with inner vacuum |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110715845A (en) * | 2019-10-28 | 2020-01-21 | 安徽万瑞冷电科技有限公司 | Sample inserted bar sealing connection device for cryostat |
| CN114383350A (en) * | 2020-10-19 | 2022-04-22 | 国仪量子(合肥)技术有限公司 | Helium circulating low-temperature constant-temperature system for paramagnetic resonance spectrometer |
| CN115127247A (en) * | 2022-05-27 | 2022-09-30 | 中科艾科米(北京)科技有限公司 | Refrigerating gas closed-loop cooling device |
| CN115163947A (en) * | 2022-05-24 | 2022-10-11 | 安徽万瑞冷电科技有限公司 | Vacuum sealing pipe joint device for fluid transmission |
| CN116031039A (en) * | 2023-03-22 | 2023-04-28 | 宁波健信超导科技股份有限公司 | Superconducting magnet heat transfer system |
-
2019
- 2019-09-01 CN CN201910826381.1A patent/CN110632956A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110715845A (en) * | 2019-10-28 | 2020-01-21 | 安徽万瑞冷电科技有限公司 | Sample inserted bar sealing connection device for cryostat |
| CN114383350A (en) * | 2020-10-19 | 2022-04-22 | 国仪量子(合肥)技术有限公司 | Helium circulating low-temperature constant-temperature system for paramagnetic resonance spectrometer |
| CN115163947A (en) * | 2022-05-24 | 2022-10-11 | 安徽万瑞冷电科技有限公司 | Vacuum sealing pipe joint device for fluid transmission |
| CN115127247A (en) * | 2022-05-27 | 2022-09-30 | 中科艾科米(北京)科技有限公司 | Refrigerating gas closed-loop cooling device |
| CN116031039A (en) * | 2023-03-22 | 2023-04-28 | 宁波健信超导科技股份有限公司 | Superconducting magnet heat transfer system |
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