A micropipette device and method for precise transfer of alkali metal elements

Abstract

The present invention belongs to alkali metal transfer technology, and specifically discloses a micropipette device and method for precise transfer of alkali metal elements. The device includes an anaerobic protection chamber, an alkali metal melting module and an alkali metal pipetting module. The alkali metal pipetting module includes a propulsion piston rod, a pipette packaging clamp and a metal capillary. A glass micropipette is arranged inside the pipette packaging clamp. The propulsion piston rod extends into the glass micropipette. The power output end of the propulsion piston rod is fixedly connected with a metal capillary. The end of the metal capillary not connected to the propulsion piston rod is inserted into the metal capillary. The outer periphery of the metal capillary is provided with a first heating unit, and the outer periphery of the first heating unit is provided with a first heat preservation unit. The method includes: heating and melting the alkali metal element to be transferred; using a pipette to absorb the alkali metal element, and micro-pipetting the alkali metal element. The present invention can realize the transfer of trace alkali metals in the nanoliter level, and has strong applicability.

Description

Technical Field

[0001] The present invention belongs to the technical field of alkali metal transfer, and more specifically, relates to a micro-liquid transfer device and method for precisely transferring alkali metal elements. Background Art

[0002] The traditional pipette micro-pipetting method is a common traditional method commonly used in the biomedical field to transfer liquid biochemical samples. Traditional pipettes are made of organic materials, and the pipetting process requires a large amount of liquid sample to fill the transmission pipeline. The liquid nuclear magnetic sample uses a large amount and is not suitable for a small amount of liquid sample. The piston pipette solves the problem of filling the transmission pipeline, but its minimum pipetting volume is in the microliter level, and the problem of the minimum pipetting volume is not solved. Moreover, this type of pipette usually works in the room temperature area, and the melting point of alkali metals is tens of degrees. For example, the melting point of rubidium is 39°C, and it is solid at room temperature, so the traditional pipette is not suitable for transferring liquid alkali metals. Since alkali metals (lithium, sodium, potassium, rubidium, cesium, francium) are very active in chemical properties and react with many organic plastics, they are generally placed in mineral oil or sealed in rare gases to prevent reactions with air or water. Unlike the traditional pipette pipetting method made of organic materials, the traditional pipette is not suitable for transferring liquid alkali metals.

[0003] The core component of chip-level atomic devices is the atomic vapor chamber. In the early production of atomic vapor chambers, chemical reactions were used to generate alkali metal elements. The byproducts produced by this method often adhere to the glass layer of the atomic vapor chamber, which will cause the light transmittance of the atomic vapor chamber to decrease and affect the interaction between the alkali metal atoms and the laser. Even if the alkali metal elements are directly filled, if the alkali metal elements are filled in excess, the alkali metal will also adhere to the glass layer of the atomic vapor chamber. If the quantitative filling method is not used, the alkali metal content of each atomic vapor chamber will be different, affecting the yield of the atomic vapor chamber.

[0004] At present, there is no publicly reported method for micro-pipetting alkali metals. Lutwak et al. only mentioned the use of a micro-small volume pipette to transfer a trace amount (1-10nL) of cesium into an atomic vapor chamber in the article "The chip-scale atomic clock low-power physics package" (36th Annual Precise Time and Time Interval Meeting). The specific device and method have not been publicly reported, and the device and method used in the article are unknown. In view of the problem of trace alkali metal transfer encountered in the process of making an atomic vapor chamber, in order to improve the transfer accuracy of alkali metal samples, increase the quality of alkali metal sample transfer, improve the performance of alkali metal sample transfer, and more effectively expand the function, it is urgent to develop a new micro-pipetting device and method for the precise transfer of alkali metal elements. Summary of the invention

[0005] In view of the above defects or improvement needs of the prior art, the present invention provides a micropipette device and method for the precise transfer of alkali metal elements, wherein a micropipette device for the precise transfer of alkali metal elements is designed in combination with the characteristics of the alkali metal elements themselves and the process characteristics of their micro-transfer, and the structures of key components such as the anaerobic protection chamber, the alkali metal melting module, the alkali metal pipetting module, the propulsion piston rod, the metal capillary, the metal capillary filament and the first heating unit and their specific settings are studied and designed. Accordingly, the capillary principle and the piston principle are utilized under anaerobic conditions to set the atmosphere of the molten state of the alkali metal elements, so as to realize the transfer of trace alkali metals in the nanoliter level, and thus the device is particularly suitable for the alkali metal filling of chip-level atomic vapor bubbles and the precise injection of alkali metal atoms.

[0006] To achieve the above object, according to one aspect of the present invention, a micropipette device for precisely transferring alkali metal elements is provided, comprising an anaerobic protection chamber and an alkali metal melting module and an alkali metal pipetting module arranged in the anaerobic protection chamber, wherein:

[0007] The alkali metal melting module is used to melt the alkali metal element to be transferred;

[0008] The alkali metal pipetting module includes a propulsion piston rod, a pipette packaging clamp and a metal capillary which are connected in sequence. A glass micropipette is arranged inside the pipette packaging clamp. The propulsion piston rod extends into the glass micropipette. A metal capillary is fixedly connected to the power output end of the propulsion piston rod. The end of the metal capillary not connected to the propulsion piston rod is inserted into the metal capillary. The metal capillary is adapted to the inner diameter of the metal capillary, and the metal capillary slides along the inner wall of the metal capillary under the driving action of the propulsion piston rod to form a piston structure. In this way, by controlling the stroke of the propulsion piston rod, the amount of alkali metal elements extracted by the metal capillary in the alkali metal melting module is the same as the amount of alkali metal elements to be transferred. A first heating unit is arranged on the periphery of the metal capillary, and a first heat preservation unit is arranged on the periphery of the first heating unit. The first heating unit is used to keep the alkali metal elements sucked into the metal capillary in a molten state at all times.

[0009] As a further preferred embodiment, a pipette scale is also provided inside the pipette package holder, and the scale of the pipette scale is arranged along the travel direction of the metal capillary, through which the amount of alkali metal elements sucked into the metal capillary or the amount of alkali metal elements removed by the metal capillary is identified.

[0010] As further preferred, the alkali metal pipetting module further comprises a stroke controller, which is arranged at one end of the pipette package holder away from the metal capillary and is used to limit the propulsion stroke of the propulsion piston rod.

[0011] As further preferred, the first heating unit includes a first heating wire, a first temperature sensing element and a first temperature controller, the first heating wire is spirally sleeved on the outer circumference of the metal capillary, the first temperature controller is used to measure the temperature of the metal capillary and send the measured temperature to the first temperature controller, the first temperature controller controls the heating power of the first heating wire according to the alkali metal element to be transferred, and adjusts the heating power of the first heating wire in real time according to the temperature feedback from the first temperature sensing element, so that the temperature of the metal capillary is consistent with the melting temperature of the alkali metal element to be transferred;

[0012] The first heat-insulating unit comprises a heat-insulating sleeve and a sleeve heat-insulating layer arranged between the inner wall of the heat-insulating sleeve and the first heating wire.

[0013] As further preferred, the metal capillary wire and the metal capillary are both made of hard metal, and the transfer volume of the metal capillary is on the order of ten nanoliters or nanoliters.

[0014] As further preferred, the alkali metal melting module includes a heating chamber, an alkali metal ampoule, a second heating unit and a second insulation unit, the alkali metal ampoule is arranged inside the heating chamber, the second heating unit and the second insulation unit are arranged between the inner wall of the heating chamber and the alkali metal ampoule, the alkali metal ampoule is used to place the alkali metal element, the second heating unit is used to heat the alkali metal element and keep the alkali metal element in a molten state, and the top of the heating chamber is also provided with a hole for opening the alkali metal ampoule.

[0015] As further preferred, the second heating unit includes a second heating wire, a second temperature sensing element and a second temperature controller, the second heating wire is spirally sleeved on the outer circumference of the alkali metal ampoule, the second temperature sensing element is used to detect the temperature of the alkali metal element in the alkali metal ampoule, the second temperature controller controls the heating power of the second heating wire according to the alkali metal element, and adjusts the heating power of the second heating wire in real time according to the temperature feedback from the second temperature sensing element, so that the alkali metal element in the alkali metal ampoule remains in a molten state;

[0016] The second heat-insulating unit comprises a heat-insulating layer arranged between the outer wall of the alkali metal ampoule bottle and the inner wall of the heating chamber and a heat-insulating base at the bottom of the heating chamber.

[0017] As a further preferred embodiment, the invention further comprises a controller, a micro motor and a visual recognition device, wherein the micro motor drives the propulsion piston rod to move under the control of the controller, and the visual recognition device is used to identify the movement process of the metal capillary filament. The controller comprises a PID controller, and the PID controller is used to adjust the power of the micro motor in real time according to the actual movement process of the metal capillary filament and the expected process of the metal capillary filament, so that the propulsion piston rod pushes the metal capillary filament to move according to the expected process, so as to accurately control the amount of alkali metal elements transferred by the metal capillary.

[0018] According to another aspect of the present invention, there is also provided a method for precisely transferring alkali metal elements, which is implemented using the above-mentioned micro-pipette device and comprises the following steps:

[0019] S1 places the alkali metal melting module and the alkali metal pipetting module in the anaerobic protection chamber;

[0020] S2 uses an alkali metal transfer module to melt the alkali metal element to be transferred and keeps the alkali metal element in a molten state;

[0021] S3 adjusts the pushing progress of the pushing piston rod so that the end of the metal capillary away from the pushing piston rod is aligned with the end of the metal capillary tube absorbing the alkali metal element;

[0022] S4: turning on the first heating unit to heat the metal capillary to the melting temperature of the alkali metal element, and keeping the metal capillary at the melting temperature of the alkali metal element;

[0023] S5: inserting the metal capillary into the alkali metal melting module, pulling the push piston rod to control the metal capillary to move along the inner wall of the metal capillary, until the amount of the alkali metal element sucked into the metal capillary is the same as the amount of the alkali metal to be transferred;

[0024] S6: placing one end of the metal capillary tube for absorbing alkali metal elements into the alkali metal filling cavity, pushing the thrust piston rod to control the metal capillary filament to move along the inner wall of the metal capillary tube until all the alkali metal elements absorbed into the metal capillary tube are transferred to the alkali metal filling cavity, thereby completing the transfer of the alkali metal elements.

[0025] As further preferred, step S specifically includes the following steps:

[0026] S51: inputting the amount of alkali metal to be transferred into the controller, and the controller generates a desired course of the metal capillary according to the amount of alkali metal to be transferred;

[0027] S52: the controller controls the micro motor to drive the propulsion piston rod to move according to the desired progress of the metal capillary wire so as to drive the metal capillary wire to move;

[0028] The S53PID controller adjusts the power of the micro motor in real time according to the actual movement progress of the metal capillary identified by the visual recognition device and the expected progress of the metal capillary, so that the thrust piston rod pushes the metal capillary to move according to the expected progress, so as to accurately control the amount of alkali metal elements sucked into the metal capillary until the amount of alkali metal elements sucked into the metal capillary is the same as the amount of alkali metal to be transferred.

[0029] In general, the above technical solution conceived by the present invention has the following technical advantages compared with the prior art:

[0030] 1. The present invention can be effectively applied to the micro-pipetting of the precise transfer of alkali metal elements, can realize the transfer of trace alkali metals in the nanoliter level, can be applied to the alkali metal filling of chip-level atomic vapor bubbles, and can precisely inject alkali metal atoms. It has a wide range of application prospects, and is specifically suitable for the precise transfer of alkali metals in quantum sensors such as atomic magnetometers, atomic clocks, and gyroscopes.

[0031] 2. The present invention studies and designs the structure and specific arrangement of key components such as the anaerobic protection chamber, alkali metal melting module, alkali metal transfer module, push piston rod, metal capillary, metal capillary wire and the first heating unit, and accordingly uses the capillary principle and piston principle under anaerobic conditions to set the atmosphere of the alkali metal element melting state to achieve nanoliter-level trace alkali metal transfer. Therefore, it has the characteristics of high transfer accuracy, simple operation, strong applicability and wide application.

[0032] 3. The present invention utilizes a metal capillary to pass through a metal capillary and can slide and cooperate in the capillary to form a piston structure. The first heating wire heats the alkali metal in the metal capillary into a liquid state, thereby reducing the waste of the alkali metal and preventing it from solidifying to facilitate transfer.

[0033] 4. The metal capillary and metal capillary materials of the present invention are hard metals such as stainless steel. The thickness of the metal capillary and the inner diameter of the metal capillary can be adjusted to adapt to the precise transfer of alkali metal elements in the tens of nanoliters or even nanoliters. The quantitative filling method will reduce the difference in alkali metal element content in each atomic vapor chamber and improve the yield of the atomic vapor chamber.

[0034] 5. Before the alkali metal to be transferred in the alkali metal ampoule of the present invention is transferred, the alkali metal in the alkali metal ampoule needs to be heated into a liquid state by a second heating wire so as to be transferred using an alkali metal pipette.

[0035] 6. The first temperature sensing element, the thermal insulation sleeve and the sleeve thermal insulation layer of the present invention are combined with the first heating wire to perform precise temperature control to keep the alkali metal in a just-melting state, thereby reducing alkali metal evaporation.

[0036] 7. The glass micropipette of the present invention is engraved with a pipetting scale to characterize the stroke of the propulsion piston rod. The glass micropipette is transparent, which is conducive to observing the internal metal capillary filament and the operation of the propulsion piston rod.

[0037] 8. The stroke controller of the present invention is sleeved outside the advancing piston rod to prevent the piston rod from overtravel, so as to prevent the metal capillary from being drawn out of the metal capillary to damage the pipette and waste alkali metal.

[0038] 9. The present invention intelligently controls the stroke of the propulsion piston rod according to the amount of alkali metal elements to be transferred, and has the characteristics of high precision, strong applicability, and simple operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 It is a structural schematic diagram of a micro-pipette device for precisely transferring alkali metal elements according to a preferred embodiment of the present invention;

[0040] Figure 2 It is a structural schematic diagram of an alkali metal liquid transfer module involved in a preferred embodiment of the present invention;

[0041] Figure 3 It is a schematic structural diagram of an alkali metal melting module involved in a preferred embodiment of the present invention.

[0042] In all the drawings, the same figure numbers represent the same technical features, specifically: 1-advancing piston rod, 2-stroke controller, 3-glass micropipette, 4-pipette scale, 5-pipette packaging clamp, 6-metal capillary, 7-metal capillary, 8-capillary sleeve, 9-first heating wire, 10-first temperature sensing element, 11-insulating sleeve, 12-sleeve insulation layer, 21-second heating wire, 22-second temperature sensing element, 23-heating chamber, 24-insulating layer, 25-alkali metal ampoule, 26-alkali metal, 27-insulating base, 31-first temperature controller, 32-second temperature controller, 41-alkali metal filling chamber, 42-filling chamber, 43-anaerobic protection chamber. DETAILED DESCRIPTION

[0043] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0044] like Figure 1As shown, a micropipette device for the precise transfer of alkali metal elements provided by an embodiment of the present invention is specifically suitable for the precise transfer of alkali metals in quantum sensors such as atomic magnetometers, atomic clocks, and gyroscopes. The alkali metals commonly used in quantum sensors are potassium, rubidium, and cesium. The device can realize the transfer of trace alkali metals in the nanoliter order and can be applied to the alkali metal filling of chip-level atomic vapor bubbles and the precise injection of alkali metal atoms. It includes an anaerobic protection chamber 43 and an alkali metal melting module and an alkali metal pipetting module arranged in the anaerobic protection chamber 43, wherein the alkali metal melting module is used to melt the alkali metal element to be transferred; the alkali metal pipetting module includes a propulsion piston rod 1, a pipette packaging clamp 5 and a metal capillary 7 connected in sequence, a glass micropipette 3 is arranged inside the pipette packaging clamp 5, the propulsion piston rod 1 extends into the glass micropipette 3, the power output end of the propulsion piston rod 1 is fixedly connected with a metal capillary filament 6, and the end of the metal capillary filament 6 not connected to the propulsion piston rod 1 is inserted into the metal capillary 7 The metal capillary filament 6 is adapted to the inner diameter of the metal capillary 7, and the metal capillary filament 6 slides along the inner wall of the metal capillary 7 under the driving action of the thrust piston rod 1 to form a piston structure. In this way, by controlling the stroke of the thrust piston rod 1, the amount of alkali metal elements extracted by the metal capillary 7 in the alkali metal melting module is the same as the amount of alkali metal elements that need to be transferred. A first heating unit is provided on the periphery of the metal capillary 7, and a first heat preservation unit is provided on the periphery of the first heating unit. The first heating unit is used to keep the alkali metal elements sucked into the metal capillary 7 in a molten state at all times.

[0045] Specifically, if Figure 2As shown, the alkali metal pipetting module includes a propulsion piston rod 1, and a stroke controller 2 prevents the propulsion piston rod 1 from overtravel. The stroke controller 2 is arranged at one end of the pipette packaging clamp 5 away from the metal capillary 7, and is used to limit the propulsion stroke of the propulsion piston rod 1. More specifically, in the present invention, the stroke controller 2 includes a first limit plate, a second limit plate and a limiting support member, which is fixedly connected to the first limit plate and the second limit plate, and is used to support the first limit plate and the second limit plate. The first limit plate is used to limit the travel distance of the pushing piston rod 1 when the metal capillary 7 absorbs alkali metal elements, so as to prevent the metal capillary 6 from being pulled out of the metal capillary 7. The second limit plate is arranged at one end close to the pipette packaging clamp 5, and is used to limit the travel distance of the pushing piston rod 1 when the metal capillary 7 transfers alkali metal elements, so that when the pushing piston rod 1 moves away from one end of the metal capillary 7 to the second limit plate, the end of the metal capillary 6 that is not connected to the pushing piston rod 1 is just aligned with the extraction end of the metal capillary 7, so that all the alkali metal elements in the metal capillary 7 are transferred. The glass micropipette 3 is engraved with a pipetting scale 4, the scale of which is arranged along the travel direction of the metal capillary 6, and the amount of alkali metal elements sucked into the metal capillary 7 or the amount of alkali metal elements removed by the metal capillary 7 is identified by the pipetting scale 4. The pipette package holder 5 protects and supports the glass micropipette 3, the metal capillary 6 passes through the metal capillary 7, the capillary sleeve 8 is sleeved outside the metal capillary 7, the first heating unit is arranged on the outer periphery of the capillary sleeve 8, and the first heating unit includes a first heating wire 9, a first temperature sensing element 10 and a first temperature controller 31, the first heating wire 9 is spirally sleeved on the outer periphery of the metal capillary 7, more specifically, the first heating wire 9 is wound on the capillary sleeve 8, the first temperature sensing element 10, the insulation sleeve 11 and the sleeve insulation layer 12 are used for temperature control. The first thermostat 31 is used to measure the temperature of the metal capillary 7 and send the measured temperature to the first thermostat 31. The first thermostat 31 controls the heating power of the first heating wire 9 according to the alkali metal element to be transferred, and adjusts the heating power of the first heating wire 9 in real time according to the temperature feedback from the first temperature sensing element 10, so that the temperature of the metal capillary 7 is consistent with the melting temperature of the alkali metal element to be transferred. The first heat preservation unit includes a heat preservation sleeve 11 and a sleeve heat preservation layer 12 provided between the inner wall of the heat preservation sleeve 11 and the first heating wire 9.

[0046] In the present invention, the metal capillary 6 and the metal capillary 7 are made of hard metal such as stainless steel. The thickness of the metal capillary 6 and the inner diameter of the metal capillary 7 can be adjusted to adapt to the precise transfer of alkali metal elements in the tens of nanoliters or even nanoliters. The quantitative filling method will reduce the difference in the alkali metal element content of each atomic vapor chamber and improve the yield of the atomic vapor chamber.

[0047] like Figure 3 As shown, the alkali metal melting module includes a heating chamber 23, an alkali metal ampoule 25, a second heating unit and a second insulation unit. The alkali metal ampoule 25 is arranged inside the heating chamber 23, and the second heating unit and the second insulation unit are arranged between the inner wall of the heating chamber 23 and the alkali metal ampoule 25. The alkali metal ampoule 25 is used to place the alkali metal element, and the second heating unit is used to heat the alkali metal element and keep the alkali metal element in a molten state. The top of the heating chamber 23 is also provided with a hole for opening the alkali metal ampoule 25. The second heating unit includes a second heating wire 21, a second temperature sensing element 22 and a second temperature controller 32. The second heating wire 21 is spirally sleeved on the outer periphery of the alkali metal ampoule 25. The second temperature sensing element 22 is used to detect the temperature of the alkali metal element in the alkali metal ampoule 25. The second temperature controller 32 controls the heating power of the second heating wire 21 according to the alkali metal element, and adjusts the heating power of the second heating wire 21 in real time according to the temperature feedback from the second temperature sensing element 22, so that the alkali metal element in the alkali metal ampoule 25 remains in a molten state. The second heat preservation unit includes a heat preservation layer 24 disposed between the outer wall of the alkali metal ampoule 25 and the inner wall of the heating chamber 23, and a heat insulation base 27 at the bottom of the heating chamber 23.

[0048] More specifically, before the alkali metal 26 to be transferred in the alkali metal ampoule 25 is transferred, the alkali metal in the alkali metal ampoule 25 needs to be heated into a liquid state by the second heating wire 21 so as to be transferred using an alkali metal pipette.

[0049] As a preferred solution of the present invention, the first thermostat and the second thermostat in the present invention are both connected to the controller, and the controller adjusts the first thermostat and the second thermostat to control the heating power of the corresponding heating wire according to the type of the alkali metal element. Accordingly, when the temperature detected by the temperature sensing element is different from the temperature value set by the controller, the controller calculates the temperature error and sends the temperature error to the thermostat, and the thermostat further adjusts the heating power of the heating wire according to the temperature error.

[0050] As a preferred embodiment of the present invention, the first heating wire 9 is evenly arranged along the outer periphery of the metal capillary 7 in a spiral shape, so that the alkali metal elements in the metal capillary 7 are evenly heated, and the corresponding second heating wire 21 is evenly arranged along the outer periphery of the alkali metal ampoule 25 in a spiral shape, so that the alkali metal elements in the alkali metal ampoule 25 are evenly heated. In the present invention, a plurality of first temperature sensing elements and a plurality of second temperature sensing elements are arranged as needed, and a plurality of first temperature sensing elements are evenly arranged along the axial direction of the metal capillary 7, and a plurality of second temperature sensing elements are evenly arranged along the axial direction of the alkali metal ampoule 25.

[0051] like Figure 1As shown, the extraction and transfer of alkali metals in the present invention are both carried out in an anaerobic environment. On the one hand, it prevents the alkali metal elements from being easily oxidized in an aerobic environment. On the other hand, it improves the adaptability of the equipment used to transfer the alkali metal elements, so that more materials are used to prepare devices for transferring alkali metal elements. Specifically, the entire process is carried out in an anaerobic protection chamber 43. The anaerobic protection chamber 43 is used to provide an anaerobic environment to ensure that the alkali metal does not contact the external open environment during the transfer process. At the same time, the transferred alkali metal elements are transferred to the alkali metal filling chamber 41 placed in the anaerobic protection chamber 43. The alkali metal filling chamber 41 is a filling chamber for alkali metal pipetting. The filling chamber 42 is made of glass or glass-bonded silicon to hold the alkali metal.

[0052] As a preferred embodiment of the present invention, the device of the present invention further includes a controller, a micro motor and a visual recognition device. The micro motor drives the propulsion piston rod 1 to move under the control of the controller. The visual recognition device is used to identify the movement process of the metal capillary 6. The controller includes a PID controller. The PID controller is used to adjust the power of the micro motor in real time according to the actual movement process of the metal capillary 6 and the expected process of the metal capillary 6, so that the propulsion piston rod 1 pushes the metal capillary 6 to move according to the expected process, so as to accurately control the amount of alkali metal elements transferred by the metal capillary 7. Among them, the visual device can obtain the actual movement process of the metal capillary 6 by directly identifying the pipetting scale 4. In the present invention, by adopting the PID controller, the alkali metal elements can be accurately extracted once in the transfer process, without adjusting the amount of alkali metal elements sucked by the metal capillary 7 back and forth, so that the whole process is precisely controlled to meet the needs of precise transfer.

[0053] The device of the present invention utilizes the piston principle, the metal capillary wire cooperates with the metal capillary, and the piston rod is pushed to control the metal capillary wire to slide in the metal capillary to transfer the alkali metal. The alkali metal element needs to be heated into a liquid state for transfer; the alkali metal to be transferred in the alkali metal ampoule also needs to be heated into a liquid state by a heating wire before transfer; the alkali metal transfer needs to be carried out in an anaerobic environment to prevent the alkali metal from being oxidized. Therefore, the micro-pipette device for the precise transfer of alkali metal elements of the present invention has a wider application field.

[0054] The working process of the device of the present invention is as follows:

[0055] Step 1: placing the alkali metal melting module and the alkali metal transfer module in the anaerobic protection chamber 43 .

[0056] Step 2: Heat and melt the alkali metal to be transferred. Use an alkali metal transfer module to melt the alkali metal element to be transferred and keep the alkali metal element in a molten state.

[0057] The alkali metal ampoule 25 containing the alkali metal to be transferred is loaded into the vertical heating chamber 23, and the second heating wire 21 heats the alkali metal to a liquid state and keeps the temperature stable. Then, the alkali metal ampoule 25 is opened, and the temperature needs to be kept stable to minimize the volatilization of the alkali metal, and the alkali metal is heated and melted.

[0058] Step three, adjusting the pushing progress of the pushing piston rod 1 so that the end of the metal capillary filament 6 away from the pushing piston rod 1 is aligned with the end of the metal capillary 7 absorbing the alkali metal element.

[0059] Step 4: Turn on the first heating unit to heat the metal capillary 7 to the melting temperature of the alkali metal element, and keep the metal capillary 7 at the melting temperature of the alkali metal element. That is, heat the metal capillary 6 and the metal capillary 7 to the melting temperature of the alkali metal, and precisely control the temperature to keep it stable.

[0060] Step 5: insert the metal capillary 7 into the alkali metal melting module, pull the push piston rod 1 to control the metal capillary filament 6 to move along the inner wall of the metal capillary 7, until the amount of alkali metal elements sucked into the metal capillary 7 is the same as the amount of alkali metal to be transferred. That is, insert the metal capillary 7 into the alkali metal ampoule 25, slowly pull the push piston rod 1 to control the travel of the metal capillary filament 6, and withdraw the pipette from the alkali metal ampoule 25 to complete the pipette to absorb the alkali metal.

[0061] (51) inputting the amount of alkali metal to be transferred into the controller, and the controller generates the desired course of the metal capillary filament 6 according to the amount of alkali metal to be transferred;

[0062] (52) The controller controls the micro motor to drive the propulsion piston rod 1 to move according to the desired progress of the metal capillary filament 6 so as to drive the metal capillary filament 6 to move;

[0063] (53) The PID controller adjusts the power of the micro motor in real time according to the actual movement process of the metal capillary 6 identified by the visual recognition device and the expected process of the metal capillary 6, so that the thrust piston rod 1 pushes the metal capillary 6 to move according to the expected process, so as to accurately control the amount of alkali metal elements sucked into the metal capillary 7 until the amount of alkali metal elements sucked into the metal capillary 7 is the same as the amount of alkali metal to be transferred.

[0064] Step 6: Place the end of the metal capillary 7 that absorbs the alkali metal element into the alkali metal filling cavity 41, and push the advancing piston rod 1 to control the metal capillary 6 to move along the inner wall of the metal capillary 7 until all the alkali metal elements absorbed into the metal capillary 7 are transferred to the alkali metal filling cavity 41, thereby completing the transfer of the alkali metal element. That is, insert the metal capillary 6 and the metal capillary 7 equipped with the alkali metal pipette into the alkali metal filling cavity 41, and push the advancing piston rod 1 as needed according to the pipetting scale 4, so that the alkali metal is discharged from the metal capillary 7 and transferred to the alkali metal filling cavity 41, thereby completing the alkali metal micro-pipetting.

[0065] Step seven, turn off the first heating unit and the second heating unit, and return all components to their original state to facilitate next use.

[0066] In the specific implementation process, it is necessary to select a suitable alkali metal pipetting amount according to the size of the alkali metal filling cavity 41, set the stroke controller 2 to push the piston rod 1 by an appropriate amount to ensure accurate pipetting scale 4 and other parameters, so as to ensure the effective stroke of the metal capillary 6 so that the metal capillary 7 is filled with the alkali metal 26 liquid to be transferred.

[0067] It will be easily understood by those skilled in the art that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A micropipette device for precise transfer of alkali metal elements, characterized in that: It comprises an anaerobic protection chamber (43) and an alkali metal melting module and an alkali metal transfer module arranged in the anaerobic protection chamber (43), wherein: The alkali metal melting module is used to melt the alkali metal element to be transferred; The alkali metal pipetting module comprises a propulsion piston rod (1), a pipette encapsulation clamp (5) and a metal capillary (7) which are connected in sequence. A glass micropipette (3) is arranged inside the pipette encapsulation clamp (5). The propulsion piston rod (1) extends into the glass micropipette (3). A metal capillary (6) is fixedly connected to the power output end of the propulsion piston rod (1). The end of the metal capillary (6) not connected to the propulsion piston rod (1) is inserted into the metal capillary (7). The metal capillary (6) is adapted to the inner diameter of the metal capillary (7). The metal capillary filament (6) slides along the inner wall of the metal capillary (7) under the driving action of the propulsion piston rod (1) to form a piston structure. In this way, by controlling the stroke of the propulsion piston rod (1), the amount of alkali metal elements extracted by the metal capillary (7) in the alkali metal melting module is the same as the amount of alkali metal elements to be transferred. The outer periphery of the metal capillary (7) is provided with a first heating unit, and the outer periphery of the first heating unit is provided with a first heat preservation unit. The first heating unit is used to keep the alkali metal elements sucked into the metal capillary (7) in a molten state at all times. The alkali metal pipetting module further comprises a stroke controller (2), wherein the stroke controller (2) is arranged at one end of the pipette packaging holder (5) away from the metal capillary (7) and is used to limit the propulsion stroke of the propulsion piston rod (1); the stroke controller (2) comprises a first limit plate, a second limit plate and a limit support member, wherein the limit support member is fixedly connected to the first limit plate and the second limit plate and is used to support the first limit plate and the second limit plate, wherein the first limit plate is used to limit the travel of the propulsion piston rod (1) when the metal capillary (7) absorbs the alkali metal element. The second limit plate is arranged at one end close to the pipette packaging holder (5) and is used to limit the travel distance of the push piston rod (1) when the metal capillary (7) transfers the alkali metal element, so that when the end of the push piston rod (1) away from the metal capillary (7) moves to the second limit plate, the end of the metal capillary (6) not connected to the push piston rod (1) is exactly aligned with the extraction end of the metal capillary (7), so that the alkali metal element in the metal capillary (7) is completely transferred; The invention also comprises a controller, a micro motor and a visual recognition device, wherein the micro motor drives the propulsion piston rod (1) to move under the control of the controller, and the visual recognition device is used to identify the movement process of the metal capillary filament (6). The controller comprises a PID controller, and the PID controller is used to adjust the power of the micro motor in real time according to the actual movement process of the metal capillary filament (6) and the expected process of the metal capillary filament (6), so that the propulsion piston rod (1) pushes the metal capillary filament (6) to move according to the expected process, so as to accurately control the amount of alkali metal elements transferred by the metal capillary (7).

2. A micropipette device for precise transfer of alkali metal elements according to claim 1, characterized in that: A pipette scale (4) is also provided inside the pipette package holder (5), and the scale of the pipette scale (4) is arranged along the travel direction of the metal capillary (6). The amount of the alkali metal element sucked into the metal capillary (7) or the amount of the alkali metal element removed from the metal capillary (7) is identified by the pipette scale (4).

3. A micropipette device for precise transfer of alkali metal elements according to claim 1, characterized in that: The first heating unit comprises a first heating wire (9), a first temperature sensing element (10) and a first temperature controller (31); the first heating wire (9) is spirally arranged on the outer circumference of the metal capillary (7); the first temperature controller (31) is used to measure the temperature of the metal capillary (7) and send the measured temperature to the first temperature controller (31); the first temperature controller (31) controls the heating power of the first heating wire (9) according to the alkali metal element to be transferred, and adjusts the heating power of the first heating wire (9) in real time according to the temperature feedback from the first temperature sensing element (10), so that the temperature of the metal capillary (7) is consistent with the melting temperature of the alkali metal element to be transferred; The first heat-insulating unit comprises a heat-insulating sleeve (11) and a sleeve heat-insulating layer (12) arranged between the inner wall of the heat-insulating sleeve (11) and the first heating wire (9).

4. A micropipette device for precise transfer of alkali metal elements according to claim 1, characterized in that: The metal capillary filament (6) and the metal capillary (7) are both made of hard metal, and the transfer volume of the metal capillary (7) is on the order of ten nanoliters or on the order of nanoliters.

5. A micropipette device for precise transfer of alkali metal elements according to claim 1, characterized in that: The alkali metal melting module comprises a heating chamber (23), an alkali metal ampoule (25), a second heating unit and a second heat-insulating unit. The alkali metal ampoule (25) is arranged inside the heating chamber (23). The second heating unit and the second heat-insulating unit are arranged between the inner wall of the heating chamber (23) and the alkali metal ampoule (25). The alkali metal ampoule (25) is used to place alkali metal elements. The second heating unit is used to heat the alkali metal elements and keep the alkali metal elements in a molten state. The top of the heating chamber (23) is also provided with a hole for opening the alkali metal ampoule (25).

6. A micropipette device for precise transfer of alkali metal elements according to claim 5, characterized in that: The second heating unit comprises a second heating wire (21), a second temperature sensing element (22) and a second temperature controller (32); the second heating wire (21) is in a spiral structure and is sleeved on the outer periphery of the alkali metal ampoule (25); the second temperature sensing element (22) is used to detect the temperature of the alkali metal element in the alkali metal ampoule (25); the second temperature controller (32) controls the heating power of the second heating wire (21) according to the alkali metal element, and adjusts the heating power of the second heating wire (21) in real time according to the temperature feedback from the second temperature sensing element (22), so that the alkali metal element in the alkali metal ampoule (25) remains in a molten state; The second heat-insulating unit comprises a heat-insulating layer (24) disposed between the outer wall of the alkali metal ampoule bottle (25) and the inner wall of the heating chamber (23), and a heat-insulating base (27) at the bottom of the heating chamber (23).

7. A method for precisely transferring alkali metal elements, implemented by using the micropipette device according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1: placing an alkali metal melting module and an alkali metal transfer module in an anaerobic protection chamber (43); S2 uses an alkali metal transfer module to melt the alkali metal element to be transferred and keeps the alkali metal element in a molten state; S3: adjusting the pushing progress of the pushing piston rod (1) so that the end of the metal capillary (6) away from the pushing piston rod (1) is aligned with the end of the metal capillary (7) absorbing the alkali metal element; S4: turning on the first heating unit to heat the metal capillary (7) to the melting temperature of the alkali metal element, and keeping the metal capillary (7) at the melting temperature of the alkali metal element; S5: inserting the metal capillary (7) into the alkali metal melting module, pulling the thrust piston rod (1) to control the metal capillary (6) to move along the inner wall of the metal capillary (7), until the amount of the alkali metal element sucked into the metal capillary (7) is the same as the amount of the alkali metal to be transferred; S6: placing one end of the metal capillary (7) that absorbs the alkali metal element into the alkali metal filling cavity (41), pushing the thrust piston rod (1) to control the metal capillary (6) to move along the inner wall of the metal capillary (7) until all the alkali metal element absorbed into the metal capillary (7) is transferred to the alkali metal filling cavity (41), thereby completing the transfer of the alkali metal element.

8. The method according to claim 7, characterized in that Step S5 specifically includes the following steps: S51: inputting the amount of alkali metal to be transferred into the controller, and the controller generates a desired process of the metal capillary filament (6) according to the amount of alkali metal to be transferred; S52: the controller controls the micro motor to drive the propulsion piston rod (1) to move according to the desired progress of the metal capillary filament (6), so as to drive the metal capillary filament (6) to move; The S53PID controller adjusts the power of the micro motor in real time according to the actual movement process of the metal capillary (6) identified by the visual recognition device and the expected process of the metal capillary (6), so that the thrust piston rod (1) pushes the metal capillary (6) to move according to the expected process, so as to accurately control the amount of alkali metal elements sucked into the metal capillary (7) until the amount of alkali metal elements sucked into the metal capillary (7) is the same as the amount of alkali metal to be transferred.

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