CN113960081B - Low-temperature automatic sample changer for scattering or diffraction experiments - Google Patents
Low-temperature automatic sample changer for scattering or diffraction experiments Download PDFInfo
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- CN113960081B CN113960081B CN202111253320.4A CN202111253320A CN113960081B CN 113960081 B CN113960081 B CN 113960081B CN 202111253320 A CN202111253320 A CN 202111253320A CN 113960081 B CN113960081 B CN 113960081B
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- 238000002474 experimental method Methods 0.000 title claims abstract description 40
- 238000005070 sampling Methods 0.000 claims abstract description 99
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- 229910052734 helium Inorganic materials 0.000 claims description 39
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 39
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- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
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- 238000000034 method Methods 0.000 abstract description 24
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
- G01N23/20033—Sample holders or supports therefor provided with temperature control or heating means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
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Abstract
The utility model provides a low temperature automatic sample changer for scattering or diffraction experiments, including sample conveying system, constant temperature system and temperature control system, sample conveying system includes sampling mechanism and passes a kind mechanism, sampling mechanism includes first drive assembly, circumference drive assembly and sampling rod, first drive assembly and circumference drive assembly are used for driving the sampling rod respectively and carry out linear motion and circumference motion in order to accomplish the sampling operation, it includes second drive assembly and sample tube support to pass the prototype mechanism, a plurality of sample tubes are placed on the sample tube support, second drive assembly drive sample tube support is linear motion and accomplishes the sampling operation. Because sampling mechanism and sampling mechanism can be in the automatic sampling of experimental process and advance, realize the automatic sample changing of experimental process for the sample changing in experimental process need not close operations such as ray beam, dismounting device, calibration sample position, has reduced the human error in the repeatability experiment, has improved experimental efficiency, has avoided the waste of beam time.
Description
Technical Field
The invention relates to the field of material analysis, in particular to a low-temperature automatic sample changer for scattering or diffraction experiments.
Background
The experimental process of scattering or diffracting neutrons, X rays and the like is to emit neutrons or X rays into a sample material, and the microstructure characteristics of the sample material can be obtained by analyzing and observing the scattering or diffracting results of the material through a detector.
The thermal motion of atoms is reduced in a low-temperature environment, so that the accuracy of structural measurement can be remarkably improved, and some samples can undergo phase change or show certain excellent performances, so that the low-temperature environment is important for research in the multidisciplinary field. In the experimental process, if the samples need to be replaced, operations such as closing the beam flow, disassembling the equipment, calibrating the sample position and the like are needed, and personal errors inherent in the repeatability test can be increased, so that the experiment of multiple samples can be carried out at one time in order to improve the experimental efficiency, avoid the waste of beam flow time and reduce the experimental errors.
Disclosure of Invention
According to the low-temperature automatic sample changer for scattering or diffraction experiments, the automatic sample changing of samples is achieved through the sample conveying system.
According to a first aspect, in one embodiment there is provided a cryogenic autosampler for scattering or diffraction experiments comprising:
a sample delivery system comprising a sampling mechanism and a sample delivery mechanism; the sampling mechanism comprises a first driving assembly, a circumferential driving assembly and a sampling rod, wherein the first driving assembly is used for driving the sampling rod to move linearly along the axial direction, and the circumferential driving assembly is used for driving the sampling rod to rotate along the circumferential direction; the sample transmission mechanism comprises a second driving assembly and a sample tube support, the second driving assembly is used for driving the sample tube support to linearly move, the linear movement direction of the sample tube support is perpendicular to the linear movement direction of the sample rod, a plurality of equidistant hole sites are formed in the sample tube support, the hole sites are used for placing sample tubes, and the sample rod is used for taking out the sample tubes and conveying the sample tubes to a target detection position;
the constant temperature system is used for providing a constant temperature environment; the constant temperature system comprises a constant temperature pipe body, the constant temperature pipe body is communicated with the sample conveying system, the target detection position is arranged in the constant temperature pipe body, and the sampling rod stretches into the constant temperature pipe body to convey the sample pipe to the target detection position;
the temperature control system comprises a temperature control seat, and the temperature control seat is arranged in the constant temperature pipe body.
In one embodiment, the sampling rod includes a sampling rod body and a lock sleeve; a locking cap is arranged on the sample tube; the lock sleeve is cylindrical, and a plurality of L-shaped grooves are formed in the contact end of the lock sleeve and the sample tube; the lock cap is cylindrical, and a plurality of cylindrical protrusions are arranged on the outer side of the lock cap; the cylindrical protrusion is matched with the L-shaped groove; the number of the L-shaped grooves is equal to or greater than the number of the cylindrical protrusions.
In an embodiment, the sampling rod further comprises an elastic piece and a lower pressure head, wherein the elastic piece and the lower pressure head are arranged inside the lock sleeve, and the elastic piece is in butt joint with the lower pressure head, so that the lock sleeve is matched with the lock cap more stably.
In an embodiment, a circular limiting sheet is further arranged on the sampling rod, so that the sample tube and the constant temperature tube body are concentric after the sample tube is conveyed to the target detection position.
In an embodiment, the sampling mechanism further comprises a first sealed cavity; the sample conveying mechanism further comprises a second sealing cavity; the first sealing cavity is communicated with the second sealing cavity; the first sealed cavity and the second sealed cavity are used for maintaining the vacuum state inside the sample transmission system.
In an embodiment, a sample exchange hole and a mounting hole are formed in the second sealing cavity, the sample exchange hole is used for placing or taking out a sample tube, and the mounting hole is used for mounting a vacuumizing pipeline.
In one embodiment, the constant temperature system further comprises a refrigeration mechanism comprising a refrigerator, a helium gas generating device, a neck tube connecting flange, a gas tube and a condensing chamber assembly; the refrigerator is fixed through the neck pipe connecting flange, a helium inlet is formed in the neck pipe connecting flange, and the helium inlet is connected with an interface of the helium generating device; the air pipe is wound at the cold end of the refrigerator, then connected into the condensing chamber assembly, then connected into the constant-temperature pipe body, and then connected with the temperature control seat.
In one embodiment, the refrigerator includes a two-stage coldhead.
In one embodiment, a gate valve is disposed between the sample delivery system and the constant temperature system, and the gate valve is used for separating or communicating the sample delivery system and the constant temperature system.
In an embodiment, the constant temperature pipe body comprises three layers of heat preservation aluminum pipes and three layers of scattering beam windows, wherein the scattering beam windows are beam inflow openings or beam outflow windows, and the scattering beam windows are made of one or more of aluminum, vanadium, titanium zirconium alloy, vanadium nickel alloy, sapphire and quartz.
According to the low-temperature automatic sample changer for scattering or diffraction experiments, the sampling mechanism and the sample conveying mechanism can automatically sample and feed samples in the experimental process, so that the automatic sample changing in the experimental process is realized, the operations of closing ray beam flow, disassembling equipment, calibrating sample positions and the like are not needed in the sample changing in the experimental process, the human error in the repeatability experiment is reduced, the experimental efficiency is improved, and the waste of the beam flow time is avoided.
Drawings
FIG. 1 is a schematic diagram of a low temperature auto-sampler for scattering or diffraction experiments in one embodiment;
FIG. 2 is a schematic diagram of a structure (after removing the first sealed cavity and the second sealed cavity) of a low-temperature automatic sample changer for scattering or diffraction experiments in one embodiment;
FIG. 3 is a schematic diagram of a sampling mechanism of a low temperature automatic sample changer for scattering or diffraction experiments according to an embodiment;
FIG. 4 is a schematic cross-sectional view of the front end structure of the sampling rod of the cryogenic automatic sampler for scattering or diffraction experiments in one embodiment;
FIG. 5 is a schematic diagram of a sample injection mechanism of a low temperature auto-sampler for scattering or diffraction experiments in one embodiment;
FIG. 6 is a schematic diagram of a constant temperature system of a low temperature automatic sample changer for scattering or diffraction experiments in one embodiment;
FIG. 7 is a schematic cross-sectional view of a constant temperature system and a temperature control system of a low temperature automatic sample changer for scattering or diffraction experiments in one embodiment;
FIG. 8 is a schematic diagram of the operation principle of the constant temperature system and the temperature control system of the low temperature automatic sample changer for scattering or diffraction experiments in one embodiment.
Detailed Description
The invention will be described in further detail below with reference to the drawings by means of specific embodiments. Wherein like elements in different embodiments are numbered alike in association. In the following embodiments, numerous specific details are set forth in order to provide a better understanding of the present application. However, one skilled in the art will readily recognize that some of the features may be omitted, or replaced by other elements, materials, or methods in different situations. In some instances, some operations associated with the present application have not been shown or described in the specification to avoid obscuring the core portions of the present application, and may not be necessary for a person skilled in the art to describe in detail the relevant operations based on the description herein and the general knowledge of one skilled in the art.
Furthermore, the described features, operations, or characteristics of the description may be combined in any suitable manner in various embodiments. Also, various steps or acts in the method descriptions may be interchanged or modified in a manner apparent to those of ordinary skill in the art. Thus, the various orders in the description and drawings are for clarity of description of only certain embodiments, and are not meant to be required orders unless otherwise indicated.
The numbering of the components itself, e.g. "first", "second", etc., is used herein merely to distinguish between the described objects and does not have any sequential or technical meaning. The terms "coupled" and "connected," as used herein, are intended to encompass both direct and indirect coupling (coupling), unless otherwise indicated.
In the existing scattering or diffraction experiment process, if a sample needs to be replaced, operations such as closing the beam current, disassembling the equipment, calibrating the sample position and the like are needed, and personal errors inherent in the repeatability test are increased.
In an embodiment of the application, the low-temperature automatic sample changer for scattering or diffraction experiments comprises a sample conveying system, a constant temperature system and a temperature control system. The sample conveying system comprises a sampling mechanism and a sample conveying mechanism, the sampling mechanism comprises a first driving assembly, a circumferential driving assembly and a sampling rod, the first driving assembly and the circumferential driving assembly are respectively used for driving the sampling rod to conduct linear motion and circumferential motion so as to complete sampling operation, the sample conveying mechanism comprises a second driving assembly and a sample tube support, a plurality of sample tubes are placed on the sample tube support, and the second driving assembly drives the sample tube support to conduct linear motion so as to complete sampling operation. The constant temperature system comprises a constant temperature pipe body, the target detection position is arranged in the constant temperature pipe body, and the sampling rod stretches into the constant temperature pipe body to convey the sample pipe to the target detection position. The temperature control system comprises a temperature control seat which is arranged at the target detection position and used for adjusting the temperature of the sample to the target temperature. The low-temperature automatic sample changer for scattering or diffraction experiments in the application realizes automatic sample changing in the experimental process through the sample conveying system, so that the sample changing in the experimental process does not need to be operated such as closing the beam current, disassembling equipment, calibrating the sample position and the like, personal errors in repeated experiments are reduced, the experimental efficiency is improved, and the waste of beam current time is avoided.
Embodiment one:
as shown in fig. 1 to 8, in one embodiment of the present application, a low-temperature automatic sample changer for scattering or diffraction experiments is provided, which includes a sample transfer system, a constant temperature system, and a temperature control system. The sample delivery system includes a sampling mechanism and a sample delivery mechanism. The sampling mechanism comprises a first driving assembly 110, a circumferential driving assembly 120 and a sampling rod 130, wherein the first driving assembly 110 is used for driving the sampling rod 130 to do linear motion, and the circumferential driving assembly 120 is used for driving the sampling rod 130 to do circumferential motion. The sample transmission mechanism comprises a second driving component 140 and a sample tube bracket 151, the second driving component 140 drives the sample tube bracket 151 to do linear motion, a plurality of equidistant hole sites for placing the sample tubes 153 are arranged on the sample tube bracket 151, in the embodiment, the number of equidistant hole sites arranged on the sample tube bracket 151 is not less than six, the sampling rod 130 is used for taking out the sample tubes 153 and conveying the sample tubes 153 to a target detection position, and in order to ensure that the sample transmission system works stably, the linear motion direction of the sampling rod 130 is perpendicular to the linear motion direction of the sample tube bracket 151. The constant temperature system is used for providing the required constant temperature environment of experiment, and the constant temperature system includes constant temperature body 240, and constant temperature body 240 and sample conveying system intercommunication, and the target detection position is located in constant temperature body 240, and sampling rod 130 stretches into constant temperature body 240 and sends sample pipe 153 to the target detection position. The temperature control system comprises a temperature control seat 310, wherein the temperature control seat 310 is arranged in a constant temperature tube body and is close to a target detection position for adjusting the temperature of a sample.
According to different experimental requirements or different experimental environments, the positions and the directions of the sampling mechanism and the sample transferring mechanism are also different, in this embodiment, the sampling mechanism is vertically arranged, the sample transferring mechanism is horizontally arranged at the lower end of the sampling mechanism, that is, the first driving assembly 110 drives the sampling rod 130 to make a linear motion along the vertical direction, and the second driving assembly 140 drives the sample tube bracket 151 to make a linear motion along the horizontal direction.
In one embodiment, the sampling rod 130 includes a sampling rod body 131 and a lock sleeve 134, a lock cap 152 is provided on the sample tube 153, and the sampling operation is completed by the engagement of the lock sleeve 134 with the lock cap 152. In an embodiment, the lock sleeve 134 is cylindrical, the contact end of the lock sleeve 134 and the sample tube 153 is provided with a plurality of L-shaped grooves, the lock cap 152 is cylindrical, a plurality of cylindrical protrusions are arranged on the outer side of the lock cap 152, the cylindrical protrusions are matched with the L-shaped grooves, and the number of the L-shaped grooves is greater than or greater than that of the cylindrical protrusions, in this embodiment, the number of the L-shaped protrusions and the number of the cylindrical protrusions are 3. Therefore, when sampling is performed, the first driving component 110 drives the sampling rod 130 to move downwards, so that the cylindrical protrusion is inserted into the L-shaped groove, the circumferential driving component 120 drives the sampling rod 130 to rotate circumferentially again, so that the cylindrical protrusion is clamped into the L-shaped groove, the first driving component 110 drives the sampling rod to move upwards again, and the sample tube 153 can be taken out from the sample tube bracket 151, so that the sampling operation is completed.
In one embodiment, to make the engagement of the lock sleeve 134 with the lock cap 152 more stable, the sampling rod 130 further includes an elastic member and a lower pressing head 137, the elastic member and the lower pressing head 137 are disposed inside the lock sleeve 134, and the elastic member abuts against the lower pressing head 137. In this embodiment, a bracket fixing plate 135 is installed at the lower end of the sampling rod main body 131, a lock sleeve 134 is installed on the bracket fixing plate 135, a spring 136 is selected by an elastic member, one end of the spring 136 is abutted against the bracket fixing plate 135, and the other end is abutted against a lower pressing head 137, so that the lower pressing head 137 can press a cylindrical protrusion on the lock cap 152 when the lock sleeve 134 is matched with the lock cap 152.
In an embodiment, in order to prevent the sample tube 153 and the sampling rod 130 from rotating in the same direction during the sampling process, the sample tube 153 and the locking cap 152 are connected through a flange, a limiting groove is symmetrically formed on the flange, a limiting protrusion 154 is correspondingly arranged on the sample tube bracket 151, and during the sampling process, the limiting protrusion 154 is clamped in the limiting groove, so that the locking cap 152 is clamped in the locking sleeve 134, the sample tube 153 and the sampling rod 130 are prevented from rotating in the same direction, and the normal sampling process is ensured.
In an embodiment, the sampling rod 130 is further provided with a circular limiting sheet 133, and the circular limiting sheet 133 is fixed on the lower side of the sampling rod main body 131, so as to ensure that the sample tube 153 is coaxial with the constant temperature tube 240 after the sample tube 153 is sent to the target detection position, so that the experiment is convenient. In this embodiment, the target detection position is provided with a sample cavity 300, the sample cavity 300 and the constant temperature tube 240 are coaxial, when the experiment is performed, the sample tube 153 extends into the sample cavity 300, the upper end of the sample cavity 300 is provided with a circular limit groove 301, and when the experiment is performed, the circular limit sheet 133 is clamped into the circular limit groove 301, so as to ensure that the sample tube 153 and the sample cavity 300 are coaxial after the sample is sent in place.
In one embodiment, the sampling mechanism further comprises a first sealed cavity 161, and the sample transfer mechanism further comprises a second sealed cavity 171, the first sealed cavity 161 being in communication with the second sealed cavity 171. The first sealed cavity 161 is hollow cuboid, and an organic glass observation window is respectively arranged in front of and behind the first sealed cavity and is used for observing the running state of the sampling mechanism in the experimental process. The second sealed cavity 171 is track-shaped, and an organic glass observation window is respectively arranged in front of and behind the second sealed cavity 171 and is used for observing the running state of the sample conveying mechanism in the experimental process. The first sealed chamber 161 and the second sealed chamber 171 serve to maintain a vacuum state inside the sample transfer system.
In an embodiment, the second sealed cavity 171 is provided with a sample exchange hole 172 and a mounting hole, wherein the sample exchange hole 172 is used for placing or taking out the sample tube 153, and the mounting hole is used for mounting the vacuumizing tube 173. The second sealed chamber 171 communicates with the thermostatic tube 240.
In one embodiment, the first driving assembly 110 includes a first motor 111, a first motor controller, a first moving stage 112, a sampling screw 113, a sampling screw nut 115, a first grating scale 114, a first driving frame 116, and a sampling support plate 117, the sampling support plate 117 is fixed on a second sealing cavity 171, the first driving member 116 is fixed on the sampling support plate 117, the first motor 111 is fixed on the first driving frame 116, one end of the sampling screw 113 is fixed on the first driving member 116, the other end is connected with the first motor 111 through a coupling 148, and the first grating scale 114 is used for feeding back the real-time position of the first moving stage 112. The sampling screw nut 115 and the sampling screw 113 form a screw nut pair for driving the first moving table 112 to do linear motion, and the first moving table 112 is connected with the sampling screw nut 115 through a screw. The first motor controller is used to control the first motor 111 to control the linear motion of the sampling rod 130. The first driving frame 116 is further provided with a limiting frame 132, and the limiting frame 132 is used for limiting and protecting the stroke of the sampling rod 130 in the vertical direction.
In an embodiment, the circumferential driving assembly 120 includes a circumferential motor 122, a circumferential motor controller, and a rotary table 121, the rotary table 121 is fixed on the first moving table 112, the sampling rod 130 is rotatably connected to the rotary table 121, and the circumferential motor 122 is used for driving the sampling rod 130 to rotate circumferentially. The circumferential motor controller is used to control the circumferential motor 122 and thus the circumferential rotation of the sampling rod 130.
In one embodiment, the second driving assembly 140 includes a sample transmission screw 143, a second guide rail 146, a second slider 147, a second motor 141, a second motor controller, a sample transmission screw nut 144, a second grating ruler 142 and a sample transmission support plate 145, the sample transmission support plate 145 is fixed on the second sealing cavity 171, the second motor 141 is fixed on the sample transmission support plate 145, one end of the sample transmission screw 143 is fixedly connected to the sample transmission support plate 145, the other end is connected to the second motor 141 through a coupling 148, and the second grating ruler 142 is used for feeding back the position of the sample transmission screw nut 144, thereby feeding back the real-time position of the sample tube 153. The second slider 147 is disposed on the second guide rail 146, the second guide rail 146 is disposed parallel to the sample feeding screw 143, and a space between the second guide rail 146 and the sample feeding screw 143 is sufficient for the sample rod 130 to pass through. The sample transmission screw nut 144 and the sample transmission screw 143 form a screw nut pair for driving the sample tube bracket 151 to do linear motion, and the sample tube bracket 151 is connected with the sample transmission screw nut 144 and the second sliding block 147 through screws. The second motor controller is used to control the second motor 141 to control the linear movement of the sample tube holder 151. Those skilled in the art will recognize that the first motor controller, the circumferential motor controller and the second motor controller may be independently disposed, or may be integrally disposed in the same control unit and electrically connected to each motor, which is not limited herein.
In one embodiment, the constant temperature system further comprises a refrigeration mechanism comprising a refrigerator 250, a helium gas generating device, a neck tube connection flange 215, a gas tube 260, and a condensing chamber assembly 270. The refrigerator 250 is fixed through a neck pipe connecting flange 215, a helium inlet 254 is formed in the neck pipe connecting flange 215, the helium inlet 254 is connected with an interface of a helium generating device, an air pipe 260 is connected with the helium inlet 254, one section of the air pipe 260 is wound at the cold head end of the refrigerator 250 and then is connected with a condensing chamber assembly 270, then is connected into a constant temperature pipe body 240 and then is connected with a temperature control seat 300. In this embodiment, the refrigerator 250 has two stages of cold heads, the first stage cold head 251 can reduce the temperature of helium gas in the gas pipe 260 to about 40K, and the second stage cold head 252 can reduce the temperature of helium gas in the gas pipe 260 to below 4.2K to liquefy the helium gas to form liquid helium. A condensing chamber assembly 270 is connected below the secondary coldhead 252 for storing the generated liquid helium to generate higher refrigeration.
In one embodiment, a gate valve 212 is disposed between the sample delivery system and the thermostatic system, the gate valve 212 being configured to separate or communicate with the thermostatic tube 240 to separate or communicate the sample delivery system and the thermostatic system. When the sample tube 153 is taken out or placed through the sample exchange hole 172, the gate valve 212 can be closed to separate the sample conveying system from the constant temperature system so as to maintain the experimental environment of the constant temperature system, and after the sample tube 153 is placed, the sample conveying system is vacuumized, and then the gate valve 212 is opened, so that the experiment can be started.
In one embodiment, the thermostat system further includes a top flange 211, the top flange 211 is provided with a through hole for the thermostat pipe 240 to pass through, the top flange 211 is provided with a sample transmission system supporting frame 174, and the second sealing cavity 171 is fixed on the sample transmission system supporting frame 174. The top cover flange 211 is provided with a plurality of mounting holes for mounting the baffle valve 214, the needle valve 213 and the gate valve 212. The flapper valve 214 is provided with an extraction port for evacuating the thermostatic system to a vacuum. The needle valve 213 is used for adjusting the flow of helium in the air pipe 260, and liquid helium generated by the needle valve 213 is cooled to 1.5K due to adiabatic expansion effect to generate 1.5K helium flow, so as to provide a low-temperature environment for the thermostatic tube 240.
In one embodiment, the thermostat body 240 is provided with a thermostat body 230 on the outside, the thermostat body 230 being connected to the top cover flange 211, the thermostat body 230 being adapted to provide a first layer of insulation for the thermostat system and to provide a vacuum environment.
In one embodiment, the refrigerator 250 is provided with a cold head sleeve 243 on the outside of the cold head, and the cold head sleeve 243 is used to prevent the loss of cold.
In one embodiment, a cold box assembly is further provided outside the thermostatic tube 240, and the cold box assembly includes a cold box assembly sleeve 221 and two cylindrical copper plates 222. The cold box assembly sleeve 221 provides a second layer of heat preservation for the constant temperature system, and the cylindrical copper plate 222 is used for packaging the cold box assembly on one hand and keeping a vacuum environment, and on the other hand, cold energy is transferred to the constant temperature pipe body 240 through the excellent heat conducting property of copper, so that the inside of the constant temperature pipe body 240 is precooled.
In one embodiment, the thermostatic tube 240 includes three layers of heat-insulating aluminum tubes 241 and three layers of radiation beam windows 242, wherein the three layers of heat-insulating aluminum tubes 241 are mainly used for heat insulation and maintain a low-temperature environment inside the thermostatic tube 240. The three-layer scattered beam window 242 is used for heat preservation, on the other hand, the scattered beam window 242 is also used as a beam entrance or a beam outflow window, different materials can be selected for manufacturing the scattered beam window 242 according to different types of spectrometers selected in different experiments, and the scattered beam window 242 can be made of materials such as aluminum, vanadium, titanium zirconium alloy, vanadium nickel alloy, sapphire or quartz which are suitable for different requirements.
In an embodiment, a heating element 311 and a temperature sensor 312 are disposed in the temperature control seat 310, the heating element 311 is connected to an output end of a temperature control apparatus, the temperature sensor 312 is connected to an input end of the temperature control apparatus, the temperature sensor 312 feeds back the temperature of the temperature control seat 310 to the temperature control apparatus, and the temperature control apparatus adjusts the output power according to the temperature of the temperature control seat 310, thereby adjusting the power of the heating element 311, thereby adjusting the temperature of the temperature control seat 310, and further adjusting the temperature of the sample.
The workflow of the sample delivery system in one embodiment of the present application is as follows:
the first motor controller controls the first motor 111 to output corresponding movement through a set program, so that the first mobile station 112 drives the circumferential driving assembly 120 to drive the sampling rod 130 to move in the vertical direction, the sampling rod 130 moves to a designated position (the matching position of the lock sleeve 134 and the lock cap 152), then the circumferential motor controller controls the circumferential motor 122 to output corresponding movement through a set program, the rotary table 121 drives the sampling rod 130 to move in the circumferential direction, the to-be-locked sleeve 134 is clamped into the lock cap 152, and the lock sleeve 134 is locked in the lock cap 152 through the action of the spring 136 and the lower pressure head 137. Then the first moving table 112 drives the sampling rod 130 to move upwards to take out the sample tube 153, meanwhile, the sample tube bracket 151 is controlled to move so that the sampling rod 130 can extend into the constant temperature tube body 240, then the first moving table 112 drives the sampling rod 130 to move downwards to send the sample tube 153 to a target detection position for detection, after the detection is completed, the first moving table 112 drives the sampling rod 130 to move upwards, meanwhile, the sample tube bracket 151 is driven to the target position, then the first moving table 112 drives the sampling rod 130 to move downwards to put the sample tube 153 back into the sample tube bracket 151, then the sampling rod 130 is driven to perform circumferential motion to separate the lock sleeve 134 from the lock cap 152, and finally the sampling rod 30 is driven to return to the initial position through the first moving table 112. The above process is described as a detection process. The second motor controller controls the second motor 141 to output corresponding movement through a set program, so that the sample tube holder 151 reciprocates in the horizontal direction, the designated sample tube 153 is sent to a predetermined sampling position, and then the above detection process is repeated, thereby completing automatic sample changing detection.
As shown in fig. 8, the working principle of the constant temperature system and the temperature control system in one embodiment of the present application is as follows:
the helium generating device comprises a circulating helium tank 281 and a dry pump 282, helium in the circulating helium tank 281 enters a constant temperature system through a helium inlet 254 under the action of the dry pump 282, the helium sequentially passes through a carbon filter 253 and a two-stage cold head, the temperature of the helium is reduced to be below 4.2K, the liquefied helium is then sent to a condensing chamber assembly 270 for storage, then the liquid helium in the condensing chamber assembly 270 flows through a needle valve 213, the temperature of the liquid helium is reduced to 1.5K due to the adiabatic expansion effect, a helium flow of 1.5K is generated, and then the helium flow of 1.5K flows through the lower part of a temperature control seat 310, so that a low-temperature environment is created. Helium in the thermostatic system is re-entered into the circulating helium valve 281 by the dry pump 282 to complete the helium circulation. The temperature control seat 310 is internally provided with a heating element 311 and a temperature sensor 312, the heating element 311 is connected with the output end of a temperature control instrument, the temperature sensor 312 is connected with the input end of the temperature control instrument, the temperature sensor 312 feeds back the temperature of the temperature control seat 310 to the temperature control instrument, and the temperature control instrument adjusts the output power according to the temperature of the temperature control seat 310, so that the power of the heating element 311 is adjusted, the temperature of the temperature control seat 310 is adjusted, and the temperature of a sample is adjusted. The gas path is also provided with a plurality of gas valves 283 for adjusting the helium flow rate at all positions of the gas path so as to meet different experimental requirements. Pressure gauges 285 are provided on both the circulating helium tank 281 and the thermostatic system for indicating the pressure conditions in the circulating helium tank 281 and the thermostatic system, respectively.
According to the low-temperature automatic sample changer for scattering or diffraction experiments, as the sampling mechanism and the sample conveying mechanism can automatically sample and feed samples in the experimental process, the automatic sample changing in the experimental process is realized, so that the operations of closing a ray beam, disassembling equipment, calibrating the position of a sample and the like are not needed in the sample changing in the experimental process, personal errors in the repeatability experiments are reduced, the experimental efficiency is improved, and the waste of the beam time is avoided.
The foregoing description of the invention has been presented for purposes of illustration and description, and is not intended to be limiting. Several simple deductions, modifications or substitutions may also be made by a person skilled in the art to which the invention pertains, based on the idea of the invention.
Claims (9)
1. A low temperature automatic sample changer for scattering or diffraction experiments, comprising:
a sample delivery system comprising a sampling mechanism and a sample delivery mechanism; the sampling mechanism comprises a first driving assembly, a circumferential driving assembly and a sampling rod, wherein the first driving assembly is used for driving the sampling rod to move linearly along the axial direction, and the circumferential driving assembly is used for driving the sampling rod to rotate along the circumferential direction; the sample transmission mechanism comprises a second driving assembly and a sample tube support, the second driving assembly is used for driving the sample tube support to linearly move, the linear movement direction of the sample tube support is perpendicular to the linear movement direction of the sample rod, a plurality of equidistant hole sites are formed in the sample tube support, the hole sites are used for placing sample tubes, and the sample rod is used for taking out the sample tubes and conveying the sample tubes to a target detection position; the sampling rod comprises a sampling rod main body and a lock sleeve, wherein the lock sleeve is arranged at the end part of the sampling rod and is used for connecting the sample tube, and a lock cap is arranged on the sample tube; the sample tube is connected with the lock cap through a flange, a limit groove is formed in the flange, a limit protrusion is correspondingly arranged on the sample tube support, and the limit protrusion is used for being matched with the limit groove so that the lock cap is clamped in the lock sleeve; the sampling rod further comprises an elastic piece and a lower pressure head, the elastic piece and the lower pressure head are arranged in the lock sleeve, and the elastic piece is in butt joint with the lower pressure head, so that the lock sleeve is matched with the lock cap more stably;
the constant temperature system is used for providing a constant temperature environment; the constant temperature system comprises a constant temperature pipe body, the constant temperature pipe body is communicated with the sample conveying system, the target detection position is arranged in the constant temperature pipe body, and the sampling rod stretches into the constant temperature pipe body to convey the sample pipe to the target detection position; the constant temperature pipe body comprises three layers of heat preservation aluminum pipes and three layers of scattered beam windows, and the scattered beam windows are beam current injection inlets or beam outflow windows; the outer side of the constant temperature pipe body is provided with a cold box assembly, the cold box assembly comprises a cold box assembly sleeve and two cylindrical copper plates, the cold box assembly sleeve is used for providing a second layer of heat preservation for the constant temperature system, and the cylindrical copper plates are used for packaging the cold box assembly and conducting heat;
the temperature control system comprises a temperature control seat, and the temperature control seat is arranged in the constant temperature pipe body.
2. The low-temperature automatic sample changer for scattering or diffraction experiments as claimed in claim 1, wherein the lock sleeve is cylindrical, and a plurality of L-shaped grooves are formed at the contact end of the lock sleeve and the sample tube; the lock cap is cylindrical, and a plurality of cylindrical protrusions are arranged on the outer side of the lock cap; the cylindrical protrusion is matched with the L-shaped groove; the number of the L-shaped grooves is equal to or greater than the number of the cylindrical protrusions.
3. The low temperature auto-sampler for scattering or diffraction experiments of claim 2 wherein the sampling rod is further provided with a circular limiting sheet to ensure that the sample tube is concentric with the thermostatic tube body after the sample tube is delivered to the target detection position.
4. The low temperature auto-sampler for scattering or diffraction experiments of claim 1, wherein the sampling mechanism further comprises a first sealed cavity; the sample conveying mechanism further comprises a second sealing cavity; the first sealing cavity is communicated with the second sealing cavity; the first sealed cavity and the second sealed cavity are used for maintaining the vacuum state inside the sample transmission system.
5. The low-temperature automatic sample changer for scattering or diffraction experiments as claimed in claim 4, wherein the second sealed cavity is provided with a sample changing hole and a mounting hole, the sample changing hole is used for placing or taking out a sample tube, and the mounting hole is used for mounting a vacuumizing tube.
6. The low temperature automated sample changer for scattering or diffraction experiments of claim 1, wherein the constant temperature system further comprises a refrigeration mechanism comprising a refrigerator, a helium gas generating device, a neck tube connecting flange, a gas tube and a condensing chamber assembly; the refrigerator is fixed through the neck pipe connecting flange, a helium inlet is formed in the neck pipe connecting flange, and the helium inlet is connected with an interface of the helium generating device; the air pipe is wound at the cold end of the refrigerator, then connected into the condensing chamber assembly, then connected into the constant-temperature pipe body, and then connected with the temperature control seat.
7. The low temperature auto-sampler for scattering or diffraction experiments of claim 6 wherein said refrigerator comprises a two-stage coldhead.
8. The low temperature automatic sampler for scattering or diffraction experiments according to claim 1, wherein a gate valve is arranged between the sample conveying system and the constant temperature system, and the gate valve is used for separating or communicating the sample conveying system and the constant temperature system.
9. The low temperature auto-sampler for scattering or diffraction experiments of claim 1, wherein the material of the scattering beam window is one or more of aluminum, vanadium, titanium-zirconium alloy, vanadium-nickel alloy, sapphire and quartz.
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| CN113960081A (en) | 2022-01-21 |
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