CN204405549U - Melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell - Google Patents
Melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell Download PDFInfo
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- CN204405549U CN204405549U CN201420852018.XU CN201420852018U CN204405549U CN 204405549 U CN204405549 U CN 204405549U CN 201420852018 U CN201420852018 U CN 201420852018U CN 204405549 U CN204405549 U CN 204405549U
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Abstract
Melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell, belong to electrochemical analysis techniques field.Microscopic heating stand: comprise thermal station shell, burner hearth, thermal station lid and pillar and base; Thermal station shell circulating cooling water route is provided with in thermal station enclosure, burner hearth body top is provided with sample cell and places groove, the left and right sides of placing groove at sample cell is symmetrically arranged with strip groove, the burner hearth main body of placing groove both sides at strip groove and sample cell is evenly equipped with resistance wire mounting hole, in resistance wire mounting hole, be provided with spiral resistance wire, resistance wire and burner hearth main body insulate and arrange; In thermal station lid main body, be provided with thermal station lid circulating cooling water route, the middle part of thermal station lid main body is provided with microlens through hole.Sample cell: be provided with quartz cover at the top of crucible; Be provided with through hole on the top of crucible, through hole is corresponding with strip groove; If crucible adopts conductive material, it simultaneously as to electrode, also can be arranged separately electrode in crucible.
Description
Technical field
The utility model belongs to electrochemical analysis techniques field, particularly relates to a kind of melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell.
Background technology
In contemporary galvanochemistry, the development of spectroelectrochemistry technology is very rapid, and electrochemical in-situ spectrum relate to numerous spectral investigation field such as ultraviolet and visible spectrum, infrared spectrum, Raman spectrum, electronics and ion power spectrum, magnetic resonance spectrum, X-ray spectrum.In the last few years along with the progress of the technology such as confocal Raman, micro-Raman, resonant Raman, and the lifting of Raman spectral instrument (detector, laser instrument etc.) performance, the temporal resolution of Raman spectral technique, spatial resolution, detection sensitivity increase substantially.Above-mentioned progress brings breakthrough to the application of Raman spectral technique in electrochemical interface, allows electrochemical in-situ Raman study and has jumped onto new step.
At first, the electrochemical in-situ Raman research that researchers carry out mainly concentrates on water solution system, also comprises the research of some non-aqueous systems.Afterwards, along with developing rapidly of ionic liquid research, the electrochemical in-situ Raman spectral investigation carrying out this system also caused the concern of researchers day by day.Also have on a small quantity about the research of the electrochemical in-situ Raman spectrum of molten salt system.
The electrochemical in-situ Raman experiment of high-temperature molten salt system needs to use special sample cell.Melten salt electriochemistry original position Raman sample cell is except will meeting the General Requirements such as corrosion-resistant, the high temperature resistance thermal shock of general fused salt Raman spectroscopic assay sample cell, thermograde be little, also need appropriate design and the arrangement of carrying out electrode, to ensure that Raman incident laser accurately can be irradiated to the requirement position of ate electrode.
Existing melten salt electriochemistry original position Raman spectral investigation microscopic heating stand and sample cell, mainly for be the Raman spectrometer of 90 ° of backscatter mode.And along with the progress of micro-Raman spectral technique, the advantage that its power density is high embodies all the more in scientific research, but modern Raman System substantially all adopts backscatter mode.In addition, the sample cell that former researcher adopts uses silica crucible splendid attire fused salt mostly, and seldom has and seal sample cell, is therefore not suitable for the molten salt system carried out with quartz reaction and high volatility and studies.
Utility model content
For prior art Problems existing, the utility model provides a kind of melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell.The utility model coordinates the Raman System of backscatter mode to use, and can obtain good experiment effect.
To achieve these goals, the utility model adopts following technical scheme: a kind of melten salt electriochemistry original position Raman spectral measurement microscopic heating stand, comprises thermal station shell, burner hearth, thermal station lid and pillar and base;
The side wall upper part of described thermal station shell is provided with contact conductor through hole, thermal station enclosure is provided with thermal station shell circulating cooling water route, thermal station outer casing bottom is provided with pillar connecting hole and resistance wire through hole, is fixed with resistance wire binding post at thermal station outer casing bottom;
Described burner hearth comprises burner hearth main body, is provided with sample cell places groove at the top of burner hearth main body, and the burner hearth main body below sample cell placement groove is provided with hearth thermocouple through hole, and described sample cell is placed groove and is connected with hearth thermocouple through hole; At the top of burner hearth main body, sample cell places the left and right sides of groove and is symmetrically arranged with and puts contact conductor strip groove, the burner hearth main body of putting contact conductor strip groove and sample cell placement groove both sides is evenly equipped with resistance wire mounting hole respectively, in resistance wire mounting hole, be provided with spiral resistance wire, described resistance wire and burner hearth main body insulate and arrange;
Described thermal station lid comprises thermal station lid main body, and the inside of thermal station lid main body is provided with thermal station lid circulating cooling water route, and the middle part of thermal station lid main body is provided with microlens through hole;
Described base is provided with pillar mounting hole, and described pillar is fixed in the pillar mounting hole of base, is provided with pillar thermopair through hole, is fixed with thermopair binding post in the bottom of pillar at the middle part of pillar;
Described thermal station lid is arranged on the top of thermal station shell, and it is corresponding that microlens through hole and sample cell place groove; Burner hearth is fixed in the space that thermal station lid and thermal station shell formed, and the resistance wire in burner hearth is connected with resistance wire binding post through after the resistance wire through hole of thermal station shell, and resistance wire and thermal station casing insulation are arranged; Pillar is threaded with the pillar connecting hole of thermal station shell, and thermopair binding post is fixed with thermopair, and the hot junction of thermopair is arranged in hearth thermocouple through hole through after pillar thermopair through hole, and the cold junction of thermopair is connected with thermopair binding post.
Described burner hearth main body adopts silicon carbide material.
Described resistance wire adopts high temperature nickel evanohm Ni20Cr80.
The described resistance wire putting contact conductor strip groove both sides adopts mode in parallel to connect.
With described microscopic heating stand with the use of sample cell, comprise crucible, the top of crucible be provided with quartz cover; Be symmetrically arranged with two through holes on the top of crucible wall, described through hole is corresponding with putting contact conductor strip groove; Crucible adopts conductive material, and it is connected with to contact conductor, is respectively arranged with working electrode and contrast electrode in crucible, and working electrode and contrast electrode go between with working electrode respectively to go between with contrast electrode and be connected.
With described microscopic heating stand with the use of sample cell, comprise crucible, the top of crucible be provided with quartz cover; Be symmetrically arranged with two through holes on the top of crucible wall, described through hole is corresponding with putting contact conductor strip groove; Be respectively arranged with electrode, working electrode and contrast electrode in crucible, electrode, working electrode and contrast electrode are connected with going between to contact conductor, working electrode to go between with contrast electrode respectively.
Described crucible and quartz cover are tightly connected.
The beneficial effects of the utility model:
1, contact conductor of the present utility model enters from the sidepiece of the crucible of carrying fused salt, thus the camera lens that can measure use for the micro-Raman above crucible provides enough spaces;
2, the compact structure of sample cell of the present utility model, microlens close to sample to be analyzed, can be applicable to the mensuration of micro-Raman spectrum;
3, the resistance wire of microscopic heating stand of the present utility model in the shape of a spiral, effectively increases length, can provide more heat, realizes high temperature measuring.
Accompanying drawing explanation
Fig. 1 is the thermal station shell mechanism schematic diagram of microscopic heating stand of the present utility model;
Fig. 2 is the front view of the burner hearth of microscopic heating stand of the present utility model;
Fig. 3 is the vertical view of the burner hearth of microscopic heating stand of the present utility model;
Fig. 4 is the side view of the burner hearth of microscopic heating stand of the present utility model;
Fig. 5 is the thermal station lid structural representation of microscopic heating stand of the present utility model;
Fig. 6 is the pillar of microscopic heating stand of the present utility model and the structural representation of base;
Fig. 7 is that the crucible of carrying sample is simultaneously as the structural representation of the sample cell to electrode;
Fig. 8 is the independent structural representation used the sample cell of electrode;
Fig. 9 is that the crucible of carrying sample is simultaneously as the structural representation after assembling the sample cell of electrode and microscopic heating stand;
Figure 10 is the structural representation after independent use is assembled the sample cell of electrode and microscopic heating stand;
Figure 11 is the original position Raman spectrogram of Pt electrode surface fused salt when negative sense increases current potential in embodiment one;
Figure 12 is the original position Raman spectrogram of Pt electrode surface fused salt when forward increases current potential in embodiment one;
Figure 13 is the cyclic voltammetry curve figure of fused salt in embodiment two;
Figure 14 is the original position Raman spectrogram of the thin liquid layer of Ni electrode surface in current potential negative sense scanning process in embodiment two;
Figure 15 is the original position Raman spectrogram of the thin liquid layer of Ni electrode surface in current potential forward scan process in embodiment two;
In figure: 1-contact conductor through hole, 2-thermal station shell water delivering orifice, 3-thermal station shell circulating cooling water route, 4-pillar connecting hole, 5-resistance wire through hole, 6-resistance wire binding post, 7-puts contact conductor strip groove, 8-burner hearth main body, 9-sample cell places groove, 10-thermopair, 11-hearth thermocouple through hole, 12-screw, 13-resistance wire mounting hole, 14-resistance wire, 15-microlens through hole, 16-thermal station lid circulating cooling water route, 17-thermal station lid circulation waterway intake-outlet, 18-pillar thermopair through hole, 19-pillar, 20-base, 21-thermopair binding post, 22-is to contact conductor, 23-contrast electrode goes between, 24-diplopore alundum tube, 25-through hole, 26-crucible, 27-contrast electrode, 28-working electrode, 29-working electrode goes between, 30-single hole alundum tube, 31-quartz cover, 32-is to electrode, 33-thermal station shell water inlet, 34-thermal station lid main body, 35-thermal station lid, 36-burner hearth, 37-thermal station shell, 38-screw.
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail.
As shown in Fig. 1 ~ Fig. 6, a kind of melten salt electriochemistry original position Raman spectral measurement microscopic heating stand, comprises thermal station shell 37, burner hearth 36, thermal station lid 35 and pillar 19 and base 20.
Described thermal station shell 37 is red copper material, the side wall upper part of described thermal station shell 37 is provided with contact conductor through hole 1, thermal station shell 37 inside is provided with thermal station shell circulating cooling water route 3, thermal station shell circulating cooling water route 3 has thermal station shell water delivering orifice 2 and thermal station shell water inlet 33, to realize the discharge of recirculated water and to pass into, thermal station shell water delivering orifice 2 and thermal station shell water inlet 33 adopt stainless steel connecting pipe, bottom thermal station shell 37, be provided with pillar connecting hole 4 and resistance wire through hole 5, bottom thermal station shell 37, be fixed with resistance wire binding post 6.
Described burner hearth 36 comprises burner hearth main body 8, burner hearth main body 8 adopts silicon carbide material, the sample cell being provided with column type at the top center place of burner hearth main body 8 places groove 9, burner hearth main body 8 below sample cell placement groove 9 is provided with the hearth thermocouple through hole 11 of column type, described sample cell is placed groove 9 and is connected with hearth thermocouple through hole 11; At the top of burner hearth main body 8, sample cell places the left and right sides of groove 9 and is symmetrically arranged with two and puts contact conductor strip groove 7, as contact conductor passage; The sample cell top of placing groove 9 with put contact conductor strip groove 7 and be connected, the burner hearth main body 8 of putting contact conductor strip groove 7 and sample cell placement groove 9 both sides is evenly equipped with 14 resistance wire mounting holes 13 respectively, in resistance wire mounting hole 13, be provided with the spiral resistance wire 14 for providing heat, resistance wire 14 is to increase its length in the shape of a spiral; Described resistance wire 14 adopts high temperature nickel evanohm Ni20Cr80, and resistance wire 14 and burner hearth main body 8 insulate and arrange; The described resistance wire 14 putting contact conductor strip groove 7 both sides adopts mode in parallel to connect.
Described thermal station lid 35 comprises thermal station lid main body 34, thermal station lid main body 34 adopts stainless steel, the inside of thermal station lid main body 34 is provided with thermal station lid circulating cooling water route 16, thermal station lid circulating cooling water route 16 has two thermal station lid circulation waterway intake-outlets 17, to realize passing into and discharging of recirculated water, thermal station lid circulation waterway intake-outlet 17 adopts stainless steel connecting pipe, be provided with circular microlens through hole 15 at the middle part of thermal station lid main body 34, microlens through hole 15 stretches into for Raman spectral measurement microlens
Described base 20 is provided with pillar mounting hole, and described pillar 19 is fixed in the pillar mounting hole of base 20, and pillar 19 adopts with base 20 and is threaded; The material of pillar 19 is red copper, and the material of base 20 is stainless steel; Be provided with pillar thermopair through hole 18 at the middle part of pillar 19, be fixed with thermopair binding post 21 in the bottom of pillar 19.
Described thermal station lid 35 is arranged on the top of thermal station shell 37, and thermal station lid 35 is connected with thread forms with thermal station shell 37, and it is corresponding that microlens through hole 15 and sample cell place groove 9; Burner hearth 36 is fixed in the space that thermal station lid 35 and thermal station shell 37 formed by screw 12 that burner hearth main body 8 is arranged and screw 38, resistance wire 14 in resistance wire mounting hole 13 is connected with resistance wire binding post 6 through after the resistance wire through hole 5 of thermal station shell 37, and resistance wire 14 and thermal station shell 37 insulate and arrange; Pillar 19 is threaded with the pillar connecting hole 4 of thermal station shell 37, thermopair binding post 21 is fixed with thermopair 10, the hot junction of thermopair 10 is arranged in hearth thermocouple through hole 11 through after pillar thermopair through hole 18, and the cold junction of thermopair 10 is connected with thermopair binding post 21.
As shown in Fig. 7, Fig. 9, with described microscopic heating stand with the use of sample cell, comprise carrying fused salt crucible 26, the top of crucible 26 is provided with quartz cover 31, and described quartz cover 31 is bondd by high-temperature cement and crucible 26 and realizes sealing; Be symmetrically arranged with two through holes 25 on the top of crucible 26 sidewall, described through hole 25 is corresponding with putting contact conductor strip groove 7, and through hole 25 is in order to pass through diplopore or single hole alundum tube, and contact conductor passes in alundum tube, and is connected with electrode; When crucible 26 adopts the conductive material such as graphite, platinum, titanium, it can simultaneously as to electrode, be connected with to contact conductor 22, in crucible 26, be respectively arranged with working electrode 28 and contrast electrode 27, working electrode 28 and contrast electrode 27 go between with working electrode respectively and 29 to go between with contrast electrode and 23 to be connected.If crucible 26 conduct is simultaneously to electrode, stretch into contact conductor 22 and contrast electrode lead-in wire 23 in two holes of so diplopore alundum tube 24 respectively, the middle part of contact conductor 22 at diplopore alundum tube 24 is stretched out from alundum tube, and be connected with crucible 26, stretch into working electrode lead-in wire 29 in the hole of single hole alundum tube 30.
As shown in Fig. 8, Figure 10, with described microscopic heating stand with the use of sample cell, comprise carrying fused salt crucible 26, the top of crucible 26 is provided with quartz cover 31, and described quartz cover 31 is bondd by high-temperature cement and crucible 26 and realizes sealing; Be symmetrically arranged with two through holes 25 on the top of crucible 26 sidewall, described through hole 25 is corresponding with putting contact conductor strip groove 7, and through hole 25 is in order to pass through diplopore or single hole alundum tube, and contact conductor passes in alundum tube, and is connected with electrode; Be respectively arranged with electrode 32, working electrode 28 and contrast electrode 27 in crucible 26, electrode 32, working electrode 28 and contrast electrode 27 29 to be gone between with contrast electrode and 23 to be connected with going between to contact conductor 22, working electrode respectively.If as to electrode when crucible 26 is different, and have special in electrode 32, then stretch into working electrode lead-in wire 29 and contrast electrode lead-in wire 23 respectively in two holes of diplopore alundum tube 24, stretch into contact conductor 22 in the hole of single hole alundum tube 30.
Adopt microscopic heating stand of the present utility model and sample cell to carry out melten salt electriochemistry original position Raman spectral measurement, its specific operation process is as follows:
Step one: put in thermal station shell 37 by burner hearth 36, makes the contact conductor through hole 1 putting contact conductor strip groove 7 and thermal station shell 37 to good, and uses screw 38 to be fixed by burner hearth 36; Resistance wire 14 is connected with temperature controller with thermopair binding post 21 respectively by resistance wire binding post 6 with thermopair 10.
Step 2: sample to be analyzed loaded in sample cell crucible 26, sample cell crucible 26 being put into burner hearth 36 places groove 9, and the through hole 25 on crucible 26 top and burner hearth 36 put contact conductor strip groove 7 to good.
Step 3: diplopore alundum tube 24 and single hole alundum tube 30 are extend in crucible 26 through the contact conductor through hole 1 of thermal station shell 37, the through hole 25 putting contact conductor strip groove 7 and crucible 26 of burner hearth 36 successively.
Step 4: if crucible 26 conduct is simultaneously to electrode, stretch into contact conductor 22 and contrast electrode lead-in wire 23 respectively from two holes of diplopore alundum tube 24, the middle part of contact conductor 22 at diplopore alundum tube 24 is stretched out from alundum tube, and be connected with as to the crucible 26 of electrode, contrast electrode lead-in wire 23 extend in crucible 26, be connected with contrast electrode 27, working electrode lead-in wire 29 extend in crucible 26 from the hole of single hole alundum tube 30, and is connected with working electrode 28.If as to electrode when crucible 26 is different, and have special in electrode 32, then working electrode lead-in wire 29 and contrast electrode lead-in wire 23 are extend in crucible 26 respectively from two holes of diplopore alundum tube 24, and be connected with working electrode 28 and contrast electrode 27 respectively; Extend into contact conductor 22 in crucible 26 from the hole of single hole alundum tube 30, and be connected with to electrode 32.
Step 5: quartz cover 31 is covered on crucible 26, and use high-temperature cement to seal.
Step 6: working electrode lead-in wire 29, contrast electrode lead-in wire 23 are connected with electrochemical workstation with to contact conductor 22.
Step 7: pass to cooling circulating water respectively by thermal station shell water inlet 33, thermal station shell circulating cooling water route 3, thermal station shell water delivering orifice 2 and thermal station lid circulation waterway intake-outlet 17,16 pairs, thermal station lid circulating cooling water route thermal station shell 37 and thermal station lid 35; Open temperature controller, according to the temperature reading of thermopair 10, regulate the input current to resistance wire 14, heating sample; Open Raman spectrometer optical excited laser, move horizontally microscopic heating stand, move up and down the exact focus of the microlens of Raman spectrometer realization to measured zone, open electrochemical workstation, to conductance cell system input electrochemical parameter, carry out electrochemistry experiment, recording responses signal, meanwhile, the real time measure working electrode district fused salt Raman spectrum.
Embodiment one:
Under 623K, KNO
3the electrochemical in-situ Raman spectroscopic assay of fused salt Pt electrode surface fused salt under potentiostatic deposition condition;
Temperature controller: Chaoyang, Beijing robot Watch Factory CKW-3100;
Raman spectrometer: the HR800 type micro laser Raman spectrometer of Japanese Horiba Jobin Y ' von company;
Laser instrument: the IK3301R-G He-Cd 325nm ultraviolet laser of Japanese Kimmon Koha company;
Microscope (camera lens): the microscope (10x microlens) of Japanese O1ympus company;
Electrochemical workstation: Dutch AUTOLAB company PGSTAT30 electrochemical workstation;
Use crucible: titanium crucible; Working electrode: Pt sheet, contrast electrode: Pt silk, to electrode: titanium crucible;
The KNO of 623K
3fused salt is the original position Raman spectrogram of Pt electrode surface fused salt when negative sense increases current potential and forward increase current potential under potentiostatic deposition condition, respectively as is illustrated by figs. 11 and 12.
Observe each spectrum shown in Figure 11, find when scanning current potential be-1.45V and more negative time, except at 1053cm in spectrum
-1and 1350cm
-1there is NO in place
3 -and NO
2 -v
1outside vibration peak, at 800cm
-1near and 1130cm
-1near have new Raman peak to occur.By analysis, think that these two peaks are respectively O
2 2-and O
2 -raman characteristic peak, namely think that current potential reaches NO
3 -reduction potential after, first there is NO
3 -reduction reaction, NO
3 --2e=NO
3 -+ O
2-, the O of generation
2-meeting and NO
3 -continuation effect generates O
2 2-and O
2 -: O
2-+ NO
3 -=NO
2 -+ O
2 2-, O
2 2-+ 2NO
3 -=2NO
2 -+ 2O
2 -.
Observe each spectrum shown in Figure 12, find under each scanning current potential, at 800cm
-1and 1130cm
-1place still old new Raman peak occurs think it is also by O
2 2-and O
2 -caused by vibration, so think O in fused salt
2-there occurs three step oxidation reaction: 2O
2--2e=O
2 2-, O
2 2--e=O
2 -, O
2 --e=O
2.
Embodiment two:
Under 823K, Li
2cO
3-Na
2cO
3fused salt under cyclic voltammetry condition, the electrochemical in-situ Raman spectroscopic assay of the thin liquid layer of Ni electrode surface fused salt;
Temperature controller: Chaoyang, Beijing robot Watch Factory CKW-3100;
Raman spectrometer: the HR800 type micro laser Raman spectrometer of Japanese Horiba Jobin Y ' von company;
Laser instrument: the IK3301R-G He-Cd 325nm ultraviolet laser of Japanese Kimmon Koha company;
Microscope (camera lens): the microscope (10x microlens) of Japanese Olympus company;
Electrochemical workstation: Dutch AUTOLAB company PGSTAT30 electrochemical workstation;
Use crucible: graphite crucible; Working electrode: Ni sheet, contrast electrode: Pt silk, to electrode: graphite flake;
Cyclic voltammetry experiment sweep velocity: 0.04V/s;
Under 823K, Li
2cO
3-Na
2cO
3the cyclic voltammetry curve of fused salt as shown in figure 13.The original position Raman spectrogram of the thin liquid layer of Ni electrode surface in current potential negative sense and forward scan process under this condition, respectively as shown in Figure 14, Figure 15.
Observe cyclic voltammetry scan curve shown in Figure 13, find in negative direction scanning process, occur three reduction current peaks A, B and C, in forward scan process, occur D, E, F and G tetra-oxidation peak.
Think that A peak correspond to CO
3 2-reduction: CO
3 2-+ 4e=C+3O
2-, in addition, think that oxidation peak B and C correspond to Na in fused salt respectively
+and Li
+the reduction of two kinds of alkali metal ions: Na
++ e=Na, Li
++ e=Li; Think and correspond to the oxidizing process of Li and Na respectively: Li-e=Li by oxidation current peak D and E occurred in forward scan process
+, Na-e=Na
+; And F and G correspond to carbon and CO respectively
3 2-oxidation: C+2O
2-=CO
2+ 4e, 2CO
3 2--4e=O
2+ 2CO
2, CO
3 2-oxidation cause anode limiting current in CV curve.
Observe the Raman spectrum shown in Figure 14, find, when scanning current potential drops to below-1.0V, to be positioned at 1065cm
-1the CO at place
3 2-v
1the intensity of vibration peak decreases, because the first reduction current peak A of Figure 13 is by CO
3 2-reduction causes, and causes CO
3 2-the decline of concentration; Raman spectrum as shown in Figure 15, can find out, when current potential scans 0.80V from 0.15V, and CO
3 2-v
1vibration peak intensity is increasing trend, and ate electrode CO is described
3 2-content is raising gradually, thiss is presumably because that anode is to CO in fused salt
3 2-the attraction of anion radical causes CO
3 2-anode migration causes CO near anode
3 2-caused by concentration increases, and when scanning current potential and being increased to 0.92V by 0.80V, CO
3 2-v
1vibration peak intensity is reduction trend, this is because under this current potential, there occurs CO
3 2-oxidation reaction, cause its concentration to decline.
Claims (7)
1. a melten salt electriochemistry original position Raman spectral measurement microscopic heating stand, is characterized in that comprising thermal station shell, burner hearth, thermal station lid and pillar and base;
The side wall upper part of described thermal station shell is provided with contact conductor through hole, thermal station enclosure is provided with thermal station shell circulating cooling water route, thermal station outer casing bottom is provided with pillar connecting hole and resistance wire through hole, is fixed with resistance wire binding post at thermal station outer casing bottom;
Described burner hearth comprises burner hearth main body, is provided with sample cell places groove at the top of burner hearth main body, and the burner hearth main body below sample cell placement groove is provided with hearth thermocouple through hole, and described sample cell is placed groove and is connected with hearth thermocouple through hole; At the top of burner hearth main body, sample cell places the left and right sides of groove and is symmetrically arranged with and puts contact conductor strip groove, the burner hearth main body of putting contact conductor strip groove and sample cell placement groove both sides is evenly equipped with resistance wire mounting hole respectively, in resistance wire mounting hole, be provided with spiral resistance wire, described resistance wire and burner hearth main body insulate and arrange;
Described thermal station lid comprises thermal station lid main body, and the inside of thermal station lid main body is provided with thermal station lid circulating cooling water route, and the middle part of thermal station lid main body is provided with microlens through hole;
Described base is provided with pillar mounting hole, and described pillar is fixed in the pillar mounting hole of base, is provided with pillar thermopair through hole, is fixed with thermopair binding post in the bottom of pillar at the middle part of pillar;
Described thermal station lid is arranged on the top of thermal station shell, and it is corresponding that microlens through hole and sample cell place groove; Burner hearth is fixed in the space that thermal station lid and thermal station shell formed, and the resistance wire in burner hearth is connected with resistance wire binding post through after the resistance wire through hole of thermal station shell, and resistance wire and thermal station casing insulation are arranged; Pillar is threaded with the pillar connecting hole of thermal station shell, and thermopair binding post is fixed with thermopair, and the hot junction of thermopair is arranged in hearth thermocouple through hole through after pillar thermopair through hole, and the cold junction of thermopair is connected with thermopair binding post.
2. melten salt electriochemistry original position Raman spectral measurement microscopic heating stand according to claim 1, is characterized in that described burner hearth main body adopts silicon carbide material.
3. melten salt electriochemistry original position Raman spectral measurement microscopic heating stand according to claim 1, is characterized in that described resistance wire adopts high temperature nickel evanohm Ni
20cr
80.
4. melten salt electriochemistry original position Raman spectral measurement microscopic heating stand according to claim 1, the resistance wire putting contact conductor strip groove both sides described in it is characterized in that adopts mode in parallel to connect.
5. with microscopic heating stand according to claim 1 with the use of sample cell, it is characterized in that comprising crucible, the top of crucible be provided with quartz cover; Be symmetrically arranged with two through holes on the top of crucible wall, described through hole is corresponding with putting contact conductor strip groove; Crucible adopts conductive material, and it is connected with to contact conductor, is respectively arranged with working electrode and contrast electrode in crucible, and working electrode and contrast electrode go between with working electrode respectively to go between with contrast electrode and be connected.
6. with microscopic heating stand according to claim 1 with the use of sample cell, it is characterized in that comprising crucible, the top of crucible be provided with quartz cover; Be symmetrically arranged with two through holes on the top of crucible wall, described through hole is corresponding with putting contact conductor strip groove; Be respectively arranged with electrode, working electrode and contrast electrode in crucible, electrode, working electrode and contrast electrode are connected with going between to contact conductor, working electrode to go between with contrast electrode respectively.
7. the sample cell according to claim 5 or 6, is characterized in that described crucible and quartz cover are tightly connected.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104502324A (en) * | 2014-12-29 | 2015-04-08 | 东北大学 | Micro heating platform for measuring molten salt electriochemistry in-situ Raman spectrum and sample cell |
| CN107389591A (en) * | 2017-06-13 | 2017-11-24 | 中国科学技术大学 | The dual-purpose in situ detection hermetic electrolyte pond of Raman and infrared spectra, use its method and application thereof |
| CN108132238A (en) * | 2018-02-14 | 2018-06-08 | 福州大学 | A kind of high frequency heating electrochemistry-Surface enhanced Raman spectroscopy detecting system |
| 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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2014
- 2014-12-29 CN CN201420852018.XU patent/CN204405549U/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104502324A (en) * | 2014-12-29 | 2015-04-08 | 东北大学 | Micro heating platform for measuring molten salt electriochemistry in-situ Raman spectrum and sample cell |
| CN104502324B (en) * | 2014-12-29 | 2017-04-05 | 东北大学 | Melten salt electriochemistry original position Raman spectral measurement microscopic heating stands |
| CN107389591A (en) * | 2017-06-13 | 2017-11-24 | 中国科学技术大学 | The dual-purpose in situ detection hermetic electrolyte pond of Raman and infrared spectra, use its method and application thereof |
| CN107389591B (en) * | 2017-06-13 | 2020-03-31 | 中国科学技术大学 | Raman and infrared spectrum dual-purpose in-situ detection sealed electrolytic cell and use method thereof |
| CN108132238A (en) * | 2018-02-14 | 2018-06-08 | 福州大学 | A kind of high frequency heating electrochemistry-Surface enhanced Raman spectroscopy detecting system |
| 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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