CN209387386U - Sample containment chamber for arrayed sample laser heating system - Google Patents

Abstract

The sample sealed cabin used in the array sample laser heating system provided by the utility model includes: a sealed cabin main body for accommodating the array sample; mechanism; the top of the main body of the airtight cabin is provided with a window. The utility model can keep array samples free from pollution and release gas phase substances generated in the heating process.

Description

Sample containment chamber for arrayed sample laser heating system

technical field

The utility model relates to the technical field of material heat treatment, in particular to a sealed cabin for a laser heating system for array samples.

Background technique

Under the framework of material genetic engineering, the preparation and characterization technology of combined array sample library is recognized as one of the search engines and efficient experimental methods to accelerate the discovery of new materials and performance screening, by preparing array sample libraries with discrete or quasi-continuous changes Or the gradient sample library, combined with the characterization technology of material structure and related properties, can quickly obtain the data of sample component screening/performance optimization, and achieve the goal of halving the research and development time and cost. In the material sample library preparation technology, the multi-channel parallel synthesis array sample library is an important branch, which can realize the rapid preparation of multiple samples, and the spatial scale and volume of each independent sample in the sample array are sufficient to meet the existing structural characterization and performance. The requirements of the test technology for the sample, thereby establishing the correlation law between material composition-process-structure-performance.

In the material preparation process, high-temperature heat treatment is an essential part of material preparation, especially for inorganic non-metallic materials such as metals and ceramics, which can realize the chemical reaction of raw materials, crystallization, phase formation, melting and casting of ingots, etc. However, rapid thermal processing technology for arrayed sample libraries required for materials genetic engineering is still blank.

Laser heating technology should become one of the effective technologies for the heating treatment of array sample library due to its fast, directional, and focusable heating characteristics. However, the laser heating speed is fast, resulting in fast material synthesis reactions, crystallization, and melting. For some synthesis reactions that contain precursors such as nitrates and sulfates, corrosive gas phase products are decomposed during high-temperature treatment and released in the reaction. In the cavity, not only the surface of the array sample is easily polluted by the generated gas phase substances, but also the released gas will corrode the equipment. At the same time, due to the high sample density or large number of samples in the array sample, if it is not placed in the cavity but exposed to the air environment to complete the laser heating reaction, it is also easy to be polluted by the environment.

Some laser heating technologies that have been developed so far are only suitable for point-by-point heating of tiny thin film samples with a single laser beam (Patent Document 1), or are only suitable for the preparation of micro-retardation films by multi-beam laser low-temperature thermal etching (Patent Document 2) , or it is only suitable for laser welding and detects overburning of solder joints (Patent Document 3). Obviously, these existing technologies are not applicable to the rapid high-temperature heat treatment of the array sample library, and there is no mechanism for protecting samples and removing reaction gases. Therefore, it is necessary to develop a parallel rapid high-temperature heat treatment device for array sample libraries to meet the technical requirements for rapid synthesis of sample libraries in a clean environment.

current technology

Patent Document 1: Chinese Patent Publication CN 106992131A;

Patent Document 2: Chinese Patent Publication CN 101498805A;

Patent Document 3: Chinese Patent Publication CN 101107501A.

Utility model content

In view of the above, the technical problem to be solved by this utility model is to provide a sample sealing chamber for the array sample laser heating system, which can keep the array sample from contamination and release the gas phase substances generated during the heating process.

In order to solve the above-mentioned technical problems, the sample sealing chamber for the array sample laser heating system provided by the utility model includes: the sealing chamber main body for accommodating the array samples; The degassing mechanism of the gas phase material; the top of the sealed cabin main body is provided with a window.

According to the utility model, the array samples contained in the main body of the sealed cabin can be effectively kept free from environmental pollution and the gaseous phase substances generated during the heating process can be released, and the laser beam can heat the array samples inside the sealed cabin through the window.

Also, in the present utility model, the window can be made of a material that can transmit laser light.

According to the utility model, the laser light can be effectively penetrated through the top window to heat the array samples in the main body of the airtight cabin.

Moreover, in the present utility model, the degassing mechanism is provided with a degassing passage communicated with the main body of the airtight chamber and a vacuum pump connected with the degassing passage.

According to the utility model, the gaseous phase substances generated in the main body of the sealed cabin during the heating process can be removed through the degassing channel through the vacuum pump.

Moreover, in the present utility model, the degassing mechanism is connected to a master control unit, and the master control unit controls the opening and closing of the vacuum pump to control the degassing action of the degassing mechanism.

According to the utility model, the degassing action of the degassing mechanism can be automatically controlled by the master control unit, so as to remove the gas released by the heating reaction of the sample.

Also, in the present utility model, the sample to be heated is prepared or assembled on the substrate in the form of an array sample, the distance between each sample in the array sample on the substrate matches the distance between multiple laser beams, and the substrate is accommodated in the Inside the main body of the airtight compartment.

According to the utility model, the alignment correspondence between the center position of each sample and the center position of the laser beam spot can be realized, and the precise heating effect of "point" to "point" can be achieved. Heating, greatly improving the heating efficiency.

According to the following specific embodiments and with reference to the accompanying drawings, the above content of the present utility model and its purpose, features and advantages will be better understood.

Description of drawings

Fig. 1 shows a schematic structural view of a sample sealed cabin for an array sample laser heating system according to an embodiment of the present invention;

Fig. 2 shows a schematic structural view of an embodiment of an array sample laser heating system applying the sample airtight cabin shown in Fig. 1;

Fig. 3 shows the experimental results of heating with the laser heating system in Fig. 2, taking {5×5} array yellow phosphor sample library heating as an example;

Figure 4 shows another experimental result of heating with the laser heating system in Figure 2, taking the infrared imaging effect of heating a ceramic sample as an example;

Reference signs:

101 - laser;

102-beam expander;

103 - mirror;

104-laser optical path;

105 - thermometer;

106 - camera;

107 - mobile station;

108 - mobile station controller;

109-main control computer;

110 - data acquisition and controller;

111-sample stage;

112-sample sealed cabin;

113-airtight cabin window.

Detailed ways

In order to make the purpose, technical solutions and advantages of the utility model clearer, the utility model will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described here are only used to explain the utility model, and are not intended to limit the utility model.

In order to meet the technical requirements for rapid heating and high-temperature treatment of array material sample libraries, and to develop a universally adaptable sealing and degassing technology and device for parallel laser heating of array samples, the utility model discloses a laser heating system for array samples In order to keep the array sample from contamination and release the gaseous substances generated during the heating process, it includes: the main body of the airtight chamber containing the array samples; A degassing mechanism for gas phase substances; a window is provided on the top of the main body of the sealed cabin, and the laser beam can pass through the window to heat the sample. Further, the utility model also provides a laser heating system for arrayed samples placed in the above-mentioned airtight cabin, including: a laser light source unit that outputs laser light to provide heating energy, and has multiple lasers arranged in parallel or in an array ; The laser beam spot adjustment unit located downstream of the laser light source unit to change the laser spot size; the sample stage for placing the array sample; the temperature measurement unit for measuring the laser heating temperature of the array sample to be heated and feeding back the heating effect ; an image recording unit for recording experimental results; a master control unit connected with the laser light source unit, the temperature measurement unit and the image recording unit. The array sample laser heating system provided by the utility model has the characteristics of parallel multi-beams and adjustable beam spots.

Fig. 1 shows the structure schematic diagram of the sample sealed cabin of the array sample laser heating system of the present invention, including the sealed cabin main body that can accommodate the array sample; it can be used to eliminate the gaseous phase substances generated by the heating reaction of the samples in the sealed cabin during the heating process The degassing mechanism; and the top window structure of the main body of the airtight chamber that allows the laser beam to penetrate.

The array sample may be {A×B} independent samples arranged in an orderly manner, and may be metal or inorganic non-metallic powder, film material and bulk sample.

FIG. 2 shows a schematic structural view of an embodiment of an arrayed sample laser heating system using the sample sealing chamber shown in FIG. 1 . Including laser light source (three parallel lasers)-101, beam expander-102, reflector for laser optical path adjustment-103, laser optical path-104, thermometer-105, camera-106, mobile station-107, mobile station controller -108, main control computer-109, data acquisition and controller-110, sample stage-111, sample airtight cabin-112, airtight cabin window-113. The system can be used for rapid and directional heating of arrayed samples to realize in-situ chemical reactions, crystallization, melting, etc. of samples, and obtain optimized sample heating effects through laser energy feeding and aging changes.

As shown in Figure 2, the laser heating system of this embodiment may include: a laser light source unit with a plurality of lasers 101 arranged in parallel or in an array to provide heating energy; a laser beam spot adjustment unit that can change the laser beam spot Size, for directional heating of samples of different sizes; sample stage, for placing array samples; temperature measurement unit, for measuring the laser heating temperature of array samples to be heated and feeding back the heating effect; image recording unit, for recording laser heating experiments image; and a master control unit connected with the above-mentioned laser light source unit, temperature measurement unit and recording unit. In this embodiment, the master control unit can be the main control computer 109 shown in FIG. 2 .

Further, the laser heating system in this embodiment may also include: a laser optical path adjustment unit, which directs the laser light to the heating point; a sample stage moving unit, which is used to realize the position matching movement and heating positioning of the array sample and the laser beam directional heating point . The above-mentioned master control unit can also be connected with the sample stage moving unit.

As also shown in Figures 1 and 2, the laser heating system of this embodiment may also include: a sample sealing chamber 112 as a sealing and degassing unit, which can keep the array samples from contamination and release gaseous substances generated during the heating process. Specifically, this sample airtight chamber 112 comprises the airtight chamber main body that holds array sample; And be used for getting rid of the degassing mechanism that generates in the said airtight chamber main body due to sample reaction in the heating process; Said airtight chamber main body The top is provided with a window (that is, the airtight cabin window 113 shown in Figure 1).

Preferably, the window may be made of a laser transmissive material. It can effectively make the laser light penetrate the top window to heat the array samples in the main body of the airtight chamber.

More specifically, the degassing mechanism includes a degassing passage communicated with the main body of the airtight chamber and a vacuum pump connected to the degassing passage. The gas phase substances generated in the main body of the airtight chamber during the heating process can be removed by a vacuum pump through the degassing channel.

Further, the degassing mechanism is connected with the main control unit (namely the main control computer 109 in the embodiment shown in FIG. 2 ), through which the general control unit controls the opening and closing of the vacuum pump to control the degassing action of the degassing mechanism.

The main control unit is used to control the changes of laser energy feeding, aging, temperature, position, etc. through the connection with the above-mentioned laser light source unit, temperature measurement unit, image recording unit, sample stage moving unit, sealing and degassing unit, so that the laser Fast, effective and fixed-point heating is achieved for each sample in the array, and gas substances generated during the heating reaction are removed in real time. Moreover, the master control unit can record experimental parameters, heating process parameter changes, heating temperature (power)-time curve, real-time video recording, and playback of experimental results on the screen through the connection with the temperature measurement unit and image recording unit. The utility model can heat several samples at the same time according to the needs, and realize the controllable adjustment of multiple parameters of laser feeding energy, aging, temperature and position, and meet the technical requirements of efficient screening and optimization of heating parameters.

Specifically, as shown in Figure 2, this embodiment shows a three-beam parallel laser heating system as an example (that is, three lasers 101 are arranged in parallel), the sample stage 111 is an array sample stage, and the array samples placed on it for {12×9} combinations. However, the number and arrangement of the lasers and array samples of the present invention are not limited thereto, and can be adjusted as required.

In this embodiment, the sample airtight cabin 112 as a sealing and degassing unit can keep the sample from being polluted and release the gaseous substances generated during the heating process. The upper cover window 113 adopts laser-transmissible materials, such as zinc selenide crystals, etc. , let the laser beam pass through the see-through window to heat the inner array sample. The sample stage 111 is placed in the sealed cabin 112 and connected to a vacuum pump through a pipeline communicating with the sealed cabin 112 . When degassing is required, the main control computer 109 as the master control unit controls the opening of the vacuum pump, and the gas in the sealed cabin 112 can be sucked out.

In addition, in this embodiment, the sample stage moving unit may include a moving stage 107, which may be an X-Y two-dimensional moving stage. The sample stage 111 is placed above the mobile stage 107 and moves synchronously with it. Specifically, the mobile platform 107 can drive the sample stage 111 placed on it to move in the X or Y direction, and the moving guide rails in two directions perpendicular to each other are arranged under it. The driving device is a servo motor or a stepping motor, and the moving distance is based on The demand can be set arbitrarily. As shown in Figure 2, the sample stage moving unit can be connected with the master control unit via the mobile stage controller 108, and under the motion command of the mobile stage controller 108, the mobile stage 107 can be moved by driving the servo motor or stepping motor to drive the The upper sample stage 111 moves to realize the matching motion and positioning heating of the array sample and the laser beam directional heating position.

In the specific operation process, the sample to be heated is first loaded into the array sample stage 111, and then the array sample stage 111 is put into the sample sealed cabin 112, and the heating parameters (target temperature) of the sample at the corresponding position are set in the main control computer 109. , heating rate, holding time, etc.), the laser passes through the window 113 at the top of the sealed cabin 112 to heat the sample. After starting heating, the data acquisition and controller 110 adjusts the output power percentage of the corresponding laser 101 according to the heating parameters of each sample, and the output laser light is irradiated on the sample after passing through the beam expander 102 and the reflector 103, and the data acquisition and controller 110 According to the temperature of the sample collected by the thermometer 105, the output power percentage of the laser 101 is adjusted in real time to ensure that the heating process meets the initial setting, and the camera 106 can observe the heating situation of the sample in real time; when one or a group of samples is heated, the main control computer 109 sends the new position to be heated to the mobile station controller 108, and the mobile station controller 108 controls the sample stage 107 to move to the designated position; the main body of the sample airtight chamber 112 is connected with a degassing unit (connected to a vacuum pump via a pipeline), and the user can Whether the degassing unit is turned on during the heating process is set in the main control computer 109 as required, and when turned on, the degassing unit can suck out the gas in the sample sealing chamber 112 .

The utility model is further described in detail below through specific examples.

Control the adjustment of laser power and the start and run of sample stage movement and temperature and imaging recording. The beam expander 102 changes the beam spot size of the laser through manual adjustment, and performs directional heating on samples of different sizes. The beam expansion range of the spot is 2 to 8 times the original spot size of the laser; The laser is directed vertically (or 90°) to the heating point to maximize the use of laser power; through the laser optical path 104, the zinc selenide single crystal window 113 of the sealed cabin 112 is irradiated onto the array sample stage 111. The temperature of the heating area and the sample state change data obtained by the thermometer 105 and the camera 106 for temperature monitoring are fed back to the main control computer 109 . The infrared temperature detection lens of the thermometer 105 is closely spaced from the array sample unit and the airtight chamber 112 , and a non-contact infrared sensor is used to monitor the temperature stability. The data collection and controller 110 is the intelligent data control center of the whole system, which is used to collect and control laser power and temperature data. Three parallel lasers 101 and three parallel high-temperature thermometers 105 are connected to the data acquisition and controller 110 for communication, so that temperature data at different laser output powers can be obtained, and further connected to the data feedback system of the main control computer 109 to perform PID heating temperature and program precise control. The mobile station controller 108 communicates with the main control computer 109 to accurately control the position of the array sample platform; three parallel high-temperature observation cameras 106 communicate with the main control computer 109 to obtain digital image data during the high-temperature heating process. During the experiment, the experimental parameters, heating process, heating temperature (power)-time curve, real-time video recording of the heating process, and screen image playback are controlled by the main control computer and displayed on the LCD screen in real time.

Taking the three-beam parallel and beam spot adjustable laser heating system of the array sample manufactured according to the example in Figure 2 as the laser heating experimental sample, the working principle and process of the laser heating system of the present invention are as follows: according to the temperature and heating time of the sample heating Requirements, as well as the size of the array sample and the distance between each sample, input and determine the working parameters and position parameters, such as laser heating spot size, target temperature and heating time, choose single beam or two or three laser beams for simultaneous heating, heating point location, etc., the main control computer 109 activates the laser 101 to heat the array sample stage 111 loaded with samples. At the same time, the thermometer 105 measures the temperature data of the heating point in real time, and feeds back the temperature information to the main control computer. The high-temperature observation camera 106 records the heating process of the sample at the heating point in real time, and the data acquisition and controller 110 outputs the laser power and the collected temperature data, and the program control of the heating process is carried out through the main control computer 109 to control the laser power, heating temperature, holding time and two The moving position of the three-dimensional mobile stage is used to make the heating temperature of each sample in the array sample reach the target setting value. Simultaneously record experimental parameters, parameter changes in the heating process, heating temperature (power)-time curve, real-time video recording of the heating process, and screen image playback. The gas products released during the sample heating reaction are discharged out of the airtight chamber through the degassing device in the airtight chamber 112 .

Example 1

A laser heating experiment was carried out on a {5×5} array of yellow phosphor powder samples using the three-beam laser heating system designed and manufactured according to Figure 2. According to the requirement, use a single beam or a combination of two or three laser beams for heating. In the {5×5} array yellow phosphor sample library, the spacing of each sample in the X-axis direction is 14 mm, which is consistent with the spacing of the laser beam, and the spacing of the samples in the Y-axis direction is 12 mm. The movement of the sample matches the heating position of the laser beam. The laser beam penetrates the top window of the airtight chamber to heat the array samples on the sample stage, and the gas phase substances generated during the heating process are removed from the airtight chamber by a vacuum pump. The main control computer 109 makes the heating of each sample in the array samples reach the target set value by adjusting the laser power, heating time and the moving position of the two-dimensional moving stage. The temperature monitoring unit measures the temperature data of the heating point in real time, and feeds back the temperature information to the master control unit. The high-speed camera records the heating process of the sample at the heating point in real time, and is connected with the intelligent display unit to record the experimental parameters, the change of the heating process parameters, the heating temperature (power)-time curve, the real-time recording of the heating process, and the screen image playback. The real-time recorded images of the heating results are shown in Figure 3.

Fig. 3 shows the experimental results of combined heating with the three-beam parallel laser heating system designed and manufactured according to Fig. 2, taking {5×5} array yellow phosphor powder sample library laser heating as an example. Put the {5×5} array sample table into the sample airtight cabin 112, set the heating parameters (target temperature, holding time) of the sample at the corresponding position in the main control computer 109, and the laser passes through the window 113 on the top of the airtight cabin 112 to sample heating. After starting the heating reaction, the used nitrate raw material decomposes, and the corrosive gaseous substances (NO ₂ ) produced are discharged out of the sealed cabin through the vacuum degassing channel of the sealed cabin. In the experiment, the heating temperature range was set to 1800-2000 °C; the heating rate of laser heating was 10 °C/s; the holding time range after heating to the specified temperature was 60-1200 s; the beam expander was adjusted so that the diameter of the laser irradiation spot was 9 mm; the thermometer The sampling interval is 1s.

In Figure 3, for the c1-t1-1 sample of the c1 series, the target heating temperature is 1800°C, and no obvious heating effect appears after holding for 60s. For the c1-t2-1 sample, the holding time is extended to 300s, and the heating effect is obvious. The heating effect of c1-t3-1, c1-t4-1, c1-t5-1 samples is more significant (the color of the heating area becomes darker) with the extension of the holding time.

For c2 series c2-t1-2 samples, the target heating temperature is 1850°C, and there is no obvious heating effect after holding for 60s. For the c2-t2-2 sample, the holding time was extended to 300s, showing an obvious heating effect. For c2-t3-2, c2-t4-2, c2-t5-2 samples, the heating effect is more significant (the color of the heating area becomes darker) as the holding time increases.

For c3, c4, and c5 series samples, the target heating temperatures are 1900°C, 1970°C, and 2000°C, respectively, and obvious heating effects appear within 60 seconds of heat preservation (the color of the heating area becomes darker).

The reason for the above-mentioned difference in heating effect is that when the target heating temperature is low (C1 and C2 series), in a short holding time (such as 60 s), neither the surface temperature nor the internal temperature of the sample reaches the melting point, and the There will be an obvious melting state, and only by further prolonging the holding time can an obvious heating and melting state be observed. When the target heating temperature is high (C3, C4 and C5 series), even in a short holding time (such as 60 s), the surface and internal temperature of the sample have reached or exceeded the melting point temperature, so the sample can be observed Melted state of the surface (heated areas become darker).

Example 2

Taking the heating of ceramic samples as an example, optimize the best observation parameters of the high-speed camera to achieve clear and accurate video recording. Single-beam laser heating is adopted, and the heating power adjustment range is 30-90W. Adjust the beam expander so that the diameter of the laser irradiation spot is 6 mm. According to the working distance of the lens, adjust the camera to the focus position. Selected filter models: wavelength 520 nm (green light) and 650 nm (red light); attenuation filter models: transmittance 2% and 0.1%. The laser beam penetrates the top window of the airtight chamber to heat the array samples on the sample stage, and the gas phase substances generated during the heating process are removed from the airtight chamber by a vacuum pump. The infrared imaging recording effect of the sample heating is shown in Figure 4.

The first group of heating imaging effect comparison: when the attenuation film is not used, only the filter (wavelength 520 nm and 650 nm) is added, if the laser power is heated above 60W, due to the strong radiation emitted by the sample when it is heated to high temperature The halo causes the image spot to appear as a white radial spot, and the shape of the sample itself cannot be observed. As the heating power continues to increase, the halo of radiation light becomes more obvious. In contrast, the halo of radiation light is slightly attenuated by using a filter with a shorter wavelength of 520 nm.

The second group of heating imaging effect comparison: use a filter with a shorter wavelength of 520 nm, and add attenuation sheets with different transmittances (transmittance 2% and 0.1%) in combination. When the combination of attenuating sheets with a transmittance of 2% is used, when the laser power is heated above 90W, the image spot appears as a white radial spot due to the radiation halo of the high-temperature melting sample, and the shape of the sample itself cannot be observed. However, when the combination of attenuating sheets with a transmittance of 0.1% is used, even when the optical power is heated above 90W, the halo of radiation light from the high-temperature melting sample is attenuated, so the positive focus imaging of the heated sample can be seen.

The third group of heating imaging effect comparison: the filter with a longer wavelength of 650 nm is used in combination with attenuation sheets with different transmittances (transmittance 2% and 0.1%). When the combination of attenuating sheets with a transmittance of 2% is used, when the laser power is heated above 60W, the shape of the sample itself becomes difficult to observe due to the radiation halo that appears in the melted sample; when the optical power further increases to above 90W, Due to the intensification of the radiation halo of the sample melted at high temperature, the image spot appears as a white radial spot, and the shape of the sample itself cannot be observed at all. However, when the combination of attenuating sheets with a transmittance of 0.1% is used, even when the optical power is heated above 90W, the halo of the radiation light of the sample melted at high temperature is attenuated, so the positive focus imaging of the heated sample can be seen, but the image The sharpness is not as good as that of short-wavelength (520 nm) filter combination imaging.

Therefore, the results of Example 2 prove that the optimal condition for image recording of ceramic sample heating is to use a shorter wavelength (520 nm) filter combined with a low transmittance attenuation film (transmittance 0.1%).

The above content is a further detailed description of the utility model in conjunction with specific implementation methods, and it cannot be determined that the specific implementation of the utility model is only limited to these descriptions. For those skilled in the art to which the utility model belongs, on the premise of not departing from the concept of the utility model, some substitutions or modifications can also be made to the described embodiments, and these substitutions or modifications should be regarded as belonging to Protection scope of the present utility model.

Claims (5)

1. A sample airtight cabin for an array sample laser heating system, characterized in that it comprises: a capsule body containing the arrayed samples; and A degassing mechanism for removing gas phase substances generated in the main body of the airtight chamber during the heating process; The top of the main body of the sealed cabin is provided with a viewing window. 2 . The sample airtight chamber according to claim 1 , wherein the window is made of a laser-transmissive material. 3 . 3 . The sample airtight chamber according to claim 1 , wherein the degassing mechanism is provided with a degassing passage communicated with the main body of the airtight chamber and a vacuum pump connected with the degassing passage. 4 . 4. The sample airtight chamber according to claim 3, wherein the degassing mechanism is connected to a master control unit, and the master control unit controls the opening and closing of the vacuum pump to control the degassing mechanism of the degassing mechanism. gas action. 5. The sample airtight cabin according to any one of claims 1 to 4, wherein the sample to be heated is prepared in the form of an array sample or assembled on a substrate, and the distance between each sample in the array sample on the substrate is The substrate is accommodated in the main body of the airtight chamber to match the spacing of the plurality of laser beams.