CN220399318U - Ultra-fast differential scanning calorimetric and laser Raman spectrum combined testing device - Google Patents
Ultra-fast differential scanning calorimetric and laser Raman spectrum combined testing device Download PDFInfo
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- CN220399318U CN220399318U CN202321862544.XU CN202321862544U CN220399318U CN 220399318 U CN220399318 U CN 220399318U CN 202321862544 U CN202321862544 U CN 202321862544U CN 220399318 U CN220399318 U CN 220399318U
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Abstract
The utility model provides a combined testing device for ultra-fast differential scanning calorimetric and laser Raman spectroscopy, and belongs to the field of high polymer material research. The problems that the existing commercial equipment of the ultrafast differential scanning calorimeter and the laser Raman spectrometer are independently used, and the in-situ analysis of the sample by the combination of the two commercial equipment cannot be realized temporarily are solved. The system comprises a spectrometer sample stage, an ultrafast differential scanning calorimeter, a control system, a Raman spectrometer, a laser Raman microscope, a laser optical system, a detector and a Raman spectrum structure, wherein the Raman spectrometer sample stage is provided with the ultrafast differential scanning calorimeter, the control system is connected with the Raman spectrometer and the ultrafast differential scanning calorimeter, the laser Raman microscope, the laser optical system, the detector and the Raman spectrum structure of the Raman spectrometer are sequentially connected, a sample is arranged in the ultrafast differential scanning calorimeter, and the laser Raman microscope is positioned above the ultrafast differential scanning calorimeter to emit laser to irradiate the sample. The ultra-fast differential scanning calorimeter is subjected to miniaturization customization, and is placed on a spectrometer sample stage, so that the ultra-fast differential scanning calorimeter can be used in combination with a Raman spectrometer.
Description
Technical Field
The utility model belongs to the field of high polymer material research, and particularly relates to a combined testing device for ultra-fast differential scanning calorimetric and laser Raman spectroscopy.
Background
With the rapid development of polymer material research, the more stringent the requirements for higher level characterization techniques. An ultrafast differential scanning calorimeter is a novel high polymer material thermodynamic characterization device which is paid attention to in recent years. Ultra-fast differential scanning calorimeter technology subjects the sample to ultra-high cooling and heating rates, which are well suited for the characterization of new materials and optimization of the production process. It enables a more careful study of the crystallization process, the phase structure, and the crystallization kinetics of the polymer. For a small amount of samples, the rapid crystallization process can be directly measured, the mechanism of the additive close to the production condition can be studied, and the material can be comprehensively thermally analyzed in a short time.
There are many characterization means for the microstructure of the polymer material. Spectroscopic characterization devices are widely used for in situ characterization due to their non-contact, non-destructive nature. For example, X-ray, raman, infrared, etc. are all the most common means of characterizing the microstructure of polymeric materials. The raman spectrum can experimentally determine the chemical properties of the polymer, such as structural units, end groups, branching types, additives, impurities, and the like, the interaction force field between molecules, the orientation of molecular chains, and the like, and obtain a large amount of structural information about the polymer material. The laser spot of a raman spectrometer can typically be on the order of microns or less, with this spot size being smaller than the sample size of an ultrafast differential scanning calorimeter, while the other large multispectral spot size or measurement range is larger than the sample size of an ultrafast differential scanning calorimeter.
Currently, commercial equipment of an ultrafast differential scanning calorimeter and a laser Raman spectrometer are used independently. The combination of two commercial devices for in situ analysis of samples is temporarily impractical. If the combination is desired, the combination must be self-modified and built.
Disclosure of Invention
In view of the above, in order to solve the technical problems mentioned in the background art, the utility model provides a combined testing device for ultra-fast differential scanning calorimeter and laser Raman spectroscopy, which is an experimental technology for in-situ microscopic characterization of a molecular structure in a high molecular thermodynamic research process, and aims to expand a characterization means of a high molecular material through the combination of an ultra-fast differential scanning calorimeter and a Raman spectroscopy, and hopefully can analyze macroscopic and microscopic characteristics of the high molecular material more truly and accurately.
In order to achieve the above purpose, the present utility model adopts the following technical scheme: the combined testing device for the ultra-fast differential scanning calorimeter and the laser Raman spectrum comprises a spectrometer sample table, a Raman spectrometer, an ultra-fast differential scanning calorimeter and a control system, wherein the ultra-fast differential scanning calorimeter is arranged on the spectrometer sample table, the control system is connected with the Raman spectrometer and the ultra-fast differential scanning calorimeter,
the Raman spectrometer comprises a laser Raman microscope, a laser optical system, a detector and a Raman spectrum structure, wherein the laser Raman microscope, the laser optical system, the detector and the Raman spectrum structure are sequentially connected, a sample is placed in the ultra-fast differential scanning calorimeter, and the laser Raman microscope is positioned above the ultra-fast differential scanning calorimeter to emit laser to irradiate the sample.
Still further, the ultrafast differential scanning calorimeter includes a window through which the laser irradiates the sample.
Still further, the window is a circular notch with a diameter of 0.5 cm.
Furthermore, the ultrafast differential scanning calorimeter also comprises a sensor and a cold and hot table, wherein the sensor is arranged on the cold and hot table, and a sample is placed on the sensor.
Furthermore, a damping connecting plate is arranged between the ultrafast differential scanning calorimeter and the spectrometer sample table.
Further, an atmosphere hose is connected to the ultrafast differential scanning calorimeter.
Further, an atmosphere hose fixing rod is fixed on the Raman spectrometer, and the atmosphere hose fixing rod is used for fixing an atmosphere hose.
Further, the maximum dimension of the ultrafast differential scanning calorimeter is 9.2cm by 7.9cm by 1.6cm.
Furthermore, the spectrometer sample stage is an electric platform, which is provided with a height-adjustable connecting component, and the height is adjusted by a control system.
Compared with the prior art, the ultra-fast differential scanning calorimeter and laser Raman spectrum combined testing device has the beneficial effects that:
1. compared with a commercial ultrafast differential scanning calorimeter with the size of 57.5cm and 45.0cm and 15cm, the ultrafast differential scanning calorimeter with the size greatly reduced can be placed on a spectrometer sample table for combined use with a Raman spectrometer.
2. The utility model adjusts the proper lens length to change the focusing multiple based on the sample size of tens of micrometers of FSC, thereby obtaining the focusing light spot with proper size, ensuring that laser can strike the sample in the ultrafast differential scanning calorimeter and returning Raman signals with sufficient precision.
3. The utility model is a testing light path matched with Raman spectrum, and the window of the ultra-fast differential scanning calorimeter is provided with a right circular notch with the diameter of 0.5cm, so that the absorption and loss of the window glass to Raman light are reduced.
4. According to the utility model, the laser Raman microscope, the damping connecting plate and the spectrometer sample table are modified, the damping connecting plate and the spectrometer sample table are locked by using a screw or mechanical buckle structure, and a rubber damping film is arranged below the damping connecting plate, so that the influence of vibration can be effectively avoided; at the same time, a confocal raman spot of a suitable size and more efficient focusing and alignment can be obtained.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model. In the drawings:
FIG. 1 is a schematic diagram of a combined test device for ultra-fast differential scanning calorimetric and laser Raman spectroscopy according to the present utility model;
FIG. 2 is a perspective view of a combined ultra-fast differential scanning calorimeter and laser Raman spectrum testing device according to the utility model;
FIG. 3 is a schematic diagram of flash differential scanning calorimeter data;
FIG. 4 is a schematic diagram of Raman spectral data;
in the figure: 1-laser Raman microscope, 2-window, 3-sample, 4-sensor, 5-cold and hot stage, 6-shock attenuation connecting plate, 7-spectrometer sample stage, 8-atmosphere hose dead lever, 9-laser optical system, 10-detector, 11-Raman spectrum structure, 12-Raman spectrometer, 13-ultrafast differential scanning calorimeter, 14-control system, 15-atmosphere hose.
Detailed Description
The technical solutions in the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model. It should be noted that, in the case of no conflict, embodiments of the present utility model and features of the embodiments may be combined with each other, and the described embodiments are only some embodiments of the present utility model, not all embodiments.
Referring to fig. 1-4 for explaining the present embodiment, an ultra-fast differential scanning calorimeter and laser raman spectrum combined test device comprises a spectrometer sample stage 7, a raman spectrometer 12, an ultra-fast differential scanning calorimeter 13 and a control system 14, wherein the ultra-fast differential scanning calorimeter 13 is placed on the spectrometer sample stage 7, the control system 14 is connected with the raman spectrometer 12 and the ultra-fast differential scanning calorimeter 13,
the Raman spectrometer 12 comprises a laser emission device 1, a laser optical system 9, a detector 10 and a Raman spectrum structure 11, wherein the laser emission device 1, the laser optical system 9, the detector 10 and the Raman spectrum structure 11 are sequentially connected, the sample 3 is placed in the ultra-fast differential scanning calorimeter 13, and the laser emission device 1 is positioned above the ultra-fast differential scanning calorimeter 13 to emit laser 1 to irradiate the sample 3.
The ultrafast differential scanning calorimeter 13 includes a window 2, and the laser light 1 irradiates the sample 3 through the window 2. The ultrafast differential scanning calorimeter 13 further comprises a sensor 4 and a cold and hot table 5, the sensor 4 is installed on the cold and hot table 5, and the sample 3 is placed on the sensor 4.
A damping connecting plate 6 is arranged between the ultrafast differential scanning calorimeter 13 and the spectrometer sample table 7.
An atmosphere hose 15 is connected to the ultrafast differential scanning calorimeter 13. An atmosphere hose fixing rod 8 is fixed on the raman spectrometer 12, and the atmosphere hose fixing rod 8 is used for fixing an atmosphere hose 15.
In terms of device hardware, the ultra-fast differential scanning calorimeter (flashDSC) is different from the traditional calorimeter, has extremely high temperature rising and falling capacity, and can be used for researching the metastable structure of a high polymer material, performing thermal analysis of a trace material and the like.
Both normal commercial ultrafast differential scanning calorimeters and raman spectrometers are large devices, each with an independent limited sample testing space. The utility model makes the ultra-fast differential scanning calorimeter miniaturized and places the ultra-fast differential scanning calorimeter into a spectrometer sample stage. The utility model customizes a miniaturized ultrafast differential scanning calorimeter with the maximum size of 9.2cm by 7.9cm by 1.6cm, compared with a commercial ultrafast differential scanning calorimeter with the maximum size of 57.5cm by 45.0cm by 15cm, the size is greatly reduced, and the combined use of the ultrasonic scanning calorimeter placed on a spectrometer sample stage and a Raman spectrometer 12 can be realized.
The size of the sample 3 in the ultrafast differential scanning calorimeter 13 is in the order of micrometers, and the size of the sample 3 is completely matched with the size of the test light spot of the laser Raman microscope 1.
The utility model is based on the sample size of tens of micrometers of FSC, the long working distance testing capability of a laser Raman microscope is improved and upgraded, the focusing times (10 times, 50 times and 100 times) are changed mainly by adjusting a proper commercial lens, and the effective working distances are 21.0mm, 10.6mm and 3.3mm respectively, so that focusing light spots with proper sizes are obtained, the laser can be ensured to strike the sample 3 in the ultra-fast differential scanning calorimeter 13, and Raman signals with sufficient precision are returned. Also, in order to cooperate with the test light path of the raman spectrum, a right circular notch with the diameter of 0.5cm is opened in the window 2 of the ultrafast differential scanning calorimeter 13, so that the absorption and loss of raman light by the window glass are avoided.
In order to realize the combination of two devices, the spectrometer sample stage 7 is an electric platform, and the effective working distance and the plane adjustable range (xyz three-axis direction adjustable ranges are 5.1cm, 7.8cm and 1.7 cm) of the two are met by arranging a height-adjustable connecting component (an electrode, a motor and the like), so that the miniaturized ultra-fast differential scanning calorimeter 13 can be focused and aligned with the damping connecting plate 6. Since the polymer sample 3 is transparent and has a small thickness, the laser confocal function of the laser raman microscope 1 will be used to adjust the measurement accuracy of the ultra-fast differential scanning calorimeter 13 in the thickness direction of the sample 3.
In terms of data acquisition and control, the unification of test data on a time line must be ensured because it is the same specific state measurement of the same process or sample by both devices.
The utility model triggers experiments from the aspect of test programs and records absolute time of experimental data acquisition through reasonable experimental design and the use of a control module, and then unifies the two experimental data together for further analysis through professional software programming, wherein the analysis data are shown in fig. 3 and 4.
The embodiments of the utility model disclosed above are intended only to help illustrate the utility model. The examples are not intended to be exhaustive or to limit the utility model to the precise forms disclosed. Many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the utility model and the practical application, to thereby enable others skilled in the art to best understand and utilize the utility model.
Claims (10)
1. The utility model provides a combination testing arrangement of ultrafast differential scanning calorimeter and laser Raman spectrum which characterized in that: comprises a spectrometer sample table (7), a Raman spectrometer (12), an ultrafast differential scanning calorimeter (13) and a control system (14), wherein the ultrafast differential scanning calorimeter (13) is arranged on the spectrometer sample table (7), the control system (14) is connected with the Raman spectrometer (12) and the ultrafast differential scanning calorimeter (13),
the Raman spectrometer (12) comprises a laser Raman microscope (1), a laser optical system (9), a detector (10) and a Raman spectrum structure (11), wherein the laser Raman microscope (1), the laser optical system (9), the detector (10) and the Raman spectrum structure (11) are sequentially connected, a sample (3) is placed in the ultrafast differential scanning calorimeter (13), and the laser Raman microscope (1) is located above the ultrafast differential scanning calorimeter (13) to emit laser to irradiate the sample (3).
2. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 1, wherein: the ultrafast differential scanning calorimeter (13) comprises a window (2), and the laser irradiates the sample (3) through the window (2).
3. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 2, wherein: the window (2) is a circular notch with the diameter of 0.5 cm.
4. A combined ultra-fast differential scanning calorimetric and laser raman spectroscopy test apparatus according to any one of claims 1-3, wherein: the ultra-fast differential scanning calorimeter (13) further comprises a sensor (4) and a cold and hot table (5), the sensor (4) is installed on the cold and hot table (5), and the sample (3) is placed on the sensor (4).
5. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 1, wherein: a damping connecting plate (6) is arranged between the ultrafast differential scanning calorimeter (13) and the spectrometer sample table (7).
6. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 1, wherein: an atmosphere hose (15) is connected to the ultrafast differential scanning calorimeter (13).
7. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 6, wherein: an atmosphere hose fixing rod (8) is fixed on the Raman spectrometer (12), and the atmosphere hose fixing rod (8) is used for fixing an atmosphere hose (15).
8. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 1, wherein: the dimensions of the sample (3) placed in the ultrafast differential scanning calorimeter (13) are in the order of micrometers.
9. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 1 or 8, wherein: the maximum size of the ultrafast differential scanning calorimeter (13) is 9.2cm by 7.9cm by 1.6cm.
10. The ultra-fast differential scanning calorimeter and laser raman spectrum combined test device according to claim 1, wherein: the spectrometer sample table (7) is an electric platform and is provided with a height-adjustable connecting part, and the height is adjusted through a control system.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321862544.XU CN220399318U (en) | 2023-07-14 | 2023-07-14 | Ultra-fast differential scanning calorimetric and laser Raman spectrum combined testing device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202321862544.XU CN220399318U (en) | 2023-07-14 | 2023-07-14 | Ultra-fast differential scanning calorimetric and laser Raman spectrum combined testing device |
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| CN220399318U true CN220399318U (en) | 2024-01-26 |
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| CN202321862544.XU Active CN220399318U (en) | 2023-07-14 | 2023-07-14 | Ultra-fast differential scanning calorimetric and laser Raman spectrum combined testing device |
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