Low-temperature objective table for selecting unstable single crystals
By designing a low-temperature stage for unstable single crystals, using temperature control system and microscope technology, the problem of single crystal weathering during the selection and loading process is solved, and a more efficient single crystal structure analysis is achieved.
Patent Information
- Application Number
- CN202510238561.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-03
- Publication Date
- 2025-06-27
AI Technical Summary
The prior art is difficult to effectively select and load unstable and weatherable single crystals, which lead to weathering in low-temperature tests and cannot complete structural analysis.
A low-temperature carrier stage is designed, including a power supply and control system, a microscope holder, an electron microscope, a heat sink and a refrigeration plate. Through the temperature control system and a control unit, a low-temperature stable environment for single crystals is achieved and the risk of weathering is reduced.
By providing a stable low temperature environment, the weathering of single crystals during the selection and loading process is reduced, the success rate of obtaining complete diffraction data of easily weathered crystals is improved, and unnecessary test times and time waste is reduced.
Smart Images
Figure CN120213987A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of crystal selection, and particularly to a low-temperature stage for unstable single crystal selection. Background Technique
[0002] Single crystal diffraction technology is a very important detection means for identifying the structure of single crystals. The quality of the crystal directly determines the quality of the diffraction data and whether its structure can be successfully analyzed ultimately. Therefore, crystal selection is a very important link in the test steps of a single crystal diffractometer, which directly determines the collection of X-ray diffraction data and whether the structure can be successfully analyzed during the single crystal test.
[0003] There is a special type of deliquescent crystal, and its selection and sample loading are extremely difficult. Such crystals will turn from single crystals into powder crystals within a limited time when they leave the mother liquor. Whether the crystal is weathered can only be found out after it is taken out of the mother liquor, so it cannot be predicted in advance. Most crystal weathering is because there are solvent molecules with relatively low boiling points in their unit cells. Once the crystal leaves the mother liquor, the solvent molecules will be lost, resulting in the collapse of the structure. For crystals with a slightly slower weathering rate, they can be appropriately selected and cut, sealed in a glass capillary filled with the mother liquor, then bonded to a glass fiber with a suitable length, and quickly placed on the crystal stage for low-temperature testing. However, it is very difficult to select special crystals with a faster weathering rate, but these crystals often have high scientific research value, and their structure data are usually information that scientific researchers extremely hope to obtain. Currently, for the situation where these crystals cannot be tested due to easy weathering, the solution can only be to replace the solution and re-culture relatively stable crystal samples. The problem of selecting deliquescent crystals has become a technical problem that single crystal testers urgently expect to solve.
[0004] Therefore, we propose a low-temperature stage for unstable single crystal selection to solve the above problems. Summary of the Invention
[0005] The purpose of the present invention is to provide a low-temperature stage for unstable single crystal selection to solve the problems of single crystal weathering during the selection and sample loading processes and the sample loading of cryogenically frozen single crystals mentioned in the above background technique.
[0006] To achieve the above purpose, the present invention provides the following technical solution: A low-temperature stage for unstable single crystal selection, including a power supply and a control system, A microscope support is installed at the top of the power supply and control system, and a display screen is connected and installed on the microscope support. An electron microscope is installed on one side of the power supply and control system. A microscope switch and an indicator light are installed near the microscope support at the top of the power supply and control system. On the other side of the microscope switch and the indicator light, a light source switch and an indicator light are installed. On the other side of the light source switch and the indicator light, a refrigeration switch and an indicator light are installed. A heat sink is installed at the top of the power supply and control system, and a refrigeration chip is installed at the top of the heat sink. A transparent stage is arranged at the top of the refrigeration chip. Arc-shaped grooves are formed on both sides of the transparent stage, and LED lamp beads are arranged in the arc-shaped grooves. A control unit and a temperature control system are arranged in the power supply and control system; The control unit includes: a temperature sensor, a controller, an actuator, and a power supply module; The temperature control system includes: a current control chip, a temperature sensor, an operational amplifier, a comparator, a power transistor, a heat sink, a refrigeration chip, and a control circuit board.
[0007] Preferably, the electron microscope is arranged above the transparent stage, which is convenient for observing the crystals on the transparent stage. The transparent setting can provide uniform illumination for the crystals placed above, so that different positions of the crystals are clearly displayed, reducing shadow and reflection problems.
[0008] Preferably, the microscope switch and the indicator light can control the electron microscope and the display screen, and can conveniently control and turn off the microscope.
[0009] Preferably, the light source switch and the indicator light control the LED lamp beads, and multiple groups of LED lamp beads are arranged at equal distances, enabling the microscope to observe more clearly and facilitating the cutting and selection of single crystals in the transparent stage.
[0010] Preferably, the refrigeration switch and the indicator light are connected to the actuator through a circuit, which is convenient for turning off and on according to the crystal conditions of different single crystals.
[0011] Preferably, the heat sink is arranged horizontally, and the refrigeration chip is arranged vertically to enhance the refrigeration effect.
[0012] Preferably, the actuator controls the heat sink and the refrigeration chip to provide a low-temperature state for the single crystal during selection and cutting, reducing the occurrence of weathering.
[0013] The present invention provides a low-temperature stage for unstable single crystal selection, having the following beneficial effects: (1) Solve the problem of single crystal weathering during the selection and sample loading process The present invention can achieve the purpose of reducing weathering during crystal selection through a heat sink, a thermoelectric cooler, a transparent sample stage, a control unit, and a temperature control system. It enables easily weathered crystals to be in a relatively stable low-temperature state, sucks out the mother liquor at low temperature, and allows these solvent molecules to maintain a stable structure after leaving the mother liquor, reducing the occurrence of collapse. Through microscopic visualization and magnification to a high-definition display, cutting and selection are carried out inside the single-crystal diffractometer, minimizing the exposure time of easily weathered crystals in a room-temperature and air environment. This improves the success rate of obtaining complete diffraction data for easily weathered crystals, reduces the waste of unnecessary time and test times, and reduces the occurrence of weathering during crystal selection and sample loading. At the same time, by virtue of the compact size of this device, it can be directly placed inside the single-crystal diffractometer, minimizing the exposure time of easily weathered crystals in a room-temperature and air environment, thus solving the problem that it is difficult to obtain complete diffraction data for easily weathered crystals.
[0014] (2) Solve the problem of sample loading for cryogenic frozen single crystals Through the combined use of a heat sink, a thermoelectric cooler, and a temperature control system, the present invention can solve the selection of crystals grown by cryogenic freezing. Since the solubility of some crystals is relatively large at room temperature, the temperature is adjusted to an appropriate value for different crystals for selection, reducing the situation where such crystals are quickly dissolved during selection at room temperature, improving the stability of the internal structure of the crystals, and reducing the occurrence of collapse. Thus, the test can be completed, providing higher value for scientific research. It can achieve full-process low-temperature operation and low-temperature testing, effectively solving the dissolution problem of such samples. BRIEF DESCRIPTION OF THE DRAWINGS In order to more clearly illustrate the technical solutions in the embodiments of the present invention or in the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.
[0016] Figure 1 It is a three-dimensional front view schematic diagram of the structure of the present invention; Figure 2 It is a front view schematic diagram of the partial structure of the present invention; Figure 3 It is an enlarged front view schematic diagram of the structure at position A of the present invention; Figure 4 It is a flow schematic diagram of the control unit of the present invention; Figure 5 It is a module flow schematic diagram of the temperature control system of the present invention.
[0017] In the figure: 1. Power supply and control system; 2. Microscope support; 3. Display screen; 4. Electron microscope; 5. Microscope switch and indicator light; 6. Light source switch and indicator light; 7. Refrigeration switch and indicator light; 8. Heat sink; 9. Refrigeration chip; 10. Transparent stage; 11. Arc-shaped groove; 12. LED lamp beads. Specific implementation mode Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0019] At the top of the power supply and control system 1, there is a microscope support 2 installed, and a display screen 3 is connected and installed on the microscope support 2. On one side of the power supply and control system 1, there is an electron microscope 4 installed. Near the microscope support 2 at the top of the power supply and control system 1, there is a microscope switch and indicator light 5 installed. On the other side of the microscope switch and indicator light 5, there is a light source switch and indicator light 6 installed. On the other side of the light source switch and indicator light 6, there is a refrigeration switch and indicator light 7 installed. At the top of the power supply and control system 1, there is a heat sink 8 installed, and a refrigeration chip 9 is installed on the top of the heat sink 8. A transparent stage 10 is arranged on the top of the refrigeration chip 9. Arc-shaped grooves 11 are opened on both sides of the transparent stage 10, and LED lamp beads 12 are arranged in the arc-shaped grooves 11. A control unit and a temperature control system are arranged in the power supply and control system 1.
[0020] The control unit includes: a temperature sensor, a controller, an actuator and a power supply module. Both the control unit and the temperature control system are installed in the power supply and control system 1.
[0021] Specifically, the temperature sensor: can monitor the temperature of the transparent stage 10 in real time and convert it into an electrical signal. In the power supply system, it provides a data basis for subsequent temperature control, so as to set an appropriate temperature according to different mother liquors.
[0022] The controller: receives and processes the signals from the temperature sensor, calculates and judges according to the preset temperature value, and then outputs a control signal to adjust the working state of the actuator. In the temperature control system, the controller can also decide whether to start the heat sink 8 and the refrigeration chip 9 according to the temperature change situation.
[0023] The actuator: takes corresponding actions according to the control signal output by the controller to achieve the purpose of temperature adjustment. In the power supply temperature control system, the actuator can control the heat sink 8, the refrigeration chip 9, etc.
[0024] Power supply module: It provides a stable DC voltage for the entire device. The power supply module has sufficient power output capacity to enable components such as temperature sensors, controllers, and actuators to work properly, and has good voltage stability and anti-interference ability.
[0025] The temperature control system includes: a current control chip, a temperature sensor, an operational amplifier, a comparator, a power transistor, a heat sink 8, a thermoelectric cooler 9, and a control circuit board.
[0026] Specifically, the electron microscope 4 is arranged above the transparent stage 10, facilitating the observation of the crystal above the transparent stage 10.
[0027] Specifically, the microscope switch and indicator light 5 can control the electron microscope 4 and the display screen 3, controlling the switch of the microscope. The light source switch and indicator light 6 control the LED lamp beads 12, and multiple groups of LED lamp beads 12 are arranged at equal intervals, increasing the brightness and visibility above the transparent stage 10. The cooling switch and indicator light 7 are connected to the actuator through a circuit. The controller and the actuator control the heat sink 8 and the thermoelectric cooler 9, turning the temperature on and off during use.
[0028] The temperature control system includes: a current control chip, a temperature sensor, an operational amplifier, a comparator, a power transistor, a heat sink 8, a thermoelectric cooler 9, and a control circuit board.
[0029] Specifically, the current control chip: This is the core component of the current control system, responsible for monitoring and controlling the current flowing through the thermoelectric cooler, and dynamically adjusting the output current according to the preset current value or temperature range to ensure that the thermoelectric cooler operates in the best working state.
[0030] The operational amplifier and the comparator: The operational amplifier is used to amplify the signal of the temperature sensor to improve the accuracy and stability of the signal. The comparator is used to compare the signal of the temperature sensor with the preset reference signal. The operational amplifier and the comparator are used together to compare the amplified temperature signal with the preset reference signal, thereby generating a control signal. When the signal of the temperature sensor reaches or exceeds the preset value, the comparator will output a control signal, triggering the current control chip to adjust the output current.
[0031] The power transistor: The power transistor, as the execution element of current control, is responsible for adjusting the current flowing through the thermoelectric cooler according to the output signal of the current control chip. It has high-speed switching characteristics and low on-resistance, enabling precise control of the current.
[0032] The heat sink: Although the heat dissipation system is not a component directly controlling the current, it has an important impact on the effect of current control, preventing the thermoelectric cooler from overheating during long-term operation, thus maintaining the stability and accuracy of current control.
[0033] Control circuit board: A circuit board that carries all of the above-mentioned electronic components and is responsible for connecting each component to form a complete current control system.
[0034] Specifically, the heat sink 8 is arranged horizontally, and the Peltier cooler 9 is arranged vertically. The horizontally arranged heat sink 8 can provide a larger heat dissipation area, which helps to more effectively disperse and release heat, thereby improving the heat dissipation efficiency. The vertically arranged Peltier cooler 9 can more effectively utilize the vertical space, reduce the floor area of the refrigeration system, and thus improve the space utilization rate.
[0035] Specifically, the display screen 3 is connected to the sensor and the temperature sensor through a circuit, and can monitor the temperature inside the transparent stage 10 in real time and adjust it after monitoring.
[0036] Each component used in this application is a product that can be directly purchased on the market. Its principle and connection method are all well-known prior arts to those skilled in the art, so they will not be elaborated here. Some components in the present invention are only for display, and corresponding circuits and circuit holes are set according to actual situations during actual use and production.
[0037] Working principle: When culturing crystals, solvents with low boiling points and easy volatility such as acetone, methanol, ethanol, and acetonitrile are generally selected. During use, open the glass door of the single crystal diffractometer, place the device inside the single crystal diffractometer, turn on the refrigeration switch and indicator light 7, the light source switch and indicator light 6, and the microscope switch and indicator light 5 in sequence, and adjust the electron microscope 4 to focus above the transparent stage 10. The LED lamp beads 12 in the two groups of arc-shaped grooves 11 provide light for the crystals. Control the temperatures of the heat sink 8 and the Peltier cooler 9 through the control unit and the temperature control system, select an appropriate temperature, suck the mother liquor containing the weathered single crystal sample and drop it on the stage, and then use a crystal picking tool to complete the washing, cutting, and selection of an ideal crystal at low temperature. Transfer the selected crystal to the loop ring and install it on the crystal stage of the single crystal diffractometer, close the glass door of the single crystal diffractometer, and collect crystal data at low temperature.
[0038] The above is all the working principles of the present invention.
[0039] The following points should be noted: First, in the description of this application, it should be noted that unless otherwise specified and defined, the terms "installed", "connected", and "coupled" should be understood in a broad sense, which can be mechanical connection or electrical connection, or the internal communication of two components, and can be directly connected. The terms "upper", "lower", "left", "right", etc. are only used to indicate the relative position relationship. When the absolute position of the object being described changes, the relative position relationship may change. Second, in the drawings of the disclosed embodiments of the present invention, only the structures related to the disclosed embodiments are involved. Other structures can refer to the general design. Without conflict, the same embodiment and different embodiments of the present invention can be combined with each other. Finally, the above are only the preferred embodiments of the present invention and are not used to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
Claims
1. A cryogenic stage for selecting unstable single crystals, comprising a power supply and a control system (1), characterized in that: A microscope support (2) is installed at the top of the power supply and control system (1), and a display screen (3) is installed at the connection of the microscope support (2); an electron microscope (4) is installed on one side of the power supply and control system (1); a microscope switch and indicator light (5) are installed at the top of the power supply and control system (1) near the microscope support (2); a light source switch and indicator light (6) are installed on the other side of the microscope switch and indicator light (5); a refrigeration switch and indicator light (7) are installed on the other side of the light source switch and indicator light (6); a heat sink (8) is installed at the top of the heat sink (8); a refrigeration fin (9) is installed at the top of the refrigeration fin (9); a transparent stage (10) is arranged at the top of the refrigeration fin (9); arc grooves (11) are opened on both sides of the transparent stage (10), and LED lamp beads (12) are arranged in the arc grooves (11); a control unit and a temperature control system are arranged in the power supply and control system (1); The control unit includes: a temperature sensor, a controller, an actuator and a power module; The temperature control system comprises: a current control chip, a temperature sensor, an operational amplifier, a comparator, a power transistor, a heat sink (8), a cooling plate (9) and a control circuit board.
2. A low temperature stage for selecting unstable single crystals according to claim 1, characterized in that: The electron microscope (4) is arranged above the transparent stage (10).
3. A low temperature stage for selecting unstable single crystals according to claim 1, characterized in that: The microscope switch and indicator light (5) controls the display screen (3) and the electron microscope (4).
4. A low temperature stage for selecting unstable single crystals according to claim 1, characterized in that: The light source switch and indicator light (6) control the LED lamp beads (12), and the LED lamp beads (12) are provided in multiple groups, and the multiple groups of LED lamp beads (12) are arranged at equal distances.
5. The low temperature stage for selecting unstable single crystals according to claim 1, characterized in that: The refrigeration switch and indicator light (7) are connected to the controller via a line.
6. A low temperature stage for selecting unstable single crystals according to claim 1, characterized in that: The heat sink (8) is arranged horizontally, and the cooling fin (9) is arranged vertically.
7. The low temperature stage for selecting unstable single crystals according to claim 1, characterized in that: The controller and the actuator are connected to the heat sink (8) and the cooling fin (9) via lines.