CN105136771A - Multifunctional gas high-pressure in situ Raman test cell and application thereof - Google Patents
Multifunctional gas high-pressure in situ Raman test cell and application thereof Download PDFInfo
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- CN105136771A CN105136771A CN201510520921.5A CN201510520921A CN105136771A CN 105136771 A CN105136771 A CN 105136771A CN 201510520921 A CN201510520921 A CN 201510520921A CN 105136771 A CN105136771 A CN 105136771A
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Abstract
A multifunctional gas high-pressure in situ Raman test cell comprises an external high pressure cylinder, an internal high pressure cylinder is arranged in the external high pressure cylinder, and the front end of the internal high pressure cylinder is provided with a diaphragm; the tail end of the internal high pressure cylinder is arranged outside the external high pressure cylinder in an extension manner, and is fixedly connected with the tail end of the external high pressure cylinder through a fastener; and a high pressure gas source goes through the internal high pressure cylinder to the front end of the internal high pressure cylinder in order to press a sample to the diaphragm. The test cell can realize in situ test of the Raman spectrum of a material under high temperature, high pressure, special atmosphere, laser irradiation and other extreme conditions. The test cell can be used to test a powder, a block, a high temperature melt, a film and various forms of samples. The test cell can continuously monitor the Raman spectrum of the material in an in-situ manner in the heating, pressurizing and atmosphere changing process in order to realize continuous in-situ tracking of the structure change, the stability and the chemical reaction process of the material.
Description
Technical field:
The present invention relates to a kind of multifunctional gas situ high pressure Raman test pool and application thereof, belong to the technical field of the multi-functional Raman test pool of spectrum associating in-situ test.
Background technology:
In recent years along with the development of science and technology, in situ detection research means achieves significant progress.Wherein infrared and Raman in situ detection technology is with the fastest developing speed, and range of application is constantly expanded, and widens multiple cross discipline and the fields such as chemistry, biology, materialogy and clinical medicine gradually from the research of initial catalytic reaction process.Such as, based on the difference of Single Walled Carbon Nanotube and multi-walled carbon nano-tubes Raman spectrum, Raman spectrum is often used to distinguish this two kinds of carbon nano-tube; In addition, Raman spectrum has become the effective means of drug ingedient qualification, medicine True-false distinguish; In addition, according to the otherness of stomach cancer cell and normal gastric cell Raman line, Raman spectroscopy can provide a kind of effective method for the early detection of cancer and diagnosis.
In addition, in order to explore the situation of change of material structure and performance under the extreme conditions such as high temperature, high pressure and special atmosphere, people by the Raman spectrum of in-situ acquisition material, the special Changing Patterns such as the change of the various material of systematic study structure under extreme conditions and functional group, electrochemical properties, corrosion process and catalytic adsorption performance.Such as, measure crystal and the melt thereof of stolzite type lead tungstate under heating condition, the ownership of each vibration mode can be determined; By analyzing the Raman spectrum of different temperatures, KNT crystal and LiB can be studied
3o
5the temperature variant rule of structure of crystal; In addition, in-situ Raman spectrum and ultraviolet spectrum are combined, the crystallization process of aluminium phosphate molecular sieve can be studied, the structural information of detection template agent and molecular sieve, directly verify the synthesis mechanism of aluminium phosphate molecular sieve by experiment; In addition, Raman spectrum have also been obtained extensive application in the research of graphenic surface absorption behavior.
Although special construction and the performance of the in-situ Raman spectral investigation material under utilizing extreme condition have made great progress, be limited to the rigors of extreme condition to equipment and annex thereof, the kind of current situ Raman Spectroscopy monitoring annex is still little.Particularly, so far we also do not find can under high temperature, high pressure, special atmosphere and the synergy of laser irradiation factors the annex of in-situ acquisition material Raman spectrum.But the performance of development to material of modern science and technology proposes more and more higher requirement, this will ask for help develop the performance of more specific process to material and regulate and control and modification.In this case, be well understood to material Changing Pattern under extreme conditions, just constitute the basis of controlled material stuctures and properties effectively.Therefore, design new multifunctional combined in-situ test pond, realize the in-situ test of material Raman spectrum under high temperature, high pressure, extraordinary atmosphere and the multifactor synergy of laser irradiation, there is important fundamental research meaning and actual application value.
Summary of the invention:
For the deficiencies in the prior art, the invention provides a kind of multifunctional gas situ high pressure Raman test pool.The present invention carries out in-situ test to the Raman spectrum of material under can be implemented in the extreme conditions such as high temperature, high pressure, special atmosphere and laser irradiation, for research specific condition under material stuctures and properties, exploitation material property regulation and control new method lay the foundation.The present invention can also be used for the sample testing the variforms such as powder, block, high-temperature fusant and film.In heating, pressurization and change in atmosphere process, can the Raman spectrum of in-situ monitoring material continuously, thus the structure of material is changed, stability and chemical reaction process etc. carry out continuous in-situ tracking.When working in in-situ test pattern, gaseous tension can from vacuum to hundreds of atmospheric pressure, and atmosphere during test can switch flexibly from inert gas to high reaction activity gas, various solvent vapo(u)rs etc.
The present invention also provides the using method of above-mentioned multifunctional gas situ high pressure Raman test pool.
Technical scheme of the present invention is as follows:
A kind of multifunctional gas situ high pressure Raman test pool, comprises outer high pressure cylinder, is provided with inner high voltage cylinder, the front end of described inner high voltage cylinder is provided with diaphragm in described outer high pressure cylinder; The end of described inner high voltage cylinder is extended on the outside of described outer high pressure cylinder and is fixedly connected with by securing member with the end of described outer high pressure cylinder; High-pressure air source through described inner high voltage cylinder to the front end press against sample of described inner high voltage cylinder to described diaphragm.Quote outer high pressure cylinder in the present invention, effect is for the parts of its inside provide support, and makes it to be unlikely to distortion when bearing high pressure.Preferably, described outer high pressure cylinder is processed by high strength steel, and according to working pressure requirement, outer high pressure cylinder can be made into single layer structure, double-decker or sandwich construction.
Quote diaphragm in the present invention, its effect comprises and participates in forming enclosed high pressure cavity and providing transmission channel for exciting light and scattered light, and they are different according to working pressure, and diaphragm can select the material processing such as glass, quartz, sapphire, adamas.
Preferred according to the present invention, in described outer high pressure cylinder, be provided with thermocouple hole insert for thermopair.
Preferred according to the present invention, there is heating part in the arranged outside of described outer high pressure cylinder.Preferably, described heating part is heating tube.The advantage herein designed is, is to heat whole test pool, for the in-situ test carrying out material provides hot conditions.
Preferred according to the present invention, be also provided with heat-insulation layer in the outside of described outer high pressure cylinder.The advantage herein designed is, reduces the temperature of thermal loss and the described test pool of maintenance, prevents high temperature failure Raman spectrometer simultaneously.
Preferred according to the present invention, the base of adjustment height is provided with in the bottom of described outer high pressure cylinder.Preferably, the base of described adjustment height is that isolation material is made.
Preferred according to the present invention, the base of described adjustment height comprises base, attachment screw and fine-tuning nut.The advantage herein designed is, supports outer high pressure cylinder and is connected with Raman spectrometer, and wherein attachment screw is used for bottom base being fixed on outer high pressure cylinder, and can regulate the angle in outer high pressure cylinder and surface level easily; Described fine-tuning nut is used for the height of external high pressure cylinder and adjusts.
Preferred according to the present invention, be fixedly installed supported flange dish at the end of described inner high voltage cylinder, described supported flange dish is fixedly connected with by the end of securing member with described outer high pressure cylinder.
Preferred according to the present invention, the end external diameter of described inner high voltage cylinder is less than the front end external diameter of described inner high voltage cylinder, is arranged with inner core O-ring seal and auxiliary seal cylinder successively at the end of described inner high voltage cylinder; Described supported flange dish compresses and is arranged on described auxiliary seal cylinder ends.
Preferred according to the present invention, be communicated with at the end of described inner high voltage cylinder and be provided with high-voltage tube, described high-pressure air source is through high-voltage tube, inner high voltage cylinder press against sample extremely described diaphragm.
Preferred according to the present invention, described high-voltage tube is connected with the end of described inner high voltage cylinder by compressing locknut; Described compression locknut is connected with the end thread of described inner high voltage cylinder; Described high-voltage tube is fixedly connected with by cutting ferrule with compression locknut.
Preferred according to the present invention, in the front end of described diaphragm and end, sealing buffering spacer is set respectively.The advantage herein designed is, is beneficial to high-pressure chamber sealing and realizes buffering between diaphragm and outer high pressure cylinder, in order to avoid damage diaphragm.
As the method for work of above-mentioned multifunctional gas situ high pressure Raman test pool, comprising:
Assemble described test pool:
1) outside high pressure cylinder is interior successively places sealing buffering spacer, diaphragm, sealing buffering spacer and inner high voltage cylinder;
2) at the end of described inner high voltage cylinder, supported flange dish is installed, is fixedly connected with by the end of securing member with described outer high pressure cylinder;
Load testing sample:
3) in described inner high voltage cylinder, sample is loaded;
4) high-pressure air source through described inner high voltage cylinder to the front end press against sample of described inner high voltage cylinder to described diaphragm;
5) in-situ Raman test is carried out to sample.Experimentally condition, adjusts running parameter, namely regulates temperature, pressure, atmosphere and laser irradiation correspondence; Working pressure can change from vacuum flexibly to hundreds of atmospheric pressure.Further, above-mentioned several parameter can change simultaneously, also can change independently of one another, and can the Raman spectrum of in-situ acquisition material continuously in change procedure.
Preferred according to the present invention, in described step 2) in, be arranged with inner core O-ring seal and auxiliary seal cylinder successively at the end of described inner high voltage cylinder; Described supported flange dish compresses and is arranged on described auxiliary seal cylinder ends.
Preferred according to the present invention, the method for work of described multifunctional gas situ high pressure Raman test pool also comprises, and thermopair is inserted thermocouple hole, realizes by adjustment heating tube the temperature regulating Raman test.
Advantage of the present invention is:
The present invention is when carrying out in-situ test, and variable element comprises temperature, pressure, atmosphere and laser irradiation; Working pressure can change from vacuum flexibly to hundreds of atmospheric pressure.Further, above-mentioned several parameter can change simultaneously, also can change independently of one another, and can the Raman spectrum of in-situ acquisition material continuously in change procedure.
Test pool of the present invention can produce high-pressure air source by external pressure gas cylinder or supercharge pump when carrying out in-situ test, also gas expansion can be made to produce high pressure by heating; When needs change in-situ test atmosphere, mixed gas can be used to pass into in-situ Raman test pool, also can bring in-situ Raman test pool into inert gas bubbling in liquid solvent.
Utilize in-situ Raman test pool of the present invention, not only can carry out conventional Raman spectrum test to material, more under the extreme conditions such as high temperature, high pressure, special atmosphere and laser irradiation, in-situ tracking test can be carried out to the state of material and performance.Utilize these specific functions, deeply can investigate the structure of material and the special change procedure of performance under extreme condition, expand investigation of materials field, the more important thing is and can explore and find more effective material modification and New Method for Processing on this basis, for development has the new material service of better performance.
Accompanying drawing explanation
The one-piece construction schematic diagram of Fig. 1 test pool of the present invention;
The vertical view of Fig. 2 base of the present invention;
The side cutaway view of Fig. 3 base of the present invention;
The side cutaway view of Fig. 4 outer high pressure cylinder of the present invention;
The side view of Fig. 5 sealing buffering spacer of the present invention;
The axial cut-open view of Fig. 6 inner high voltage of the present invention cylinder;
The side view of Fig. 7 inner core O-ring seal of the present invention;
The side cutaway view of Fig. 8 auxiliary seal cylinder of the present invention;
Fig. 9 utilizes in-situ Raman test pool of the present invention to record organism CH
3nH
3the normal pressure Raman spectrogram of I;
Figure 10 utilizes in-situ Raman test pool of the present invention to record the normal pressure Raman spectrogram of organism oxine aluminium;
Figure 11 utilizes in-situ Raman test pool of the present invention to record inorganics TiO
2normal pressure Raman spectrogram;
Figure 12 is composite semiconductor CH in 4.5MPa nitrogen
3nH
3pbI
3alternating temperature in-situ Raman spectrogram;
Composite semiconductor CH under Figure 13 normal pressure
3nH
3pbI
3alternating temperature in-situ Raman spectrogram;
The alternating temperature in-situ Raman spectrogram of composite semiconductor 1,1-dibutyl-4,4-dipyridine under Figure 14 normal pressure;
The CH that Figure 15 structure is close
3nH
3pbI
3and CH
3nH
3pbBr
3the room temperature normal pressure Raman spectrogram of two kinds of crystal;
In Fig. 1-8: 1, attachment screw, 2, fine-tuning nut, 3, base, 4, outer high pressure cylinder, 5, diaphragm, 6, sample, 7, sealing buffering spacer, 8, inner high voltage cylinder, 9, heating tube, 10, heat-insulation layer, 11, thermocouple hole, 12, inner core O-ring seal, 13, supported flange dish, 14, trip bolt, 15, auxiliary seal cylinder, 16, cutting ferrule, 17, locknut is compressed, 18, high-voltage tube, 19, the front extreme direction of described test pool; 20, the end direction of described test pool.
Embodiment:
Below in conjunction with specific embodiment and Figure of description, the present invention is described in detail, but be not limited thereto.
As shown in figures 1-8.
Embodiment 1,
A kind of multifunctional gas situ high pressure Raman test pool, comprises outer high pressure cylinder 4, is provided with inner high voltage cylinder 8, the front end of described inner high voltage cylinder 8 is provided with diaphragm 5 in described outer high pressure cylinder 4; The end of described inner high voltage cylinder 8 is extended on the outside of described outer high pressure cylinder 4 and is fixedly connected with by securing member 14 with the end of described outer high pressure cylinder 4; High-pressure air source through described inner high voltage cylinder 8 to the front end press against sample 6 of described inner high voltage cylinder 8 to described diaphragm 5.
Embodiment 2,
A kind of multifunctional gas situ high pressure Raman test pool as described in Example 1, its difference is, in described outer high pressure cylinder, 4 are provided with thermocouple hole 11 for thermopair insertion.
Heating part is had in the arranged outside of described outer high pressure cylinder 4.Described heating part is heating tube 9.
Heat-insulation layer 10 is also provided with in the outside of described outer high pressure cylinder 4.
Embodiment 3,
A kind of multifunctional gas situ high pressure Raman test pool as described in Example 1, its difference is, is provided with the base of adjustment height in the bottom of described outer high pressure cylinder 4.The base of described adjustment height is that isolation material is made.
The base of described adjustment height comprises base 3, attachment screw 1 and fine-tuning nut 2.
Embodiment 4,
A kind of multifunctional gas situ high pressure Raman test pool as described in Example 1, its difference is, be fixedly installed supported flange dish 13 at the end of described inner high voltage cylinder 8, described supported flange dish 13 is fixedly connected with by the end of securing member 14 with described outer high pressure cylinder 4.
The end external diameter of described inner high voltage cylinder 8 is less than the front end external diameter of described inner high voltage cylinder 8, is arranged with inner core O-ring seal 12 and auxiliary seal cylinder 15 successively at the end of described inner high voltage cylinder 8; Described supported flange dish 13 compresses and is arranged on described auxiliary seal cylinder 15 end.
Described inner high voltage cylinder 8 end be communicated be provided with high-voltage tube 18, described high-pressure air source through high-voltage tube 18, inner high voltage cylinder 8 press against sample 6 to described diaphragm 5.
Described high-voltage tube 18 is connected with the end of described inner high voltage cylinder 8 by compressing locknut 17; Described compression locknut 17 is connected with the end thread of described inner high voltage cylinder 8; Described high-voltage tube 8 is fixedly connected with by cutting ferrule 16 with compression locknut 17.
Sealing buffering spacer 7 is set respectively in the front end of described diaphragm 5 and end.
Embodiment 5,
The method of work of multifunctional gas situ high pressure Raman test pool as described in Example 4, comprising:
Assemble described test pool:
1) outside high pressure cylinder 4 is interior successively places sealing buffering spacer 7, diaphragm 5, sealing buffering spacer 7 and inner high voltage cylinder 8;
2) at the end of described inner high voltage cylinder 8, supported flange dish 13 is installed, is fixedly connected with by the end of securing member 14 with described outer high pressure cylinder 4;
Load testing sample:
3) in described inner high voltage cylinder 8, sample 6 is loaded;
4) high-pressure air source through described inner high voltage cylinder 8 to the front end press against sample 6 of described inner high voltage cylinder 8 to described diaphragm 5;
5) in-situ Raman test is carried out to sample 6.Experimentally condition, adjusts running parameter, namely regulates temperature, pressure, atmosphere and laser irradiation correspondence; Working pressure can change from vacuum flexibly to hundreds of atmospheric pressure.Further, above-mentioned several parameter can change simultaneously, also can change independently of one another, and can the Raman spectrum of in-situ acquisition material continuously in change procedure.
Embodiment 6,
The method of work of multifunctional gas situ high pressure Raman test pool as described in Example 5, its difference is, in described step 2) in, be arranged with inner core O-ring seal 12 and auxiliary seal cylinder 15 successively at the end of described inner high voltage cylinder 8; Described supported flange dish 13 compresses and is arranged on described auxiliary seal cylinder 15 end.
Embodiment 7,
The method of work of multifunctional gas situ high pressure Raman test pool as described in Example 5, its difference is, the method of work of described multifunctional gas situ high pressure Raman test pool also comprises, and thermopair is inserted thermocouple hole 11, realizes by adjustment heating tube 9 temperature regulating Raman test.
Application examples 1 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, according to different test conditions, described high-pressure air source can multiple choices, such as:
Described high-pressure air source is inertia gases at high pressure (normal pressure ~ 15MPa) by external Ar (or N
2) high-pressure cylinder introduced by high-voltage tube;
Described high-pressure air source is that the gases at high pressure (normal pressure ~ 15MPa) of high reaction activity are by external O
2(or NO
2deng) high-pressure cylinder inputted by high pressure steel;
Described high-pressure air source is: by nitrogen bubbling carry its steam and enter in-situ test pond in the high pressure bubbler that organic solvent is housed, provide the special atmosphere that in-situ test needs.
Application examples 2 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in normal pressure nitrogen atmosphere, measure organism CH
3nH
3the Raman spectrum of I, as shown in Figure 9.
Application examples 3 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in normal pressure nitrogen atmosphere, measure the Raman spectrum of organism oxine aluminium, as shown in Figure 10.
Application examples 4 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in normal pressure nitrogen atmosphere, gather inorganics TiO
2the Raman spectrum of powder, as shown in figure 11.
Application examples 5 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in high pressure oxygen atmosphere, measure TiO
2the Raman spectrum of porous membrane.
Application examples 6 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in 4.5MPa nitrogen, recorded CH
3nH
3pbI
3alternating temperature Raman spectrum, as shown in figure 12.
Application examples 7 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in 0.1MPa nitrogen atmosphere, recorded CH
3nH
3pbI
3alternating temperature Raman spectrum, as shown in figure 13.
Application examples 8 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, in 0.1MPa nitrogen atmosphere, record the alternating temperature Raman spectrum of 1,1-dibutyl-4,4-dipyridine, as shown in figure 14.
Application examples 9 of the present invention:
Utilize the test pool described in embodiment 1-4 to carry out Hi-pot test to testing sample, utilize the method for work described in embodiment 6,7, utilize the CH that Raman spectrum specification configuration is similar
3nH
3pbI
3and CH
3nH
3pbBr
3two kinds of crystal, as shown in figure 15.
Claims (10)
1. a multifunctional gas situ high pressure Raman test pool, is characterized in that, this test pool comprises outer high pressure cylinder, is provided with inner high voltage cylinder, the front end of described inner high voltage cylinder is provided with diaphragm in described outer high pressure cylinder; The end of described inner high voltage cylinder is extended on the outside of described outer high pressure cylinder and is fixedly connected with by securing member with the end of described outer high pressure cylinder; High-pressure air source through described inner high voltage cylinder to the front end press against sample of described inner high voltage cylinder to described diaphragm.
2. a kind of multifunctional gas situ high pressure Raman test pool according to claim 1, is characterized in that, is provided with thermocouple hole and inserts for thermopair in described outer high pressure cylinder.
3. a kind of multifunctional gas situ high pressure Raman test pool according to claim 1, is characterized in that, it is characterized in that have heating part in the arranged outside of described outer high pressure cylinder; Also heat-insulation layer is provided with in the outside of described outer high pressure cylinder.
4. a kind of multifunctional gas situ high pressure Raman test pool according to claim 1, is characterized in that, be provided with the base of adjustment height in the bottom of described outer high pressure cylinder; The base of described adjustment height comprises base, attachment screw and fine-tuning nut.
5. a kind of multifunctional gas situ high pressure Raman test pool according to claim 1, it is characterized in that, be fixedly installed supported flange dish at the end of described inner high voltage cylinder, described supported flange dish is fixedly connected with by the end of securing member with described outer high pressure cylinder.
6. a kind of multifunctional gas situ high pressure Raman test pool according to claim 5, it is characterized in that, the end external diameter of described inner high voltage cylinder is less than the front end external diameter of described inner high voltage cylinder, is arranged with inner core O-ring seal and auxiliary seal cylinder successively at the end of described inner high voltage cylinder; Described supported flange dish compresses and is arranged on described auxiliary seal cylinder ends.
7. a kind of multifunctional gas situ high pressure Raman test pool according to claim 1, is characterized in that, is communicated with is provided with high-voltage tube at the end of described inner high voltage cylinder, and described high-pressure air source is through high-voltage tube, inner high voltage cylinder press against sample extremely described diaphragm.
8. a kind of multifunctional gas situ high pressure Raman test pool according to claim 7, is characterized in that, described high-voltage tube is connected with the end of described inner high voltage cylinder by compressing locknut; Described compression locknut is connected with the end thread of described inner high voltage cylinder; Described high-voltage tube is fixedly connected with by cutting ferrule with compression locknut; Preferably, sealing buffering spacer is set respectively in the front end of described diaphragm and end.
9. the method for work of multifunctional gas situ high pressure Raman test pool as described in claim 1-8 any one, it is characterized in that, the method comprises:
Assemble described test pool:
1) outside high pressure cylinder is interior successively places sealing buffering spacer, diaphragm, sealing buffering spacer and inner high voltage cylinder;
2) at the end of described inner high voltage cylinder, supported flange dish is installed, is fixedly connected with by the end of securing member with described outer high pressure cylinder;
Load testing sample:
3) in described inner high voltage cylinder, sample is loaded;
4) high-pressure air source through described inner high voltage cylinder to the front end press against sample of described inner high voltage cylinder to described diaphragm;
5) in-situ Raman test is carried out to sample.
10. the method for work of multifunctional gas situ high pressure Raman test pool as claimed in claim 9, is characterized in that, in described step 2) in, be arranged with inner core O-ring seal and auxiliary seal cylinder successively at the end of described inner high voltage cylinder; Described supported flange dish compresses and is arranged on described auxiliary seal cylinder ends; Preferably, the method for work of described multifunctional gas situ high pressure Raman test pool also comprises, and thermopair is inserted thermocouple hole, realizes by adjustment heating tube the temperature regulating Raman test.
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| IT202000023584A1 (en) * | 2020-10-07 | 2022-04-07 | Velp Scient Srl | BASIC METHOD AND ANALYZER FOR ORGANIC AND INORGANIC SAMPLES |
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| CN112730551A (en) * | 2020-12-16 | 2021-04-30 | 南方科技大学 | In-situ electrolytic cell for high-voltage electrochemistry |
| CN113916765A (en) * | 2021-11-03 | 2022-01-11 | 中国石油大学(华东) | In-situ heating type Raman-electrochemical reaction device |
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