X-ray single crystal diffraction sample picking device and method of use

By designing a portable, temperature-controlled, and ventilated X-ray single-crystal diffraction sample selection device, employing a double-layer jet tube and microscope, the problem of selecting and transferring air-sensitive samples in a single-crystal diffraction device is solved, achieving rapid and safe sample processing, and is applicable to multiple single-crystal diffractometers.

CN116008273BActive Publication Date: 2025-11-28INST OF CHEM CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202310016485.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-01-06
Publication Date
2025-11-28
Estimated Expiration
2043-01-06

AI Technical Summary

Technical Problem

Existing single-crystal diffraction devices suffer from problems such as limited space, inconvenient operation, inability to control temperature, lack of ventilation system, and incompatibility with multiple instruments when selecting and transferring air-sensitive samples, which makes the samples easily damaged.

Method used

A portable, temperature-controlled X-ray single-crystal diffraction sample selection device with a ventilation system was designed. It uses a double-layer jet tube to provide inert gas protection and combines a portable frame and microscope to achieve rapid sample selection and transfer.

Benefits of technology

It enables rapid and safe selection and transfer of air-sensitive samples, preventing sample deterioration during selection and transfer without affecting instrument testing and maintenance, and is suitable for multiple single-crystal diffractometers.

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Abstract

The application provides an X-ray single crystal diffraction sample selection device and a use method. The X-ray single crystal diffraction sample selection device comprises a moving frame, a selection table, a microscope, a sample table and a double-layer jet pipe. The selection table is movably arranged on the moving frame. The microscope is arranged on the selection table. The sample table is arranged on an objective table of the microscope. The double-layer jet pipe is arranged on the selection table and is connected with a low-temperature inert gas source and a room-temperature inert gas source respectively. The double-layer jet pipe can jet double-layer inert gas towards the sample table. The inner layer and the outer layer of the double-layer inert gas are the low-temperature inert gas and the room-temperature inert gas respectively. Compared with the prior art, the application can realize selection and rapid transfer of air-sensitive samples and prevent the air-sensitive samples from deteriorating during the selection and transfer.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of X-ray single crystal diffraction, and in particular to an X-ray single crystal diffraction sample selection device and a use method thereof. BACKGROUND

[0002] Single crystal X-ray diffraction (SXRD) is a technique that uses the periodic arrangement of atoms within a crystal to diffract X-rays of a specific wavelength. The diffraction pattern is collected and a series of data reduction and correction steps are performed to obtain a set of diffraction data. A specialized crystal structure analysis and refinement software is then used to analyze the structure and obtain the atomic coordinates of the compound. This information is used to determine the molecular structure, bond lengths, bond angles, and the arrangement of the molecule in space. SXRD has become an essential tool in scientific research related to synthetic chemistry, including coordination chemistry, metal-organic chemistry, organic chemistry, inorganic materials chemistry, and bioinorganic chemistry. It is particularly useful in the study of crystal engineering and supramolecular chemistry.

[0003] Before single crystal testing, two steps of sample selection and transfer are required. The first step is selection. The single crystal samples prepared in the laboratory are usually small (on the order of hundreds of microns) and need to be selected under an optical microscope. Sometimes, the single crystal needs to be cut to obtain a more ideal sample, ensuring better test results. The selection process is usually carried out at room temperature and in an air environment, and generally takes tens of seconds to several minutes, depending on the quality of the sample and the experience of the selector. The second step is transfer. The sample is fixed on a loop (a ring-shaped filament made of high molecular material) or a glass filament (a glass filament drawn under heated conditions), and then transferred to a crystal loading platform. The above method is the most commonly used method for selecting and transferring conventional samples. However, the sample selection and transfer processes in the above method are carried out in an air environment, which is not suitable for samples sensitive to oxygen, water, and temperature, as well as air-sensitive samples that are easily weathered by losing solvent molecules. Since air-sensitive samples are easily damaged during selection and transfer, selecting and transferring such samples is challenging.

[0004] For the selection and transfer of air-sensitive samples, Chinese Patent No. CN108572185 A discloses a sample loading system suitable for air-sensitive samples, which achieves rapid selection and transfer of air-sensitive samples by setting a low-temperature crystal picking stage and a microscopic imaging unit inside a single-crystal diffractometer. This system has the following disadvantages: (1) The space above the crystal stage of the instrument is narrow, making sample selection above the crystal stage extremely inconvenient and easy to touch the low-temperature probe; (2) The low-temperature crystal picking stage and the microscopic imaging unit are both inside the instrument, resulting in a narrow internal space of the entire instrument, which affects the maintenance and repair of the instrument; (3) The low-temperature crystal picking stage does not have a temperature control device and cannot provide a sample picking environment with different temperatures; (4) There is no ventilation system, and the sample is selected directly in the mother liquor, and the evaporation of the solution is detrimental to the health of the operator; (5) One set of devices is only suitable for one instrument. Summary of the Invention

[0005] The purpose of this invention is to address the shortcomings of the prior art by providing a portable, temperature-controlled X-ray single-crystal diffraction sample selection device and its usage method that is compatible with multiple single-crystal diffractometers and can be used in conjunction with a single device. This device enables the selection and rapid transfer of air-sensitive samples, preventing the air-sensitive samples from deteriorating during the selection and transfer process.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides an X-ray single-crystal diffraction sample selection device, comprising:

[0008] Mobile rack;

[0009] A sorting table, which is movably mounted on the mobile frame;

[0010] A microscope, which is mounted on the selection stage;

[0011] A sample stage, which is disposed on the stage of the microscope;

[0012] A double-layered jet pipe is disposed on the selection stage. The double-layered jet pipe includes an outer layer pipe and an inner layer pipe. The outer layer pipe is spaced apart and sleeved outside the inner layer pipe. The outer layer pipe and the inner layer pipe are respectively provided with an outer layer air inlet and an inner layer air inlet. The outer layer air inlet is connected to a room temperature inert gas source, and the inner layer air inlet is connected to a low temperature inert gas source. The jet nozzles of the double-layered jet pipe face and are close to the sample stage.

[0013] Preferably, the inert gas source is a nitrogen source.

[0014] Preferably, the mobile rack is provided with a slide rail, one end of which extends out of the mobile rack, and the selection table is provided with a sliding block sleeved on the slide rail.

[0015] Preferably, the bottom end of the mobile rack is provided with several lockable universal wheels.

[0016] Preferably, the temperature control instrument is further provided, the temperature sensor is arranged in the inner layer pipe and close to the air outlet, the heating assembly is arranged in the inner layer pipe and close to the inner layer air inlet, and the temperature control instrument is electrically connected with the temperature sensor and the heating assembly, respectively.

[0017] Preferably, the air extraction assembly is further provided, the air extraction assembly comprises an air extraction pump and an air extraction pipe, the air extraction pump is connected with the air extraction pipe, the air extraction pipe is arranged on the selection table and located at one side of the microscope, and the air extraction port of the air extraction pipe is located at the side of the sample table.

[0018] Preferably, the double-layer air outlet pipe and the air extraction pipe are respectively installed on the selection table through adjustable installation assemblies, the adjustable installation assembly comprises a circular fixing rod, a connecting piece and a clamping piece, the circular fixing rod is vertically and fixedly arranged on the selection table, the connecting piece is movably sleeved on the circular fixing rod, the connecting piece can move up and down along the axis of the circular fixing rod and / or rotate around the axis of the circular fixing rod, the connecting piece is provided with a first locking screw for locking the connecting piece, and the clamping piece comprises a chuck and a circular connecting rod which are connected together, the circular connecting rod is movably inserted on the connecting piece, the circular connecting rod can move along its axis and / or rotate around its axis, and the connecting piece is provided with a second locking screw for locking the circular connecting rod.

[0019] In the second aspect, the application further provides a use method of the X-ray single crystal diffraction sample selection device as described in the first aspect, comprising the following steps:

[0020] Moving the X-ray single crystal diffraction sample selection device to the outside of the single crystal diffractometer, and moving the selection table to the position close to the crystal loading table in the single crystal diffractometer;

[0021] Turning on the room temperature inert gas source and the low temperature inert gas source;

[0022] Turning on the temperature control instrument and setting the required temperature, then adjusting the sizes of the air flow in the outer layer pipe and the inner layer pipe, respectively, and waiting for the temperature on the sample table to reach the specified temperature;

[0023] Placing several drops of single crystal protection oil on the slide, taking the sample from the sample bottle and placing it in the single crystal protection oil, and then placing the slide on the sample table;

[0024] The sample picking and sticking is carried out under a microscope, and then the sample is quickly transferred to the crystal loading platform;

[0025] The X-ray single crystal diffraction sample picking device is moved to other positions in the laboratory, and the room temperature inert gas source, the low temperature inert gas source and the temperature controller are turned off.

[0026] Compared with the prior art, the X-ray single crystal diffraction sample picking device has the following beneficial effects:

[0027] (1) The double-layer jet pipe can jet double-layer inert gas to the sample platform, wherein the inner-layer inert gas is low-temperature inert gas, which can protect the sample during picking to prevent the sample from deteriorating during picking, and the outer-layer inert gas is room temperature inert gas, which can prevent water vapor around the sample from condensing when picking at low temperature;

[0028] (2) The picking table can be moved to a position inside the single crystal diffractometer as close to the crystal loading platform as possible, which can shorten the distance between the picking table and the crystal loading platform, realize quick transfer of the sample, and prevent the picked sample from deteriorating during transfer due to too long transfer time;

[0029] (3) The whole device adopts a movable design, the whole device can be moved outside the single crystal diffractometer before picking, the picking table can be moved into the shielding bin of the single crystal diffractometer for sample picking and loading, and the whole device can be quickly and conveniently moved away after loading, which does not affect sample testing and instrument maintenance and repair and can be used for all single crystal diffractometers in the laboratory;

[0030] (4) The gas extraction pipe can timely extract the gas volatilized from the mother liquor to prevent the gas volatilized from the mother liquor from polluting the laboratory air and harming the health of experimental personnel;

[0031] (5) The device can be used in cooperation with a tube sealing device to seal the tube under low temperature conditions, solving the problem of picking and transferring of samples cultured under low temperature and unable to be separated from the mother liquor. BRIEF DESCRIPTION OF DRAWINGS

[0032] In order to more clearly illustrate the specific embodiments of the present application, the drawings required to be used in the specific embodiments will be briefly introduced. It should be noted that in all the drawings, the elements or parts are not necessarily drawn according to the actual proportions.

[0033] Figure 1 It is a schematic diagram of the whole structure of the X-ray single crystal diffraction sample picking device described in the embodiments of the present application;

[0034] Figure 2 It is a schematic diagram of the whole structure of the X-ray single crystal diffraction sample picking device described in the embodiments of the present application; Figure 1 It is a local enlarged view of A in the above figure;

[0035] Figure 3The adjustable mounting assembly in the X-ray single crystal diffraction sample selection device is shown in the overall structure schematic diagram of the embodiment of the present application.

[0036] Figure 4 The use state schematic diagram of the X-ray single crystal diffraction sample selection device is shown in the embodiment of the present application.

[0037] In the figure:

[0038] 1, mobile rack; 11, slide rail; 12, universal wheel; 2, selection table; 21, sliding block; 3, microscope; 31, object table; 4, sample table; 5, double-layer jet pipe; 51, outer layer air inlet; 52, inner layer air inlet; 6, temperature controller; 7, air extraction assembly; 71, air extraction pump; 72, air extraction pipe; 8, adjustable mounting assembly; 81, circular fixing rod; 82, connecting piece; 821, first locking screw; 822, second locking screw; 83, clamping piece; 831, chuck; 832, circular connecting rod; 9, single crystal diffractometer. DETAILED DESCRIPTION

[0039] In order to make the purpose, technical scheme and advantages of the present application clearer, the technical scheme of the present application will be described clearly and completely below in conjunction with the drawings. Obviously, the described embodiments are some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without making creative efforts fall within the scope of protection of the present application.

[0040] In the description of the present application, it should be noted that the orientation or position relationship indicated by the terms "upper", "lower", "inner", "outer" and the like is based on the orientation or position relationship shown in the drawings, and is only for the convenience of describing the present application and simplifying the description, and does not indicate or imply that the system or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application. In addition, the terms "first", "second", etc. are used to distinguish parts, and have no special meaning unless otherwise stated. They cannot be understood as indicating or implying relative importance.

[0041] In the description of the present application, it should be noted that, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0042] Single-crystal X-ray diffraction (SXRD) is a commonly used technique for obtaining information about the molecular spatial structure, bond lengths, bond angles, and spatial arrangement of molecules in compounds. Before conducting single-crystal testing, sample selection and transfer are necessary. Currently, most existing single-crystal sample selection devices perform sample selection and transfer directly in the atmospheric environment. For samples sensitive to oxygen, water, and temperature, and those prone to weathering due to the loss of solvent molecules, atmospheric selection and transfer can easily lead to degradation. Therefore, these single-crystal sample selection devices are not suitable for selecting and transferring sensitive single-crystal samples. This invention provides an X-ray single-crystal diffraction sample selection device and its usage method, which enables the selection and rapid transfer of air-sensitive samples, preventing their degradation during the selection and transfer process.

[0043] Exemplary embodiments of the invention will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the invention and to fully convey the scope of the invention to those skilled in the art.

[0044] Example 1

[0045] like Figures 1-4 As shown, this embodiment of the invention provides an X-ray single-crystal diffraction sample selection device, comprising:

[0046] Mobile rack 1 is used to install components. When in use, it can be moved to the vicinity of single crystal diffractometer 9. After sample selection and loading are completed, it can be moved to a place away from single crystal diffractometer 9 or to the vicinity of another single crystal diffractometer 9 for sample selection and loading.

[0047] Selection stage 2 is movably mounted on the mobile frame 1 and can be moved to a position near the crystal carrier within the shielding chamber of the single crystal diffractometer 9.

[0048] Microscope 3 is mounted on the selection stage 2;

[0049] Sample stage 4 is set on the stage 31 of microscope 3 and is used to place the sample to be selected.

[0050] The double-layer jet pipe 5 is set on the selection stage 2. The double-layer jet pipe 5 includes an outer tube and an inner tube. The outer tube is spaced outside the inner tube. The outer tube and the inner tube are respectively provided with an outer air inlet 51 and an inner air inlet 52. The outer air inlet 51 is connected to a room temperature inert gas source, and the inner air inlet 52 is connected to a low temperature inert gas source. The jet nozzle of the double-layer jet pipe 5 is oriented towards and close to the sample stage 4.

[0051] It can be understood that the inert gas source can adopt inert gases such as argon, helium and nitrogen. Preferably, the inert gas source of the embodiment is a nitrogen source.

[0052] On the one hand, the sample picking table 2 can be moved to a position close to the crystal loading table in the shielding cabin of the single crystal diffractometer 9, which can shorten the distance between the sample picking table 2 and the crystal loading table, realize the rapid transfer of the sample, and prevent the picked sample from being damaged in the transfer process due to the long transfer time. At the same time, the whole embodiment adopts a movable design, and when used, the movable rack 1 can be moved outside the single crystal diffractometer 9 and the sample picking table 2 can be moved into the single crystal diffractometer 9 for sample picking and sample loading. After the sample loading is completed, the movable rack 1 can be quickly and conveniently moved away, which does not affect the sample testing and instrument maintenance and repair and can be used for all single crystal diffractometers 9 in the laboratory.

[0053] In addition, the embodiment of the present application can also be used in cooperation with a tube sealing device to seal the tube under low temperature conditions, solving the problem of picking and transferring the sample cultured under low temperature conditions which cannot be separated from the mother liquor.

[0054] Specifically, the movable rack 1 is provided with a slide rail 11 extending out of the movable rack 1, and the sample picking table 2 is provided with a sliding block 21 slidingly sleeved on the slide rail 11. When used, the movable rack 1 can be first moved outside the single crystal diffractometer 9 and the end of the slide rail 11 extending out of the movable rack 1 is inserted into the shielding cabin of the single crystal diffractometer 9, and then the sample picking table 2 is moved to a position close to the crystal loading table in the single crystal diffractometer 9 through the sliding block 21 along the slide rail 11 for sample picking and sample loading.

[0055] It can be understood that in other embodiments, the sample picking table 2 can also be moved on the movable rack 1 through other transmission mechanisms, and the present application does not make any limitation thereon. For example, in other specific embodiments, a transmission screw rod extending out of the movable rack 1 can be arranged on the movable rack 1, and a screw nut screwing on the transmission screw rod can be arranged on the sample picking table 2, and the sample picking table 2 can be driven to move by rotating the transmission screw rod.

[0056] Further, the bottom end of the movable rack 1 is provided with a plurality of lockable universal wheels 12, which can be used to move the movable rack 1 to a target position, and then lock the universal wheels 12 to prevent the movable rack 1 from moving. Of course, in other embodiments, the moving mechanism can also be moved by other moving components or by manpower in the form of lifting, and the present application does not make any limitation thereon.

[0057] Further, the temperature controller 6 is arranged, a temperature sensor is arranged in the inner layer pipe and close to the air outlet, a heating assembly is arranged in the inner layer pipe and close to the inner layer air inlet 52, and the temperature controller 6 is electrically connected with the temperature sensor and the heating assembly respectively. In use, the required air temperature of the inner layer pipe can be set through the temperature controller 6, the actual air temperature of the inner layer pipe is detected in real time by the temperature sensor and the detection result is fed back to the temperature controller 6, the actual air temperature detected by the temperature sensor is compared with the set air temperature by the temperature controller 6, and the heating power of the heating assembly is adjusted according to the comparison result, so as to adjust the air temperature of the inner layer pipe, so that the actual air temperature of the inner layer pipe is the same as the set air temperature.

[0058] In the embodiment, the temperature controller 6 is arranged, the air temperature of the inner layer pipe can be adjusted according to the required protection temperature of different samples, and the samples can be fully protected.

[0059] Further, the air pump 71 and the air pipe 72 are arranged, the air pump 71 is connected with the air pipe 72, the air pipe 72 is arranged on the selection table 2 and located on one side of the microscope 3, and the air outlet of the air pipe 72 is located on the side of the sample table 4. The air pump 71 includes a common pump such as an axial flow pump.

[0060] When the sample that cannot be separated from the mother liquor is selected or sealed, the air pump 71 and the air pipe 72 can cooperate to timely remove the gas volatilized from the mother liquor, so as to prevent the gas volatilized from the mother liquor from polluting the laboratory air and harming the health of the experimental personnel.

[0061] Further, as shown in Figure 3 The double-layer air pipe 5 and the air pipe 72 are respectively arranged on the selection table 2 through the adjustable mounting assembly 8, the adjustable mounting assembly 8 includes a circular fixing rod 81, a connecting piece 82 and a clamping piece 83, the circular fixing rod 81 is vertically fixed on the selection table 2, the connecting piece 82 is movably sleeved on the circular fixing rod 81, the connecting piece 82 can move up and down along the axis of the circular fixing rod 81 and / or rotate around the axis of the circular fixing rod 81, the connecting piece 82 is provided with a first locking screw 821 for locking the connecting piece 82, the clamping piece 83 includes a chuck 831 and a circular connecting rod 832 connected together, the circular connecting rod 832 is movably inserted on the connecting piece 82, the circular connecting rod 832 can move along its axis and / or rotate around its axis, and the connecting piece 82 is provided with a second locking screw 822 for locking the circular connecting rod 832.

[0062] In use, the adjustable mounting assembly 8 can be used to adjust the mounting height and the inclination angle of the double-layered air jet pipe 5 and the air extraction pipe 72, respectively, so that the mounting position of the double-layered air jet pipe 5 and the air extraction pipe 72 can be adjusted according to actual needs.

[0063] Embodiment Two

[0064] The embodiment of the present application provides a use method of the X-ray single crystal diffraction sample picking device as described in Embodiment One, and specifically includes the following steps:

[0065] Step One: Move the X-ray single crystal diffraction sample picking device to the outside of the single crystal diffractometer 9 by moving the rack 1, and move the sample picking table to the inside of the single crystal diffractometer 9 as close to the crystal loading table as possible.

[0066] Step Two: Turn on the room temperature inert gas source and the low temperature inert gas source.

[0067] Step Three: Turn on the temperature controller 6 and set the required temperature, then adjust the air flow in the outer tube and the inner tube, respectively, and wait for the temperature on the sample table 4 to reach the specified temperature.

[0068] Step Four: Place a few drops of single crystal protective oil on the slide, take the sample from the sample bottle and place it in the single crystal protective oil, and then place the slide on the sample table 4.

[0069] Step Five: Perform sample picking and sticking under the microscope 3, and then quickly transfer the sample to the crystal loading table.

[0070] Step Six: Move the X-ray single crystal diffraction sample picking device to other locations in the laboratory by moving the rack 1, and turn off the room temperature inert gas source, the low temperature inert gas source and the temperature controller 6.

[0071] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. An X-ray single crystal diffraction sample picking device, characterized in that, The utility model relates to a kind of movable rack (1);Pick table (2) is movably arranged on the movable rack (1);Microscope (3) is arranged on the pick table (2);Sample table (4) is arranged on the objective table (31) of the microscope (3);Double-layer air jet pipe (5) is arranged on the pick table (2), and the double-layer air jet pipe (5) includes outer layer pipe and inner layer pipe, the outer layer pipe is spaced apart and is sleeved on the outside of the inner layer pipe, outer layer air inlet (51) and inner layer air inlet (52) are respectively arranged on the outer layer pipe and the inner layer pipe, the outer layer air inlet (51) is connected with room temperature inert gas source, the inner layer air inlet (52) is connected with low-temperature inert gas source, and the air jet port of the double-layer air jet pipe (5) is towards and close to the sample table (4). The inert gas source is a nitrogen source. The movable rack (1) is provided with a slide rail (11) on the movable rack (1), one end of the slide rail (11) extends out of the movable rack (1), and the pick table (2) is provided with a sliding block (21) slidably sleeved on the slide rail (11). The bottom end of the movable rack (1) is provided with a plurality of lockable universal wheels (12). Further comprising temperature controller (6), temperature sensor is arranged in the inner layer pipe and close to the air jet port, heating assembly is arranged in the inner layer pipe and close to the inner layer air inlet (52), and the temperature controller (6) is electrically connected with the temperature sensor and the heating assembly respectively. Further comprising air extraction assembly (7), the air extraction assembly (7) includes air extraction pump (71) and air extraction pipe (72), the air extraction pump (71) is connected with the air extraction pipe (72), the air extraction pipe (72) is arranged on the pick table (2) and located on one side of the microscope (3), and the air extraction port of the air extraction pipe (72) is located on the periphery of the sample table (4).

2. The X-ray single crystal diffraction sample picking device of claim 1, wherein, The double-layer air jet pipe (5) and the air extraction pipe (72) are respectively installed on the pick table (2) through adjustable mounting assembly (8), the adjustable mounting assembly (8) includes circular fixing rod (81), connecting piece (82) and clamping piece (83), the circular fixing rod (81) is vertically fixed and arranged on the pick table (2), the connecting piece (82) is movably sleeved on the circular fixing rod (81), the connecting piece (82) can move up and down along the axis of the circular fixing rod (81) and / or rotate around the axis of the circular fixing rod (81), the connecting piece (82) has first locking screw (821) for locking the connecting piece (82) on the connecting piece (82), the clamping piece (83) includes chuck (831) and circular connecting rod (832) connected together, the circular connecting rod (832) is movably inserted into the connecting piece (82), the circular connecting rod (832) can move along its axis and / or rotate around its axis, and the connecting piece (82) has second locking screw (822) for locking the circular connecting rod (832) on the connecting piece (82).

3. The X-ray single crystal diffraction sample picking device of claim 1, wherein, The utility model relates to a kind of movable rack (1);Pick table (2) is movably arranged on the movable rack (1);Microscope (3) is arranged on the pick table (2);Sample table (4) is arranged on the objective table (31) of the microscope (3);Double-layer air jet pipe (5) is arranged on the pick table (2), and the double-layer air jet pipe (5) includes outer layer pipe and inner layer pipe, the outer layer pipe is spaced apart and is sleeved on the outside of the inner layer pipe, outer layer air inlet (51) and inner layer air inlet (52) are respectively arranged on the outer layer pipe and the inner layer pipe, the outer layer air inlet (51) is connected with room temperature inert gas source, the inner layer air inlet (52) is connected with low-temperature inert gas source, and the air jet port of the double-layer air jet pipe (5) is towards and close to the sample table (4).

4. The X-ray single crystal diffraction sample picking device of claim 1, wherein, The inert gas source is a nitrogen source.

5. The X-ray single crystal diffraction sample picking device of claim 1, wherein, The movable rack (1) is provided with a slide rail (11) on the movable rack (1), one end of the slide rail (11) extends out of the movable rack (1), and the pick table (2) is provided with a sliding block (21) slidably sleeved on the slide rail (11).

6. The X-ray single crystal diffraction sample picking device of claim 1, wherein, The bottom end of the movable rack (1) is provided with a plurality of lockable universal wheels (12).

7. An X-ray single crystal diffraction sample picking device as claimed in claim 6, characterized in that Further comprising temperature controller (6), temperature sensor is arranged in the inner layer pipe and close to the air jet port, heating assembly is arranged in the inner layer pipe and close to the inner layer air inlet (52), and the temperature controller (6) is electrically connected with the temperature sensor and the heating assembly respectively.

8. A method of using an X-ray single crystal diffraction sample picking device according to any one of claims 1-7, wherein, Further comprising air extraction assembly (7), the air extraction assembly (7) includes air extraction pump (71) and air extraction pipe (72), the air extraction pump (71) is connected with the air extraction pipe (72), the air extraction pipe (72) is arranged on the pick table (2) and located on one side of the microscope (3), and the air extraction port of the air extraction pipe (72) is located on the periphery of the sample table (4). The double-layer air jet pipe (5) and the air extraction pipe (72) are respectively installed on the pick table (2) through adjustable mounting assembly (8), the adjustable mounting assembly (8) includes circular fixing rod (81), connecting piece (82) and clamping piece (83), the circular fixing rod (81) is vertically fixed and arranged on the pick table (2), the connecting piece (82) is movably sleeved on the circular fixing rod (81), the connecting piece (82) can move up and down along the axis of the circular fixing rod (81) and / or rotate around the axis of the circular fixing rod (81), the connecting piece (82) has first locking screw (821) for locking the connecting piece (82) on the connecting piece (82), the clamping piece (83) includes chuck (831) and circular connecting rod (832) connected together, the circular connecting rod (832) is movably inserted into the connecting piece (82), the circular connecting rod (832) can move along its axis and / or rotate around its axis, and the connecting piece (82) has second locking screw (822) for locking the circular connecting rod (832) on the connecting piece (82). Including following steps: Moving the X-ray single crystal diffraction sample picking device outside the single crystal diffractometer (9), moving the picking table (2) inside the single crystal diffractometer (9) as close to the crystal loading table as possible; Turning on the room temperature inert gas source and the low temperature inert gas source; Turning on the temperature controller (6) and setting the required temperature, then adjusting the air flow in the outer tube and the inner tube respectively, waiting for the temperature on the sample table (4) to reach the specified temperature; Placing a few drops of single crystal protective oil on a glass slide, taking the sample from the sample bottle and placing it in the single crystal protective oil, then placing the glass slide on the sample table (4); Picking and pasting the sample under the microscope (3), then quickly transferring the sample to the crystal loading table; Moving the X-ray single crystal diffraction sample picking device to other locations in the laboratory, turning off the room temperature inert gas source, the low temperature inert gas source and the temperature controller (6).

Citation Information

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