CN113960081A - 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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- CN113960081A CN113960081A CN202111253320.4A CN202111253320A CN113960081A CN 113960081 A CN113960081 A CN 113960081A CN 202111253320 A CN202111253320 A CN 202111253320A CN 113960081 A CN113960081 A CN 113960081A
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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
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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
- 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 scattering or diffraction experiment are with low temperature automatic sample changing ware, including sample transfer system, constant temperature system and temperature control system, sample transfer system includes sampling mechanism and passes a kind mechanism, sampling mechanism includes first drive assembly, circumference drive assembly and thief rod, first drive assembly and circumference drive assembly are used for driving the thief rod respectively and carry out linear motion and circumferential motion in order to accomplish the sample operation, pass a kind mechanism and include second drive assembly and sample tube support, a plurality of sample tubes are placed on sample tube support, second drive assembly drive sample tube support is linear motion and accomplishes the appearance operation of advancing. Because the sampling mechanism and the sample transmission mechanism can automatically sample and sample in the experimental process, automatic sample changing in the experimental process is realized, so that operations such as closing the beam current of the rays, disassembling equipment, calibrating the position of a sample and the like are not needed in the sample changing in the experimental process, the artificial error in a repeatability experiment is reduced, the experimental efficiency is improved, and the waste of the beam current time is avoided.
Description
Technical Field
The invention relates to the field of material analysis, in particular to a low-temperature automatic sample changer for a scattering or diffraction experiment.
Background
The experimental process of scattering or diffraction of neutrons, X-rays and the like is to emit neutrons or X-rays into a sample material, and analyze and observe the scattering or diffraction result of the material through a detector, so that the microstructure characteristics of the sample material can be obtained.
Under the low-temperature environment, the thermal motion of atoms is reduced, the structural measurement precision can be obviously improved, and some samples can generate phase change or show certain excellent performance, so that the low-temperature environment is very important for the research in the multidisciplinary field. In the experimental process, if the sample needs to be changed, operations such as closing the beam current, disassembling the equipment and calibrating the position of the sample need to be performed, inherent human errors in the repeatability test can be increased, and the experiment of a plurality of samples can be performed at one time in order to improve the experimental efficiency, avoid the waste of the beam current time and reduce the experimental errors.
Disclosure of Invention
In view of the above technical problems, the present application provides a low temperature auto-sampler for scattering or diffraction experiments, which realizes automatic sample changing through a sample transfer system.
According to a first aspect, there is provided in one embodiment a low temperature autosampler for scattering or diffraction experiments, comprising:
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, wherein the first driving assembly is used for driving the sampling rod to linearly move 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 move linearly, the linear movement direction of the sample tube support is perpendicular to the linear movement direction of the sampling rod, a plurality of equidistant hole sites are formed in the sample tube support and used for placing sample tubes, and the sampling rod is used for taking out the sample tubes and conveying the sample tubes to a target detection position;
a constant temperature system 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 extends 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 thief rod comprises a thief rod body and a lock sleeve; a lock 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 part and a lower pressing head, the elastic part and the lower pressing head are arranged inside the lock sleeve, and the elastic part is abutted against the lower pressing head, so that the lock sleeve and the lock cap are more stably matched.
In an embodiment, the sampling rod is further provided with a round limiting sheet to ensure that the sample tube and the constant temperature tube body are coaxial after the sample tube is conveyed to the target detection position.
In one embodiment, the sampling mechanism further comprises a first sealed cavity; the sample conveying mechanism further comprises a second sealed cavity; the first sealed cavity is communicated with the second sealed cavity; the first sealed cavity and the second sealed cavity are used for maintaining a vacuum state inside the sample transmission system.
In an embodiment, 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 vacuum-pumping pipeline.
In one embodiment, the constant temperature system further comprises a refrigeration mechanism, wherein the refrigeration mechanism comprises a refrigerator, a helium gas generation device, a neck pipe connecting flange, a gas pipe and a condensation 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 gas generating device; the air pipe is wound at the cold end of the refrigerator, is connected into the condensation chamber component, is connected into the constant temperature pipe body, and is connected with the temperature control seat.
In one embodiment, the refrigerator includes a two-stage cold head.
In one embodiment, 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.
In one embodiment, the constant temperature tube body comprises three layers of heat-insulating aluminum tubes and three layers of scattering beam windows, the scattering beam windows are beam injection ports 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 the scattering or diffraction experiment, the sampling mechanism and the sample transfer mechanism can automatically sample and feed samples in the experiment process, so that automatic sample changing in the experiment process is realized, operations such as closing of a ray beam, disassembling of equipment, and calibrating of the position of a sample are not needed in sample changing in the experiment process, human errors in a repeatability experiment are reduced, the experiment efficiency is improved, and waste of beam time is avoided.
Drawings
FIG. 1 is a schematic diagram of a low temperature autosampler for scattering or diffraction experiments in an embodiment;
FIG. 2 is a schematic diagram of the structure of the low temperature autosampler for scattering or diffraction experiments (after removing the first and second sealed cavities) in one embodiment;
FIG. 3 is a schematic diagram of a sampling mechanism of the low temperature autosampler for scattering or diffraction experiments in one embodiment;
FIG. 4 is a schematic cross-sectional view of the front end structure of a sampling rod of the low temperature autosampler for scattering or diffraction experiments in an embodiment;
FIG. 5 is a schematic diagram of a sample injection mechanism of the low temperature autosampler for scattering or diffraction experiments in one embodiment;
FIG. 6 is a schematic diagram showing the structure of a constant temperature system of the low temperature autosampler for scattering or diffraction experiments in an embodiment;
FIG. 7 is a schematic sectional view of a constant temperature system and a temperature control system of the low temperature autosampler for scattering or diffraction experiments in an embodiment;
FIG. 8 is a schematic diagram showing the operation of the constant temperature system and the temperature control system of the low temperature autosampler for scattering or diffraction experiments in one embodiment.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings. Wherein like elements in different embodiments are numbered with like associated elements. In the following description, numerous details are set forth in order to provide a better understanding of the present application. However, those skilled in the art will readily recognize that some of the features may be omitted or replaced with other elements, materials, methods in different instances. In some instances, certain operations related to the present application have not been shown or described in detail in order to avoid obscuring the core of the present application from excessive description, and it is not necessary for those skilled in the art to describe these operations in detail, so that they may be fully understood from the description in the specification and the general knowledge in the art.
Furthermore, the features, operations, or characteristics described in the specification may be combined in any suitable manner to form various embodiments. Also, the various steps or actions in the method descriptions may be transposed or transposed in order, as will be apparent to one of ordinary skill in the art. Thus, the various sequences in the specification and drawings are for the purpose of describing certain embodiments only and are not intended to imply a required sequence unless otherwise indicated where such sequence must be followed.
The numbering of the components as such, e.g., "first", "second", etc., is used herein only to distinguish the objects as described, and does not have any sequential or technical meaning. The term "connected" and "coupled" when used in this application, unless otherwise indicated, includes both direct and indirect connections (couplings).
In the existing scattering or diffraction experiment process, if a sample needs to be replaced, the operations of closing the beam current, detaching equipment, calibrating the position of the sample and the like need to be carried out, and the inherent artificial errors in the repeatability test can be increased, in order to improve the experiment efficiency, avoid the waste of the beam current time and reduce the experiment errors, the experiment of a plurality of samples can be carried out at one time is very important, therefore, the inventor designs a low-temperature automatic sample changer for the scattering or diffraction experiment, the automatic sample change in the experiment process is realized through a sample transmission system, the operations of closing the beam current, detaching equipment, calibrating the position of the sample and the like are not needed, the artificial errors in the repeatability experiment are reduced, the experiment efficiency is improved, and the waste of the beam current time is avoided.
In the embodiment of the application, the low-temperature automatic sample changer for the scattering or diffraction experiment 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 perform 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 perform 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, and the temperature control seat is arranged at the target detection position and used for adjusting the temperature of the sample to the target temperature. The automatic low-temperature sample changer for the scattering or diffraction experiments in the application realizes automatic sample changing in the experiment process through the sample conveying system, so that operations such as closing of ray beams, dismounting of equipment, and sample position calibration are not needed in sample changing in the experiment process, human errors in repeatability experiments are reduced, the experiment efficiency is improved, and waste of beam time is avoided.
The first embodiment is as follows:
as shown in fig. 1 to 8, in one embodiment of the present application, a low-temperature autosampler for scattering or diffraction experiments is provided, which includes a sample delivery 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 component 110, a circumferential driving component 120 and a sampling rod 130, wherein the first driving component 110 is used for driving the sampling rod 130 to do linear motion, and the circumferential driving component 120 is used for driving the sampling rod 130 to do circumferential motion. The sample transferring mechanism comprises a second driving assembly 140 and a sample tube support 151, the second driving assembly 140 drives the sample tube support 151 to do linear motion, a plurality of equidistant hole sites are formed in the sample tube support 151 and used for placing sample tubes 153, in the embodiment, the equidistant hole sites formed in the sample tube support 151 are not less than six, a sampling rod 130 is used for taking out the sample tubes 153 and sending the sample tubes 153 to a target detection position, and in order to enable the sample transferring system to work stably, the linear motion direction of the sampling rod 130 is perpendicular to the linear motion direction of the sample tube support 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, constant temperature body 240 and sample transmission system intercommunication, and the target detection position is located in constant temperature body 240, and thief rod 130 stretches into constant temperature body 240 and delivers to the target detection position with sample cell 153. The temperature control system comprises a temperature control seat 310, wherein the temperature control seat 310 is arranged in the constant temperature tube body, is close to the target detection position and is used for adjusting the temperature of the sample.
According to different experiment requirements or different experiment environments, the positions and the directions of the sampling mechanism and the sample transmission mechanism are different, in this embodiment, the sampling mechanism is vertically arranged, the sample transmission 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 linear motion along the vertical direction, and the second driving assembly 140 drives the sample tube support 151 to make linear motion along the horizontal direction.
In one embodiment, the sampling rod 130 includes a sampling rod main body 131 and a lock sleeve 134, a lock cap 152 is disposed on the sample tube 153, and the sampling operation is completed by the cooperation of the lock sleeve 134 and the lock cap 152. In an embodiment, the lock sleeve 134 is cylindrical, a plurality of L-shaped grooves are formed in a contact end of the lock sleeve 134 and the sample tube 153, the lock cap 152 is cylindrical, a plurality of cylindrical protrusions are formed on an outer side of the lock cap 152, the cylindrical protrusions are matched with the L-shaped grooves, the number of the L-shaped grooves is greater than or equal to that of the cylindrical protrusions, and 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 assembly 110 drives the sampling rod 130 to move downwards so that the cylindrical protrusion is inserted into the L-shaped groove, the circumferential driving member 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 assembly 110 drives the sampling rod to move upwards again, the sample tube 153 can be taken out of the sample tube support 151, and sampling operation is completed.
In one embodiment, to make the engagement between the lock sleeve 134 and 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, the bracket fixing plate 135 is installed to the lower end of the sampling rod main body 131, the lock sleeve 134 is installed on the bracket fixing plate 135, the spring 136 is selected by the elastic member, one end of the spring 136 abuts against the bracket fixing plate 135, and the other end abuts against the lower pressure head 137, so that the lower pressure head 137 can press the 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 from rotating in the same direction as the sampling rod 130 during sampling, the sample tube 153 is connected to the lock cap 152 through a flange, the flange is symmetrically provided with a limiting groove, the sample tube holder 151 is correspondingly provided with a limiting protrusion 154, the limiting protrusion 154 is clamped in the limiting groove during sampling, so that the lock cap 152 is clamped in the lock sleeve 134, the sample tube 153 is prevented from rotating in the same direction as the sampling rod 130, and the sampling process is ensured to be normal.
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 to ensure that the sample tube 153 and the constant temperature tube 240 are coaxial after the sample tube 153 is sent to the target detection position, so as to facilitate the experiment. In this embodiment, the target detection position is provided with a sample chamber 300, the sample chamber 300 and the constant temperature tube 240 are coaxial, when the experiment is performed, the sample tube 153 extends into the sample chamber 300, the upper end of the sample chamber 300 is provided with a circular limiting groove 301, and when the experiment is performed, the circular limiting sheet 133 is clamped into the circular limiting groove 301 to ensure that the sample tube 153 and the sample chamber 300 are coaxial after the sample is delivered in place.
In an embodiment, the sampling mechanism further includes a first sealed cavity 161, and the sample transfer mechanism further includes a second sealed cavity 171, and the first sealed cavity 161 is communicated with the second sealed cavity 171. The first sealed cavity 161 is a hollow cuboid, and an organic glass observation window is respectively arranged in front of and behind the first sealed cavity and used for observing the running state of the sampling mechanism in the experimental process. The second sealed cavity 171 is in a runway shape, and an organic glass observation window is respectively arranged in front of and behind the second sealed cavity 171 and used for observing the running state of the sample transfer mechanism in the experimental process. The first and second sealed chambers 161 and 171 are used to maintain a vacuum state inside the sample transfer system.
In an embodiment, the second sealed chamber 171 is provided with a sample changing hole 172 and a mounting hole, the sample changing hole 172 is used for placing or taking out the sample tube 153, and the mounting hole is used for mounting the evacuation tube 173. The second sealed chamber 171 communicates with the thermostatic tube body 240.
In an 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 ruler 114, a first driving frame 116, and a sampling supporting plate 117, the sampling supporting plate 117 is fixed on the second sealed cavity 171, the first driving member 116 is fixed on the sampling supporting 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 ruler 114 is used for feeding back a 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 movable stage 112 to perform linear motion, and the first movable stage 112 is connected with the sampling screw nut 115 through a screw. The first motor controller is used to control the first motor 111 and thus the linear motion of the thief rod 130. The first driving rack 116 is further provided with a limiting rack 132, and the limiting rack 132 is used for limiting and protecting the vertical stroke of the sampling rod 130.
In one embodiment, the circumferential driving assembly 120 includes a circumferential motor 122, a circumferential motor controller, and a rotating table 121, the rotating table 121 is fixed on the first moving table 112, the sampling rod 130 is rotatably connected to the rotating 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 to control the circumferential rotation of the thief rod 130.
In an embodiment, the second driving assembly 140 includes a sample transmission screw rod 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 142 and a sample transmission support plate 145, the sample transmission support plate 145 is fixed on the second sealed cavity 171, the second motor 141 is fixed on the sample transmission support plate 145, one end of the sample transmission screw rod 143 is fixedly connected to the sample transmission support plate 145, the other end of the sample transmission screw rod is connected to the second motor 141 through a coupling 148, and the second grating 142 is used for feeding back the position of the sample transmission screw nut 144, so as to feed back the real-time position of the sample tube 153. The second slide 147 is disposed on the second guide rail 146, the second guide rail 146 is disposed parallel to the sample transfer screw 143, and the distance between the second guide rail 146 and the sample transfer screw 143 is sufficient for the sampling 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 holder 151 to make linear motion, and the sample tube holder 151, the sample transmission screw nut 144 and the second slider 147 are screwed together. The second motor controller is used to control the second motor 141 to control the linear motion of the sample tube holder 151. As will be understood by those skilled in the art, 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 to be electrically connected to each motor, which is not limited herein.
In one embodiment, the thermostatic system further comprises a refrigeration mechanism comprising a refrigerator 250, a helium gas generating device, a neck connecting flange 215, a gas pipe 260, and a condensation 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 gas generating device, an air pipe 260 is connected with the helium inlet 254, one section of the air pipe 260 is wound on the cold head end of the refrigerator 250 and then is connected to a condensation chamber assembly 270, then is connected to the inside of the constant temperature pipe body 240, and then is connected with the temperature control base 300. In this embodiment, the refrigerator 250 has two stages of cold heads, the first stage cold head 251 can reduce the temperature of the helium gas in the gas pipe 260 to about 40K, and the second stage cold head 252 can reduce the temperature of the helium gas in the gas pipe 260 to below 4.2K to liquefy the helium gas to form liquid helium. A condenser chamber assembly 270 is connected below the secondary cold head 252 for storing the generated liquid helium to produce higher cold.
In one embodiment, a gate valve 212 is disposed between the sample transfer system and the constant temperature system, and the gate valve 212 is used for separating or communicating with the constant temperature tube 240 so as to separate or communicate the sample transfer system and the constant temperature system. When the sample tube 153 is taken out or placed through the sample changing hole 172, the gate valve 212 can be closed to separate the sample conveying system and the constant temperature system so as to maintain the experiment environment of the constant temperature system, after the sample tube 153 is placed, the sample conveying system is vacuumized, and the gate valve 212 is opened again, so that the experiment can be started.
In one embodiment, the thermostatic system further includes a top cover flange 211, a through hole is formed on the top cover flange 211 for the thermostatic tube 240 to pass through, a sample transfer system support 174 is disposed on the top cover flange 211, and the second sealed chamber 171 is fixed on the sample transfer system support 174. The top cover flange 211 is provided with a plurality of mounting holes for mounting the flapper valve 214, the needle valve 213 and the gate valve 212. The flapper valve 214 is provided with a suction port for drawing the thermostatic system into a vacuum state. The needle valve 213 is used to adjust the flow rate of the helium gas in the gas pipe 260, and on the other hand, the generated liquid helium passes through the needle valve 213 and is cooled to 1.5K due to adiabatic expansion effect, so as to generate a helium flow of 1.5K, thereby providing a low-temperature environment for the thermostatic tube 240.
In one embodiment, a thermostat barrel 230 is disposed outside the thermostatic tube 240, the thermostat barrel 230 is connected to the top flange 211, and the thermostat barrel 230 is used for providing a first layer of thermal insulation and a vacuum environment for the thermostatic system.
In one embodiment, a coldhead sleeve 243 is disposed outside the coldhead of the refrigerator 250, and the coldhead sleeve 243 is used to prevent the dissipation of cold energy.
In one embodiment, a cold box assembly is further disposed 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, the cylindrical copper plate 222 is used for packaging the cold box assembly on one hand, a vacuum environment is kept, on the other hand, cold energy is transmitted to the constant temperature tube body 240 through excellent heat conduction performance of copper, and precooling is performed inside the constant temperature tube body 240.
In one embodiment, the thermostatic tube 240 includes three layers of heat-insulating aluminum tubes 241 and three layers of scattering beam windows 242, and the three layers of heat-insulating aluminum tubes 241 are mainly used for heat insulation to maintain a low-temperature environment inside the thermostatic tube 240. The three layers of scattering beam windows 242 are used for heat preservation on one hand, and on the other hand, the scattering beam windows 242 are also used as beam current injection ports or beam current outflow windows, different materials can be selected for manufacturing the scattering beam windows 242 aiming at different types of spectrometers selected in different experiments, and the materials of the scattering beam windows 242 can be aluminum, vanadium, titanium-zirconium alloy, vanadium-nickel alloy, sapphire, quartz and the like which are suitable for different requirements.
In an embodiment, the temperature control base 310 is provided with a heating element 311 and a temperature sensor 312, the heating element 311 is connected to an output end of a temperature controller, the temperature sensor 312 is connected to an input end of the temperature controller, the temperature sensor 312 feeds back the temperature of the temperature control base 310 to the temperature controller, and the temperature controller adjusts output power according to the temperature of the temperature control base 310, so as to adjust power of the heating element 311, thereby adjusting the temperature of the temperature control base 310, and further adjusting the temperature of the sample.
The workflow of the sample transfer system in one embodiment of the present application is as follows:
the first motor controller controls the first motor 111 to output corresponding motion through a set program, so that the first mobile station 112 drives the circumferential driving assembly 120, and further drives the sampling rod 130 to move in the vertical direction, when the sampling rod 130 moves to a specified position (where the lock sleeve 134 is matched with the lock cap 152), the circumferential motor controller controls the circumferential motor 122 to output corresponding motion through the set program, so that the rotating table 121 drives the sampling rod 130 to move in the circumferential direction, when the lock sleeve 134 is clamped into the lock cap 152, and through the action of the spring 136 and the lower pressing head 137, the lock sleeve 134 is locked in the lock cap 152. Then the first moving stage 112 drives the sampling rod 130 to move upwards to take out the sample tube 153, and at the same time, the sample tube holder 151 is controlled to move so that the sampling rod 130 can extend into the constant temperature tube 240, then the first moving stage 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 stage 112 drives the sampling rod 130 to move upwards, and simultaneously drives the sample tube holder 151 to the target position, then the first moving stage 112 drives the sampling rod 130 to move downwards to place the sample tube 153 back into the sample tube holder 151, then the sampling rod 130 is driven to move circumferentially 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 by the first moving stage 112. Note that the above process is 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 detection process is repeated to complete automatic sample change detection.
As shown in fig. 8, the operation principle of the constant temperature system and the temperature control system in one embodiment of the present application is as follows:
the helium gas generating device comprises a circulating helium tank 281 and a dry pump 282, under the action of the dry pump 282, helium gas in the circulating helium tank 281 enters a constant temperature system through a helium gas inlet 254, the helium gas is liquefied into liquid helium after the temperature of the helium gas is reduced to below 4.2K through a carbon filter 253 and a two-stage cold head in sequence, then the liquid helium is sent to a condensation chamber assembly 270 to be stored, then the liquid helium in the condensation chamber assembly 270 flows through a needle valve 213, the temperature is reduced to 1.5K due to the adiabatic expansion effect, a helium gas flow of 1.5K is generated, and then the helium gas flow of 1.5K flows through the lower part of a temperature control seat 310 to create a low-temperature environment. Helium in the constant temperature system is re-introduced 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 controller, the temperature sensor 312 is connected with the input end of the temperature controller, the temperature sensor 312 feeds back the temperature of the temperature control seat 310 to the temperature controller, and the temperature controller adjusts the output power according to the temperature of the temperature control seat 310, so as to adjust the power of the heating element 311, adjust the temperature of the temperature control seat 310 and further adjust the temperature of a sample. And a plurality of air valves 283 are arranged on the air path and used for adjusting the flow rate of the helium at each position of the air path so as to meet different experimental requirements. Pressure gauges 285 are provided on both the circulating helium tank 281 and the thermostatic system to indicate pressure conditions in the circulating helium tank 281 and the thermostatic system, respectively.
According to the low-temperature automatic sample changer for the scattering or diffraction experiments, the sampling mechanism and the sample transfer mechanism can automatically sample and sample in the experiment process, so that automatic sample changing in the experiment process is realized, operations such as closing of a ray beam, disassembling of equipment, and calibrating of the position of a sample are not needed in sample changing in the experiment process, human errors in repeated experiments are reduced, experiment efficiency is improved, and waste of beam time is avoided.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (10)
1. A low temperature autosampler for scattering or diffraction experiments, comprising:
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, wherein the first driving assembly is used for driving the sampling rod to linearly move 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 move linearly, the linear movement direction of the sample tube support is perpendicular to the linear movement direction of the sampling rod, a plurality of equidistant hole sites are formed in the sample tube support and used for placing sample tubes, and the sampling rod is used for taking out the sample tubes and conveying the sample tubes to a target detection position;
a constant temperature system 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 extends 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.
2. The cryogenic autosampler of claim 1, wherein said thief rod comprises a thief rod body and a lock sleeve; a lock 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.
3. The low-temperature autosampler for scattering or diffraction experiments according to claim 2, wherein said sampling rod further comprises an elastic member and a lower pressing head, said elastic member and said lower pressing head are disposed inside said lock sleeve, said elastic member abuts against said lower pressing head, so that said lock sleeve and said lock cap are more stably engaged.
4. The cryo-autosampler for scattering or diffraction experiments according to claim 3, wherein said rod further comprises a circular stop sheet to ensure that said sample tube is coaxial with said thermostatic tube after said sample tube is brought to the target detection position.
5. The low-temperature autosampler for scattering or diffraction experiments according to claim 1, wherein said sampling mechanism further comprises a first sealed chamber; the sample conveying mechanism further comprises a second sealed cavity; the first sealed cavity is communicated with the second sealed cavity; the first sealed cavity and the second sealed cavity are used for maintaining a vacuum state inside the sample transmission system.
6. The low-temperature automatic sample changer for scattering or diffraction experiments as claimed in claim 5, wherein the second sealed cavity is provided with sample changing holes and mounting holes, the sample changing holes are used for placing or taking out sample tubes, and the mounting holes are used for mounting vacuum-pumping tubes.
7. The low-temperature automatic sample changer for scattering or diffraction experiments according to claim 1, wherein the constant temperature system further comprises a refrigerating mechanism, and the refrigerating mechanism comprises a refrigerator, a helium gas generating device, a neck pipe connecting flange, a gas pipe 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 gas generating device; the air pipe is wound at the cold end of the refrigerator, is connected into the condensation chamber component, is connected into the constant temperature pipe body, and is connected with the temperature control seat.
8. The cryogenic autosampler of claim 7, wherein said refrigerator comprises a two stage cold head.
9. The low-temperature autosampler for scattering or diffraction experiments according to claim 1, characterized in that a gate valve is provided between the sample transfer system and the constant temperature system, and the gate valve is used for separating or communicating the sample transfer system and the constant temperature system.
10. The cryogenic autosampler of claim 1, wherein said thermostatic tube body comprises three layers of thermal insulating aluminum tubes and three layers of scattering beam windows, said scattering beam windows being beam injection ports or beam outflow ports, said scattering beam windows being made of one or more of aluminum, vanadium, titanium zirconium alloy, vanadium nickel alloy, sapphire and quartz.
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