阅读说明：本技术 一种激光加热的单传感器快速扫描量热仪 (Laser heating single-sensor rapid scanning calorimeter ) 是由 周东山 朱逸夫 姜菁 薛奇 罗少川 王晓亮 江伟 季青 于 2019-11-20 设计创作，主要内容包括：本发明公开了一种激光加热的单传感器快速扫描量热仪,包括FSC样品室,位于FSC样品室内用于承载样品的芯片传感器、用于加热样品的激光加热器、用于拍摄样品图像的红外相机、通信终端以及控制电子元件；FSC样品室中心设有一作为光路通道的透视窗口,激光加热器、红外相机均位于透视窗口顶部；红外相机与通信终端连接；控制电子元件一端连接通信终端,另一端分别与激光加热器和芯片传感器连接。本发明快速扫描量热仪首次采用激光加热器对样品进行完全可控的快速加热,并使用红外相机来辅助激光瞄准,避免对样品周围区域加热；相比传统的传感器内加热,能够提供最直接的能量输入,避免传感器加热器和样品之间的热滞后,具有更高的温度控制响应速率,可实现更快的升降温扫描。(The invention discloses a laser-heated single-sensor rapid scanning calorimeter, which comprises an FSC sample chamber, a chip sensor, a laser heater, an infrared camera, a communication terminal and a control electronic element, wherein the chip sensor is positioned in the FSC sample chamber and used for bearing a sample; a perspective window serving as a light path channel is arranged in the center of the FSC sample chamber, and the laser heater and the infrared camera are both positioned at the top of the perspective window; the infrared camera is connected with the communication terminal; one end of the control electronic element is connected with the communication terminal, and the other end of the control electronic element is respectively connected with the laser heater and the chip sensor. The rapid scanning calorimeter of the invention firstly adopts the laser heater to carry out completely controllable rapid heating on the sample, and uses the infrared camera to assist laser aiming, thereby avoiding heating the area around the sample; compare heating in traditional sensor, can provide the most direct energy input, avoid the thermal lag between sensor heater and the sample, have higher temperature control response rate, can realize faster heating and cooling and scan.)

1. A laser heating single-sensor rapid scanning calorimeter is characterized by comprising an FSC sample chamber (1), a chip sensor (2) which is positioned in the FSC sample chamber (1) and used for bearing a sample (200), a laser heater (3) used for heating the sample, an infrared camera (4) used for shooting an image of the sample, a communication terminal (5) and a control electronic component (6);

a perspective window (102) serving as a light path channel is arranged in the center of the FSC sample chamber (1), and the laser heater (3) and the infrared camera (4) are both positioned at the top of the perspective window (102) and can be aligned to a sample (200) in the FSC sample chamber (1);

the infrared camera (4) is connected with the communication terminal (5), and the shot pictures are sent to the communication terminal (5) through infrared imaging; and one end of the control electronic element (6) is connected with the communication terminal (5), and the other end of the control electronic element is respectively connected with the laser heater (3) and the chip sensor (2).

2. The laser-heated single-sensor rapid scanning calorimeter of claim 1, wherein the control electronic component (6) is internally provided with a PID temperature controller (61) for outputting heating power to the laser heater (3), and a data acquisition card (62) for recording a real-time temperature value of the sample fed back by the chip sensor (2);

one end of a PID temperature controller (61) is connected with the communication terminal (5), and the other end is connected with the laser heater (3);

one end of the data acquisition card (62) is connected with the chip sensor (2); the other end is connected with a communication terminal (5).

3. A laser heated single sensor fast scanning calorimeter according to claim 1, wherein the FSC sample chamber (1) comprises a sealed chamber (101), a hot and cold stage (103) located within the sealed chamber (101), and a PCB contact plate (104);

the chip sensor (2) is positioned above the cold and hot table (103), the PCB contact plate (104) is pressed on the chip sensor (2) through an embedded metal contact pin (105), and signal transmission is carried out between the PCB contact plate and an FSC (106) outside the sample chamber through a lead;

a light path channel is reserved in the centers of the cold and hot table (103), the chip sensor (2) and the PCB contact plate (104) and corresponds to the perspective window (102);

one end of the cold and hot platform (103) is connected with a cold source outside the sample chamber through a pipeline, and the other end is connected with an environment control device (107) outside the sample chamber through a lead;

and a gas inlet (108) and a gas outlet (109) are respectively reserved on two sides of the sealed cavity (101).

4. Laser heated single sensor fast scanning calorimeter according to claim 1, characterized in that a heater (21) and a thermopile (22) are provided inside the chip sensor (2).

5. Laser heated single sensor rapid scanning calorimeter according to claim 1, characterised in that the front end of the laser heater (3) is provided with a laser beam guide (31).

6. Laser heated single sensor fast scanning calorimeter according to claim 1, characterised in that the infrared camera (4) is equipped with a microscope lens.

7. A method of laser heating with a single sensor fast scanning calorimeter of claim 1, comprising the steps of:

(1) the FSC sample room (1), the laser heater (3), the infrared camera (4), the communication terminal (5) and the control electronic element (6) are installed;

(2) placing an infrared display card at a sample loading position of a chip sensor (2) in an FSC sample chamber (1), starting a laser heater (3) to carry out laser irradiation, observing a laser heating position through an infrared camera (4) and adjusting laser focusing until a laser spot is brightest;

(3) removing the infrared display card, loading a sample to be detected on the chip sensor (2), starting a laser heater (3) to perform laser irradiation, finely adjusting the position of the sample according to the diameter and the thickness of the sample, and finishing laser position adjustment and laser focusing;

(4) the required heat treatment process is edited through the communication terminal (5), the temperature-time curve is sent to the control electronic element (6) in the form of voltage vs time, the control electronic element (6) drives the laser heater (3) to output heating power according to a voltage vs time signal, meanwhile, the control electronic element (6) receives a sample real-time temperature value fed back by the chip sensor (2), and the sample real-time temperature value is stored and generated to the communication terminal (5) to be compared with a set temperature.

Technical Field

The invention belongs to the field of detection equipment, and particularly relates to a laser heating single-sensor rapid scanning calorimeter.

Background

Ultrafast scanning calorimeter (FSC) Using nanoscale thin film chip Sensors micron-sized samples can be performed up to 10⁶K/s heating and cooling scanning calorimetry research can carry out high-sensitivity detection and regulation on the temperature of a sample through a heater and a thermopile which are arranged in a sensor film. However, there is still a significant thermal resistance between the sample and the heater, and at present, the thermal contact between the sample and the heater is mainly improved by pre-melting the sample or using a heat-conducting glue/oil or the like, but is not applicable to all samples. In addition, the internal heater can heat the sensor around the sample, so that energy loss is caused, and the additional heat capacity of the system is increased. By using laser heating instead of heating by the heater inside the sensor, it is possible to provide energy input to the sample as directly as possible, avoiding thermal lag between the sensor heater and the sample, and greatly reducing the additional heat capacity of the sensor electronics. Although the thermal resistance between the sample and the thermopile still exists, using laser heating, the sample may be placed directly over the thermopile and the coupling between the sample and the thermopile may be maximized, thereby reducing the number of thermopiles needed to obtain an accurate thermal signal, e.g., a single thermopile sensor may be used to detect smaller onesAnd (3) sampling.

Laser heating and rapid scanning calorimeter are combined, the laser melting process of additive manufacturing industry can be simulated, the heating and curing process of printing materials in the 3D printing process can be simulated through experiments, and parameter reference and material performance characterization and screening are provided for industrial production. However, the combination of laser heating and rapid scanning calorimetry is limited to auxiliary heating by using laser, and the heating is not controllable, mainly using laser pulses to perform a temperature jump experiment on a heated sample. A PID control system above 100kHz is required to achieve rapid and controllable laser heating, as well as more accurate laser aiming to avoid heating of areas outside the sample, including sensor heaters and thermopiles, etc.

Disclosure of Invention

The purpose of the invention is as follows: the present invention derives from the need for an improved upgrade of the ultra-Fast Scanning Calorimeter (FSC), and can provide the most direct energy input by completely replacing the sensor internal heater of the conventional FSC with laser heating. The focused heat input heats the sample most quickly, avoids thermal delays between the heater and the sample, and achieves faster cooling after heating is turned off.

In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:

a laser-heated single-sensor rapid scanning calorimeter comprises an FSC sample chamber, a chip sensor, a laser heater, an infrared camera, a communication terminal and a control electronic element, wherein the chip sensor is positioned in the FSC sample chamber and used for bearing a sample;

the center of the FSC sample chamber is provided with a perspective window serving as a light path channel, and the laser heater and the infrared camera are positioned at the top of the perspective window and can be aligned with a sample in the FSC sample chamber;

the infrared camera is connected with the communication terminal and sends the shot picture to the communication terminal through infrared imaging; and one end of the control electronic element is connected with the communication terminal, and the other end of the control electronic element is respectively connected with the laser heater and the chip sensor.

The communication terminal receives an infrared imaging photo shot by an infrared camera, assists a laser heater to focus and accurately aims at a sample for heating; the control electronic component controls the heating power of the laser heater on one hand, and obtains the sample temperature information fed back by the chip sensor in real time on the other hand, so as to provide information for adjusting the heating power of the laser heater in the next step.

Specifically, a PID temperature controller for outputting heating power to the laser heater and a data acquisition card for recording a real-time temperature value of a sample fed back by the chip sensor are arranged in the control electronic element;

one end of the PID temperature controller is connected with the communication terminal, and the other end of the PID temperature controller is connected with the laser heater; the system comprises a communication terminal control page and a PID temperature controller, wherein the communication terminal control page is used for sending heating power information of a laser heater to the PID temperature controller;

one end of the data acquisition card is connected with the chip sensor; the other end of the laser heater is connected with a communication terminal, and the data acquisition card receives the real-time temperature value of the sample fed back by the chip sensor, stores the real-time temperature value and generates the real-time temperature value to the communication terminal so as to provide information for next step of adjusting the heating power of the laser heater.

Specifically, the FSC sample chamber comprises a sealed cavity, a cold and hot platform and a PCB contact plate, wherein the cold and hot platform and the PCB contact plate are positioned in the sealed cavity;

the chip sensor is positioned above the cold and hot table, the PCB contact plate is pressed on the chip sensor through an embedded metal pin, and signal transmission is carried out between the PCB contact plate and the FSC outside the sample chamber through a lead;

a light path channel is reserved in the centers of the cold and hot table, the chip sensor and the PCB contact plate and corresponds to the perspective window;

one end of the cold and hot platform is connected with a cold source outside the sample chamber through a pipeline, and the other end of the cold and hot platform is connected with an environment control device outside the sample chamber through a lead;

and a gas inlet and a gas outlet are respectively reserved on two sides of the sealed cavity.

Specifically, a heater and a thermopile are arranged in the chip sensor.

Further, in order to avoid the chip sensor from being mechanically vibrated by the laser heater to generate noise, a laser beam guide such as an optical fiber may be used.

Further, the infrared camera is provided with a microscope lens.

The invention also provides a method for carrying out laser heating by the laser heating single-sensor rapid scanning calorimeter, which comprises the following steps:

(1) the FSC sample chamber, the laser heater infrared camera, the communication terminal and the control electronic element are installed;

(2) placing an infrared display card at a sample loading position of a chip sensor in an FSC sample chamber, starting a laser heater for laser irradiation, observing a laser heating position through an infrared camera and adjusting laser focusing until a laser spot is brightest;

(3) removing the infrared display card, loading a sample to be detected on the chip sensor, starting a laser heater to perform laser irradiation, finely adjusting the position of the sample according to the diameter and the thickness of the sample, and finishing laser position adjustment and laser focusing;

(4) the required heat treatment process is edited through the communication terminal, the temperature-time curve is sent to the control electronic element in the form of voltage vs time, the control electronic element drives the laser heater to output heating power according to a voltage vs time signal, meanwhile, the control electronic element receives a sample real-time temperature value fed back by the chip sensor, and the sample real-time temperature value is stored and generated to the communication terminal to be compared with the set temperature.

Has the advantages that:

the rapid scanning calorimeter of the invention firstly adopts the laser heater to carry out completely controllable rapid heating on the sample, and uses the infrared camera to assist laser aiming, thereby avoiding heating the area around the sample; compared with the traditional heating in the sensor, the sensor can provide the most direct energy input; the focused heat input can heat the sample most quickly, avoid thermal lag between the sensor heater and the sample, have higher temperature control response rate, and can realize faster temperature rise and fall scanning.

Drawings

The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.

Fig. 1 is a schematic view of the overall structure of the laser heating rapid scanning calorimeter of the invention.

FIG. 2 is a schematic diagram of the sample chamber structure of the laser heating rapid scanning calorimeter of the present invention.

Fig. 3A is a graph of the melting and solidification process of Al7075 particles as observed by a conventional ultrafast scanning calorimeter.

Fig. 3B is a diagram of the melting and solidification process of Al7075 particles as observed by a laser-heated rapid scanning calorimeter of the present invention.

Fig. 4A is a measured temperature vs time curve of the laser heating rapid scanning calorimeter and a built-in heater of the sensor.

Fig. 4B is a heating start-up process curve of the laser heating rapid scanning calorimeter and the built-in heater of the sensor.

Wherein each reference numeral represents: 1 FSC sample chamber; 101 sealing the cavity; 102 a perspective window; 103, a cold-hot table; 104 a PCB contact plate; 105 metal pins; 106 FSC; 107 an environmental control device; 108 a gas inlet; 109 a gas outlet; 2, a chip sensor; 21 a heater; 22 a thermopile; 3, a laser heater; 31 a laser beam guide; 4, an infrared camera; 5, a communication terminal; 6 control electronics; 61 PID temperature controller; 62, a data acquisition card; 200 samples.

Detailed Description

The invention will be better understood from the following examples.

The structures, proportions, and dimensions shown in the drawings and described in the specification are for understanding and reading the present disclosure, and are not intended to limit the scope of the present disclosure, which is defined in the claims, and are not essential to the skilled in the art. In addition, the terms "upper", "lower", "front", "rear" and "middle" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the relative positions may be changed or adjusted without substantial technical changes.

As shown in fig. 1 and 2, the rapid scanning calorimeter of the present invention comprises an FSC sample chamber 1, a chip sensor 2 located in the FSC sample chamber 1 for carrying a sample 200, a laser heater 3 for heating the sample, an infrared camera 4 for taking an image of the sample, a communication terminal 5, and control electronics 6.

The center of the FSC sample room 1 is provided with a perspective window 102 as a light path channel, and the laser heater 3 and the infrared camera 4 are both positioned at the top of the window 102 and can be aligned with a sample 200 in the FSC sample room 1.

The infrared camera 4 is connected with the communication terminal 5, and sends the shot pictures to the communication terminal 5 through infrared imaging; and one end of the control electronic component 6 is connected with the communication terminal 5, and the other end of the control electronic component is respectively connected with the laser heater 3 and the chip sensor 2. The control electronic component 6 is internally provided with a PID temperature controller 61 for outputting heating power to the laser heater 3 and a data acquisition card 62 for recording the real-time temperature value of the sample fed back by the chip sensor 2.

One end of the PID temperature controller 61 is connected with the communication terminal 5, and the other end is connected with the laser heater 3; the system comprises a communication terminal control page and a PID temperature controller, wherein the communication terminal control page is used for sending heating power information of a laser heater to the PID temperature controller;

one end of the data acquisition card 62 is connected with the chip sensor 2; the other end is connected with a communication terminal 5, and the data acquisition card receives the real-time temperature value of the sample fed back by the chip sensor, stores the real-time temperature value and generates the real-time temperature value to the communication terminal, so as to provide information for next adjustment of the heating power of the laser heater.

The FSC sample chamber 1 comprises a sealed cavity 101, a cold and hot table 103 and a PCB contact plate 104, wherein the cold and hot table 103 is positioned in the sealed cavity 101; the chip sensor 2 is positioned above the cold and hot table 103, the PCB contact plate 104 is pressed on the chip sensor 2 through an embedded metal pin 105, and signal transmission is carried out between the PCB contact plate and an FSC106 outside the sample chamber through a lead; an optical path channel is reserved in the centers of the cold and hot table 103, the chip sensor 2 and the PCB contact plate 104 and corresponds to the perspective window 102.

One end of the cold and hot platform 103 is connected with a cold source outside the sample chamber through a pipeline, and the other end is connected with an environment control device 107 outside the sample chamber through a lead; a gas inlet 108 and a gas outlet 109 are respectively reserved on two sides of the sealed cavity 101, different atmospheres or gas purging is used from the gas inlet and the gas outlet according to different use requirements, and in order to avoid sample temperature fluctuation caused by gas flow turbulence, a molecular valve or other gas valves which can be used for ultra-slow gas flow fine adjustment can be used.

The chip sensors 2 can be all chip sensors (XEN393, xenon Integration) containing thermocouples available to the ultra-fast scanning calorimeter. The chip sensor has a silicon nitride film containing a heater 21 for additional ultrafast scanning calorimetry and a thermopile 22 providing a temperature signal in volts for controlling and recording the temperature of the sample. The sample is placed on the heater and thermopile and the sample may be any particulate, 1-500 μm diameter spheroidal particle, for example, the international organization for standardization ISO recommends powder particles (20-200 μm diameter) for additive manufacturing to be perfectly suitable for the present invention. To achieve faster temperature control, small particle samples are preferred to avoid thermal hysteresis problems inside the sample. Unlike conventional rapid calorimeters, where the internal heater of the sensor is not used for sample heating, the modular structure of the present invention allows for the rapid re-coupling of the internal heater into a single sensor, even into a differential ultrafast scanning calorimetry setup, to simulate a laser heating process, which facilitates the quantitative measurement of actual heat flow.

The use method of the rapid scanning calorimeter comprises the following steps: a sample 200 is loaded on the chip sensor 2, the laser heater 3 is turned on, and the temperature of the sample is observed through the infrared camera 4 so as to adjust the aiming focus of the laser; a temperature program (temperature-time curve) required by setting is set on a user interface of the communication terminal 5 and sent to a control electronic element 6 (a National instruments 6365 data acquisition card, an SRS SIM960 PID controller), a PID temperature controller 61 for outputting heating power to the laser heater 3 and a data acquisition card 62 for recording a real-time temperature value of a sample fed back by the chip sensor 2 are arranged in the control electronic element 6; the PID temperature controller 61 outputs heating power to the laser heater 3 according to the received set value, and the data acquisition card 62 receives the real-time temperature value of the sample fed back by the thermopile 22 in the chip sensor 2, stores and generates the real-time temperature value to the communication terminal 5, and provides information for next adjustment of the heating power of the laser heater 3.

In the laser heating process, only the temperature value of the sample is recorded, but the specific absorbed energy value of the sample cannot be measured, so that the temperature program can be repeated by using the heater 21 inside the chip sensor 2 to carry out an ultrafast scanning calorimetry experiment, and the change of heat flow when the same temperature change of the sample is realized is recorded, thereby calculating the change of physical parameters such as heat capacity and the like.

The power of the laser heater 3 (MXL-III-880 infrared laser manufactured by Changchun new industry photoelectric technology Co., Ltd.) is adjusted by the PID temperature controller 61 to adjust the input voltage value, and the laser heater adjusts the corresponding output power according to the input voltage. An infrared camera 4(FLIR SC7000 infrared camera is provided with a 7-fold microscope lens) is used for observing the temperature change of the sample, and the laser aiming is judged according to the heating of the sample. If an ultra-fast infrared imaging camera (above 10 kHz) is used, the temperature of the sample in the laser heating experiment can be recorded at the same time and compared with the temperature value fed back by the sensor thermopile 22.

The user interface on the communication terminal (PC/laptop/tablet etc.) edits the required thermal treatment process (temperature vs time) which temperature-time curve will be provided to the control electronics of the device in the form of voltage vs time. The control electronics modulate the power of the laser through a PID temperature controller, setting PID output settings according to the voltage input range of the laser heater. For example, if the input voltage to the laser heater is 0-1V (corresponding to laser power from 0-100%), then the PID output is set to 0 to 1. The user can change the PID settings from laser to laser. The control electronic element outputs voltage to the laser according to an experimental program, the laser heats a sample, the thermopile on the chip sensor measures temperature and feeds the temperature back to the control electronic element according to a voltage value, when the voltage of the thermopile is higher or lower than a set value, the PID controller of the control electronic element correspondingly adjusts the driving voltage of the laser to complete a set temperature-time curve, the data acquisition card records the temperature change of the sample in the experimental process, and sends the data to the communication terminal for storage and further analysis. To achieve fast temperature control, the control electronics require electronics with extremely high response rates, with a minimum bandwidth of 100 kHz.

The user interface is programmed using Labview software, has been widely used in existing FSC devices, and has been improved according to use. The commercial laser heater who buys has the laser controller to the output of input voltage value control laser, only need with the control electronic component of this application with the laser controller, and give with certain voltage, can control laser output and heat. This application mainly uses laser heater (replaces chip sensor internal heating ware) to heat the sample, according to thermopile voltage feedback's sample temperature signal, carries out fast control and feedback laser heater through the PID controller to realize quick controllable program heating.

To avoid the chip sensor from being mechanically vibrated by the laser and thereby generating noise, a laser beam guide such as an optical fiber (CNI polarization maintaining fiber) may be used. Fixing the optical fiber to the sample chamber may reduce the wobble of the laser beam on the sample with a corresponding reduction in interference with the calorimetric signal. Of course, laser beam directors are only suitable for certain types of lasers and require the addition of a light focusing element behind the director.

Focusing the laser directly on the sample can provide maximum energy to the sample and avoid heating surrounding sensor elements. The method can be used for assisting laser aiming and focusing through an infrared imaging camera, and comprises the following specific experimental steps: firstly, placing an infrared display card under an infrared camera, carrying out laser irradiation, observing a laser heating position through the infrared camera, and adjusting laser focusing (laser focusing lens adjustment) until a laser point is brightest (the diameter of the laser point is about 8 mu m); placing a sample (the diameter is about 15 mu m) at the position of an infrared display card, raising the temperature of the sample by laser irradiation, finely adjusting the position of the sample according to the diameter and the thickness of the sample (fine adjustment of a microscope stage), positioning a focused laser point at the center of the sample, and completing laser position adjustment and laser focusing. In addition, infrared imaging is carried out to record the temperature of the sample, and meanwhile, the thermopile on the sensor also measures the internal temperature of the sample, so that comparison can be carried out. The infrared thermal imager can detect about 100x100 μm under corresponding magnification²Thermal radiation of the sensor area. If the temperature of the sample particles and the sensor are to be recorded in real time during the test, an infrared imaging camera with a high frame rate and high sensitivity is required, e.g. approximately 7ms is required to heat from room temperature to 1000K at a rate of 100000K/s, and at least 1 frame per 10K is required to have a frame rate of at least 10 kHz.

In conventional ultrafast scanning calorimetry, the heater of the sensor is placed in the thin film, so that there is a significant thermal resistance between the sample and the heater, and the heater also heats the sensor around the sample at the same time. Laser heating can then provide energy to the sample as directly as possible by focusing and appropriate aiming, avoiding thermal lag between the sensor heater and the sample. In addition, laser heating can also avoid coupling of the sensor heater with the thermopile. The thermal resistance between the sample and the thermopile is still present and there is no way to remotely measure the temperature of the sample faster and more accurately so far. But with laser heating the sample can be placed directly over the thermopile and the coupling between the sample and the thermopile can be increased to the maximum possible, thereby reducing the number of thermopiles needed to obtain an accurate thermal signal, e.g. a single thermopile sensor can be used to detect smaller samples. Ultra-fast temperature control allows any linear, non-linear temperature-time thermal processing procedure up to 1000000K/s or faster to be performed.

The temperature of the thermopile will be recorded during execution of the user-set temperature profile, and when an endothermic or exothermic phase transition occurs, the temperature of the sample will deviate from the set value due to latent heat to present a corresponding endothermic or exothermic peak indicating the melting or crystallization process occurring in the sample. The information has important value in the fields of additive manufacturing, basic theory research and industrial application research which need ultra-rapid heat treatment. The ultrafast scanning calorimeter can quantitatively analyze the change of heat flow in a sample, and after a laser heating experiment, the experiment can be repeated by using a heater inside the sensor to obtain quantitative heat flow data so as to perform heat capacity analysis. And the temperature of the sample under the same condition can be provided by matching with a rapid infrared imaging camera, and is compared with the temperature data measured by the thermopile.

Laser pulses have been used to heat the sample and record the sample heating temperature via a thermocouple, but the heating process is not controllable. Except that the sample temperature was recorded after the laser pulse was emitted. The invention firstly feeds the temperature measured by the thermocouple back to the laser controller and correspondingly adjusts the laser power in real time and rapidly, so that the laser heating is completely controllable heating. The speed of receiving and adjusting the signals is very fast, the following experiment results show that the controllable fast temperature rise and drop program can be realized, the thermal hysteresis phenomenon is eliminated, and the temperature regulation response rate and the controllable temperature rise and drop rate are improved by one order of magnitude. Meanwhile, independent laser heating can not obtain equivalent thermal physical information of heat flow and heat capacity, the invention can switch between laser heating and heating of a traditional FSC internal heater at any time, and the FSC is used for repeating a temperature vs time program recorded during laser heating, so that data such as heat flow, heat capacity and the like with physical significance are obtained. In addition, laser heated single sensor fast scanning calorimeters can achieve higher scan rates using a single sensor relative to conventional FSCs using two sensors (reference and sample sensors).

Fig. 3A and 3B show the melting and crystallization processes of two adjacent Al7075 particles observed by a conventional ultrafast scanning calorimeter and a laser heating calorimeter of the present invention, respectively. The sample is subjected to temperature rise and drop experiments at different scanning rates (conventional internal sensor heating and controllable laser heating), and melting peaks and crystallization peaks of the sample are observed, and the results show that 1) the laser heating rapid calorimeter can realize controllable rapid scanning, and the highest scanning rate (such as 100,000K/s in figure 3B) of the laser heating rapid calorimeter can be higher than that of a conventional ultrafast scanning calorimeter (10,000K/s in figure 3A) by one order of magnitude; 2) when a conventional internal sensor is heated, a melting peak of a sample moves to a high temperature along with the increase of a scanning rate, which indicates that obvious thermal hysteresis exists between the sample and a heater, and in a laser heating experiment, the melting peak moves to a low temperature along with the increase of the scanning rate, and a crystallization peak moves to a high temperature along with the increase of the scanning rate, which indicates that the temperature of the sample can be ensured to be higher than the temperature of the sensor by laser heating, so that the thermal hysteresis between the sample and the heater is avoided, and a more accurate thermal analysis result is obtained.

Fig. 4A and 4B are graphs showing the comparison of the temperature control performance of the laser heating and the sensor built-in heater. Wherein the temperature increase/decrease rate is 10,000K/s, fig. 4A is a time curve of the actually measured temperature vs, and fig. 4B is a heating start-up process. It can be seen from fig. 4A that the response rate of the laser heating temperature control is fast enough to allow fast temperature compensation when the sample melts and crystallizes, so that the heating curve conforms to the set program, while the thermal hysteresis of the heater built in the sensor (fig. 4B) and the sample, and a significant temperature jump can be seen on the heating curve. As can be seen in fig. 4B, the laser heating can complete temperature adjustment and stabilization within 0.2ms, while the built-in heater needs 2m to achieve temperature adjustment, and can complete overshoot to reach a stable temperature after 4.5ms, and the temperature control response rate of the laser heating is about one order of magnitude faster than that of the sensor built-in heater.

The present invention provides a method and a thought of a laser heating single-sensor fast scanning calorimeter, and a method for implementing the technical scheme has many methods and ways, the above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.