Cold and hot stage for laser ablation system

Abstract

The invention belongs to the technical field of laser ablation, and particularly relates to a cold and hot table for a laser ablation system, the cold and hot table comprises a base and a control system, the top of the base is fixedly connected with a cold and hot table main body, the cold and hot table main body is arranged in a U shape, and an unclosed cavity structure is arranged between the base and the cold and hot table main body; a temperature control chamber is fixedly connected to the bottom face of the cooling and heating table body, cooling and heating execution assemblies are arranged in an inner cavity of the temperature control chamber, a plurality of light holes are formed in the temperature control chamber, the cooling and heating execution assemblies are all connected with a control system, and two compressed springs are assembled on the top face, close to the left side, of the cooling and heating table body. Bolts are movably connected to the positions, close to one ends, of the side walls of the compression springs correspondingly and are in threaded connection with the cooling and heating table body. According to the invention, the temperature can be accurately controlled, the uniform temperature, freezing point temperature, inclusion system, composition and salinity test of the inclusion can be realized, and the cold and hot table can also perform laser ablation inductively coupled plasma mass spectrometry analysis on geology, liquid, biology, materials and other samples requiring accurate temperature control under accurate temperature control.

Description

Technical Field

[0001] The invention belongs to the technical field of laser ablation, and in particular relates to a hot and cold stage used in a laser ablation system. Background Art The laser ablation hot and cold stage is a device that combines laser ablation technology with hot and cold stage technology and is used in geology, material science, biology, and semiconductor manufacturing. Its main function is to use laser ablation technology to remove the surface layer of the material while controlling the temperature of the sample to study the behavior of the material under different temperature conditions.

[0002] Inclusions are of great significance for the study of geological processes, because they contain the "mother liquor" of rock formation and mineralization, and can objectively reflect the original appearance of geological history. In 1858, British scholar Sorby proposed the principle and method of inclusion geological thermometer, which led the study of inclusions into the temperature measurement stage. Deich (1955) of France, Smith (1963) of Canada, and Roedder of the United States published many papers on the study of mineralization fluid inclusions, promoting the application of inclusions from single temperature measurement to mineralization fluid research.

[0003] By using a hot and cold stage, the temperature of the inclusion can be precisely controlled, the thermal stability of the packaging material at high or low temperatures and its impact on the overall performance can be studied, the temperature changes in the actual use environment can be simulated, and the performance of the packaging material in the thermal cycle, such as the thermal expansion coefficient and thermal conductivity, can be evaluated. However, most of the hot and cold stages for inclusions currently use a microscope to perform uniform temperature measurement and test the freezing point temperature, but due to structural problems, they cannot be directly used for laser ablation. There is no mature hot and cold stage on the market that can be directly used for laser ablation. Summary of the invention

[0004] The purpose of the present invention is to provide a hot and cold stage for a laser ablation system, which can achieve precise temperature control and realize uniform temperature, freezing point temperature, inclusion system, composition and salinity testing. Moreover, the hot and cold stage can also perform laser ablation inductively coupled plasma mass spectrometry analysis on geological, liquid, biological, material and other samples requiring precise temperature control under precise temperature control.

[0005] The technical solution adopted by the present invention is as follows: A hot and cold stage for a laser ablation system comprises a base and a control system, wherein a hot and cold stage body is fixedly connected to the top of the base, the hot and cold stage body is arranged in a U shape, an unclosed cavity structure is formed between the base and the hot and cold stage body, a temperature control chamber is fixedly connected to the bottom surface of the hot and cold stage body, a hot and cold actuating assembly is arranged in the inner cavity of the temperature control chamber, the hot and cold actuating assembly is connected to the control system, and two compression springs are arranged near the left side of the top surface of the hot and cold stage body.

[0006] Furthermore, bolts are movably connected to the side walls of the compression spring near one end, and the bolts are threadedly connected to the main body of the hot and cold table.

[0007] Furthermore, the compression spring is arranged in a Z shape.

[0008] Furthermore, a sample groove is provided on the top surface of the hot / cold stage body near the left side, and the compression spring abuts against the surface of the sample in the sample groove to fix the sample.

[0009] Furthermore, the cold and hot execution components include a refrigeration tube, a heating tube, a liquid nitrogen tank and a frequency conversion pump arranged in the inner cavity of the temperature control chamber, the two ends of the refrigeration tube and the heating tube pass through the temperature control chamber and the base in sequence, the refrigeration tube and the heating tube are both against the bottom of the cold and hot table body, the end face of the refrigeration tube is fixedly connected with a joint, the joint is divided into an output end and an input end, a delivery pipe is fixedly connected to the joint at one end of the refrigeration tube, the other end of the delivery pipe is connected to the liquid nitrogen tank, the other end of the refrigeration tube is fixedly connected to the joint at the other end of the refrigeration tube with a liquid outlet pipe, the other end of the liquid outlet pipe is connected to the frequency conversion pump, the air outlet of the frequency conversion pump can be connected to the air pipe, and the exhaust gas is used for purging glass lenses, etc.

[0010] Furthermore, a thermocouple is installed on the inner wall of the temperature control chamber, the heating tube and the thermocouple are both connected to the joint, and the wires on the heating tube and the thermocouple are both electrically connected to the control system.

[0011] Furthermore, the control system includes a PID controller and a computer, the PID controller is electrically connected to the heating tube, the thermocouple, and the variable frequency pump, the PID controller is connected to the computer, and the computer includes temperature control software.

[0012] Furthermore, a plurality of light-transmitting holes are provided on the bottom surface of the temperature control chamber, and the light from the transmitted light can be irradiated from below the hot and cold stages through the light-transmitting holes to the lower surface of the sample.

[0013] Furthermore, a liquid level meter is installed in the liquid nitrogen tank.

[0014] The technical effects achieved by the present invention are: A hot and cold stage for a laser ablation system of the present invention can realize precise temperature control, uniform temperature, freezing point temperature, inclusion system, composition and salinity testing through the mutual cooperation among a base, a hot and cold stage body, a temperature control chamber, a hot and cold execution component and a control system, and the hot and cold stage body can also perform laser ablation inductively coupled plasma mass spectrometry analysis on geological (including inclusions), liquids, organisms, materials and other samples requiring precise temperature control under precise temperature control. Compared with the hot and cold stage body used in laser ablation in the prior art, the present solution has better temperature control effect and simpler structure, so as to facilitate later maintenance and expansion. In addition, in combination with the control system, the temperature of the hot and cold stage body and multiple data of the sample during the laser ablation process can be intuitively viewed in real time. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 is a schematic diagram of the overall structure of an embodiment of the present invention; Figure 2 It is a structural schematic diagram of the main body of the hot and cold stage according to an embodiment of the present invention; Figure 3 is a schematic diagram of the internal structure of a temperature control chamber according to an embodiment of the present invention; Figure 4 is a bottom view of a base according to an embodiment of the present invention; Figure 5 It is a schematic diagram of the structure of a compression spring according to an embodiment of the present invention; Figure 6 It is a block diagram of a control system according to an embodiment of the present invention.

[0016] In the accompanying drawings, the components represented by the reference numerals are listed as follows: 1. Base; 2. Hot and cold table body; 3. Temperature control room; 4. Refrigeration tube; 5. Heating tube; 6. Connector; 7. Compression spring; 8. Bolt; 9. Thermocouple; 10. Sample groove; 11. Light hole; 12. Liquid level gauge; 13. Liquid nitrogen tank; 14. Frequency conversion pump; 15. Delivery pipe; 16. Liquid outlet pipe; 17. Cable connector. DETAILED DESCRIPTION

[0017] In order to make the purpose and advantages of the present invention more clearly understood, the present invention is specifically described below in conjunction with embodiments. It should be understood that the following text is only used to describe one or several specific embodiments of the present invention, and does not strictly limit the scope of protection of the specific claims of the present invention.

[0018] like Figure 1-Figure 6 As shown, a hot and cold stage for a laser ablation system includes a base 1 and a control system. A hot and cold stage body 2 is fixedly connected to the top of the base 1. The hot and cold stage body 2 is arranged in a U shape. An unclosed cavity structure is formed between the base 1 and the hot and cold stage body 2. A temperature control chamber 3 is fixedly connected to the bottom surface of the hot and cold stage body 2. Hot and cold actuator components are arranged in the inner cavity of the temperature control chamber 3. Both the hot and cold actuator components are connected to the control system. Two compression springs 7 are installed near the left side of the top surface of the hot and cold stage body 2.

[0019] Among them, the hot and cold actuator components are used to cool and heat the hot and cold table body 2. The hot and cold table body 2 can transfer low and high temperatures to the sample, and the temperature control range can reach -196℃-600℃, with a control accuracy of 0.01℃, thereby achieving the purpose of high-precision temperature control.

[0020] Specifically, the hot and cold stage proposed in this scheme is a special sample stage for laser ablation, which is mainly used for inclusion research and data analysis experiments. The research contents of inclusions under a microscope are usually divided into: shape, color, size, number, distribution, phase state and filling degree of the inclusions. The main instrument used is a microscope with a camera.

[0021] In addition, the homogenization temperature, freezing point temperature, inclusion system, composition and salinity of the inclusions are determined as follows: a. Homogenization method for measuring homogenization temperature Principle: Select gas-liquid two-phase inclusions (inclusions that are single-phase when captured), and use the hot and cold stage body 2 to heat to a certain temperature so that the gas-liquid two-phases are transformed into a single phase, and the phase state (single phase) when the inclusions are formed is restored. The instantaneous temperature at the time of restoration is the homogenization temperature of the inclusions. Main instruments and equipment of the homogenization method: microscopic heating stage, temperature measurement part, light source and microscope, etc.; b. Determination of the freezing point temperature and salinity of inclusions. The freezing method for determining the freezing point temperature uses the principle that salt solutions of different concentrations have different freezing points to determine the freezing point temperature of the liquid phase of the inclusions; the method for measuring the temperature of fluid inclusions is based on detailed observation and identification of various phases (solid phase, liquid phase, gas phase) containing fluids in the inclusions, and by regulating the temperature increase (or decrease) to measure and observe and record the temperature of various instantaneous phase changes of the inclusions, and compare with the experimental phase diagram of the known relevant system to determine the system and composition to which the inclusion fluid belongs. According to the freezing point temperature of the measured inclusions, the fluid salinity is determined according to the temperature-salinity-density phase diagram or parameter table.

[0022] Therefore, the present invention can also be applied to laser ablation inductively coupled plasma mass spectrometry analysis of geological (including inclusions), liquid, biological, material and other samples requiring precise temperature control under precise temperature control.

[0023] like Figure 2 and Figure 5 As shown, the side wall of the compression spring 7 near one end is movably connected with a bolt 8, and the bolt 8 is threadedly connected to the hot and cold stage body 2. The compression spring 7 is made of high carbon steel, stainless steel, alloy steel, etc. These materials have good elasticity and wear resistance and are used to fix the sample or the container of the sample to ensure that the sample can always remain in a stable state during laser ablation or other operations, so that the operator can observe its morphological changes and record data.

[0024] like Figure 5 As shown, the compression spring 7 is arranged in a Z shape. By arranging it in a Z shape, on the one hand, it is convenient to make one end of it abut against the surface of the hot and cold table body 2, so that it can play a fixing role for samples of different sizes. On the other hand, one end of the compression spring 7 is connected by the connecting bolt 8 and is in a tilted state. Therefore, when the other end of the compression spring 7 is pulled upward, the downward pressure of the compression spring 7 will be increased, further playing a role in stable fixing.

[0025] like Figure 2 As shown, a sample groove 10 is provided on the top surface of the hot / cold stage body 2 near the left side, and a compression spring 7 abuts against the sample surface of the sample groove 10 to fix the sample.

[0026] Among them, when the sample is small or in a scattered state, it can be placed in the sample groove 10 to store the sample. The hot and cold stage body 2 is convenient for evenly transferring the temperature to the sample, so as to realize laser ablation of small and scattered samples. In addition, it can also fix containers with a small supporting area.

[0027] like Figure 1 and Figure 3 As shown, the cold and hot execution components include a refrigeration tube 4, a heating tube 5, a thermocouple 9, a liquid nitrogen tank 13 and a frequency conversion pump 14 arranged in the inner cavity of the temperature control chamber 3. The two ends of the refrigeration tube 4 and the heating tube 5 pass through the temperature control chamber 3 and the base 1 in sequence. The refrigeration tube 4 and the heating tube 5 are both against the bottom of the cold and hot table body 2. The end face of the refrigeration tube 4 is fixedly connected with a joint 6, and the joint 6 is divided into an output end and an input end. In actual application, the diameter of the joint 6 is smaller than the diameter of the refrigeration tube 4. A delivery pipe 15 is fixedly connected to the joint 6 at one end of the refrigeration tube 4, and the other end of the delivery pipe 15 is connected to the liquid nitrogen tank 13. A liquid outlet pipe 16 is fixedly connected to the joint 6 at the other end of the refrigeration tube 4, and the other end of the liquid outlet pipe 16 is connected to the frequency conversion pump 14. The air outlet of the frequency conversion pump 14 can be connected to the air pipe, and the exhaust gas is used for purging glass lenses, etc.

[0028] Among them, the frequency conversion pump 14 is provided with a frequency converter, which is the core device for controlling the operating power of the frequency conversion pump 14. By adjusting the frequency and voltage of the motor, the frequency converter can realize precise control of the pump speed; the frequency converter can adjust the working frequency of the motor, thereby changing the speed of the pump. The higher the frequency, the faster the speed, and the flow rate and power will increase accordingly; otherwise, they will decrease; the frequency converter can also adjust the voltage of the motor to optimize the power output and efficiency. When the liquid nitrogen enters the refrigeration tube 4, when the low temperature is transferred to the surface of the hot and cold table body 2, the thermocouple 9 is used for real-time monitoring, and the temperature is fed back to the temperature control software in the computer. When the temperature is about to reach the set range, the frequency converter can be used to control the operating power of the frequency conversion pump 14, reduce the flow rate of liquid nitrogen, and maintain the current temperature. After the liquid nitrogen discharged from the refrigeration tube 4 passes through the frequency conversion pump 14, the gas outlet of the frequency conversion pump 14 can be connected to the gas pipe, and the tail gas is used for purging glass lenses, etc., to achieve the purpose of recycling.

[0029] In addition, if the refrigeration pipe 4 or the variable frequency pump 14 cannot withstand the low temperature of liquid nitrogen, the liquid nitrogen can be first converted into gas by an evaporator and then transported, which can also achieve the low temperature effect.

[0030] like Figure 1As shown, a thermocouple 9 is installed on the inner wall of the temperature control chamber 3, a cable connector 17 is installed on the side wall of the temperature control chamber 3, the heating tube 5 and the thermocouple 9 are electrically connected to the cable connector 17, and the cable connector 17 is electrically connected to the control system.

[0031] Specifically, the thermocouple 9 used in this solution is an E-type thermocouple 9, which has a detection temperature range of -200°C to +900°C, has high sensitivity, and is suitable for applications requiring high precision.

[0032] like Figure 1 and Figure 6 As shown, the control system includes a PID controller and a computer. The PID controller is electrically connected to the heating tube 5, the thermocouple 9, and the variable frequency pump 14. The PID controller is connected to the computer, and the computer includes temperature control software.

[0033] Among them, using a control system to control the temperature of the hot and cold stage body 2 to achieve laser ablation of samples at different temperatures belongs to the existing technology in other fields. The control system needs to be used in conjunction with a specific program. Since it is widely used in the existing technology, the system will not be described in detail in this solution.

[0034] like Figure 4 As shown, the bottom surface 3 of the temperature control chamber is provided with a plurality of light-transmitting holes 11, and the bottom surface of the sample groove 10 is also provided with light-transmitting holes 11, and light can pass through the light-transmitting holes 11 from below the hot and cold stages to illuminate the lower surface of the sample.

[0035] In addition, in actual applications, the compression spring 7 can be removed according to the sample specifications, and the sample can be fixed in the light-transmitting hole 11 in the sample groove 10 by means of a mushroom nail. The specific implementation method will not be described and limited in this solution, and can be selected according to actual needs.

[0036] Among them, a radiator can be installed on the bottom surface of the base 1 according to needs. The radiator adopts a brushless motor cooling fan with large air volume and low noise. No matter whether the hot and cold table body 2 is in a low temperature state or a high temperature state, when it is necessary to restore the room temperature or change the temperature, the radiator can be operated through the PID controller to accelerate the air circulation around the hot and cold table body 2 and realize rapid temperature rise and fall.

[0037] like Figure 1 As shown, a liquid level meter 12 is installed in the liquid nitrogen tank 13. The liquid level meter 12 is used to monitor the liquid level information of the liquid nitrogen inside the liquid nitrogen tank 13, so as to replenish the liquid nitrogen in time. This is a prior art and will not be described in detail in this solution.

[0038] The working principle of the present invention is as follows: firstly, the sample is placed on the hot and cold stage body 2, and then the temperature of the hot and cold stage body 2 is controlled according to the conditions of laser ablation. When the hot and cold stage body 2 needs to be cooled to below zero, the temperature value can be inputted by the temperature control software in the computer, and then the start command is issued to the variable frequency pump 14 through the PID controller. The variable frequency pump 14 is operated to extract liquid nitrogen from the liquid nitrogen tank 13 into the refrigeration pipe 4, and the refrigeration pipe 4 transfers the low temperature to the hot and cold stage body 2. At this time, the temperature change on the hot and cold stage body 2 can be monitored in real time by the thermocouple 9, and the real-time temperature is fed back to the temperature control software. When the temperature of the hot and cold stage body 2 reaches the set range, the power of the variable frequency pump 14 is reduced, and the supply flow rate of liquid nitrogen becomes smaller to maintain the current temperature, and then other operations such as laser ablation are performed on the sample. When the temperature of the hot and cold table body 2 needs to be raised, the temperature value is inputted by the temperature control software in the computer, and the start command is issued to the heating tube 5 through the PID controller, and the heating tube 5 starts to generate heat and transfer the heat to the hot and cold table body 2. When the temperature reaches the set range, the laser ablation and other operations on the sample are started to achieve precise temperature control, uniform temperature, freezing point temperature, inclusion system, composition and salinity testing. Moreover, the hot and cold table body 2 can also perform femtosecond laser ablation analysis on the inclusions under precise temperature control. Compared with the existing hot and cold table body 2 used in laser ablation, this solution has better temperature control effect and simpler structure, which is convenient for later maintenance and expansion. In addition, combined with the control system, the temperature of the hot and cold table body 2 and multiple data of the inclusions during the laser ablation process can be intuitively viewed in real time.

[0039] The above is only a preferred embodiment of the present invention. It should be noted that, for those skilled in the art, several improvements and modifications can be made without departing from the principles of the present invention, and these improvements and modifications should also be considered as the protection scope of the present invention. The structures, devices and operating methods not specifically described and explained in the present invention shall be implemented according to the conventional means in the art unless otherwise specified and limited.

Claims

1. A hot and cold stage for a laser ablation system, characterized in that: The invention comprises a base (1) and a control system, wherein a hot / cold table body (2) is fixedly connected to the top of the base (1), the hot / cold table body (2) is arranged in a U shape, an unenclosed cavity structure is formed between the base (1) and the hot / cold table body (2), a temperature control chamber (3) is fixedly connected to the bottom surface of the hot / cold table body (2), a hot / cold actuating assembly is arranged in the inner cavity of the temperature control chamber (3), and the hot / cold actuating assembly is connected to the control system, and two compression springs (7) are installed near the left side of the top surface of the hot / cold table body (2).

2. The hot and cold stage for a laser ablation system according to claim 1, characterized in that: The side walls of the compression spring (7) are movably connected to bolts (8) near one end, and the bolts (8) are threadedly connected to the hot and cold table body (2).

3. The hot and cold stage for a laser ablation system according to claim 1, characterized in that: The compression spring (7) is arranged in a Z shape.

4. The hot and cold stage for a laser ablation system according to claim 1, characterized in that: A sample groove (10) is provided on the top surface of the hot / cold stage body (2) near the left side for placing a sample, and the compression spring (7) abuts against the surface of the sample in the sample groove (10) for fixing the sample.

5. The hot and cold stage for a laser ablation system according to claim 1, characterized in that: The cold and hot execution assembly comprises a refrigeration tube (4), a heating tube (5), a liquid nitrogen tank (13) and a variable frequency pump (14) which are arranged in the inner cavity of the temperature control chamber (3); the two ends of the refrigeration tube (4) and the heating tube (5) pass through the temperature control chamber (3) and the base (1) in sequence; the refrigeration tube (4) and the heating tube (5) are both against the bottom of the cold and hot table body (2); the end surface of the refrigeration tube (4) is fixedly connected to a joint (6); the joint (6) at one end of the refrigeration tube (4) is fixedly connected to a delivery tube (15); the other end of the delivery tube (15) is connected to the liquid nitrogen tank (13); the joint (6) at the other end of the refrigeration tube (4) is fixedly connected to a liquid outlet tube (16); the other end of the liquid outlet tube (16) is connected to the variable frequency pump (14).

6. The hot and cold stage for a laser ablation system according to claim 5, characterized in that: A thermocouple (9) is installed on the side wall of the temperature control chamber (3), a cable connector (17) is installed on the side wall of the temperature control chamber (3), the heating tube (5) and the thermocouple (9) are both electrically connected to the cable connector (17), and the cable connector (17) is electrically connected to a control system.

7. The hot and cold stage for a laser ablation system according to claim 6, characterized in that: The control system comprises a PID controller and a computer. The PID controller is electrically connected to the heating tube (5), the thermocouple (9), and the variable frequency pump (14). The PID controller is connected to the computer. The computer comprises temperature control software.

8. The hot and cold stage for a laser ablation system according to claim 5, characterized in that: The bottom surface of the temperature control chamber (3) is provided with a plurality of light-transmitting holes (11).

9. The hot and cold stage for a laser ablation system according to claim 5, characterized in that: A liquid level meter (12) is installed in the liquid nitrogen tank (13).

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