CN113916765A - In-situ heating type Raman-electrochemical reaction device - Google Patents
In-situ heating type Raman-electrochemical reaction device Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 68
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 48
- 238000003487 electrochemical reaction Methods 0.000 title claims abstract description 20
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 70
- 238000012360 testing method Methods 0.000 claims abstract description 45
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 27
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- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
An in-situ heating Raman-electrochemical reaction device. The invention particularly relates to an in-situ heating Raman-electrochemical reaction device. The invention aims to solve the problem that the existing in-situ Raman test method is only suitable for detecting metal corrosion at a specific temperature and cannot detect corrosion conditions at different temperatures. The device consists of a first beaker, a second beaker, a peristaltic pump, a Raman optical microscope, a Raman test pool, an in-situ heating table, an air bag and an external power supply voltage controller; and the lower part of the Raman test pool 5 is provided with an in-situ heating table, and the in-situ heating table is connected with an external power supply voltage controller through a pipeline. The in-situ Raman spectrum is coupled with an in-situ electrochemical testing device, so that dynamic and differential detection of local corrosion of metal at different temperatures is realized. The method helps to overcome the defect of local corrosion micro-area information, optimize the material structure and solve the problems of unstable material structure and the like.
Description
Technical Field
The invention particularly relates to an in-situ heating Raman-electrochemical reaction device.
Background
When an electrochemical material is researched, parameters such as physical and electrochemical information of a local corrosion area are commonly used for representing the corrosion rate of metal. However, in recent years, a great deal of study of scholars finds that the accuracy is greatly limited when the corrosion rate of metal is tested due to the limitation of mesoscopic size and the irregular limitation of local corrosion areas, and the acquisition of local corrosion information and the understanding of corrosion mechanisms are influenced. Raman spectroscopy is widely used in research of electrochemical materials as a technique that can be used to analyze information such as a spatial structure and an electrochemical component of a material on a molecular level. The Raman spectrum has the advantages of large information amount, simple sample pretreatment, small water interference, no damage and the like, and the corrosion detection of the coupling optical microscope and the Raman spectrum also makes new progress in the targeted research of the local corrosion of metal. By coupling the electrochemical in-situ test device with the in-situ Raman spectrum technology, information such as potential, surface chemistry and the like can be acquired, and the blank of local corrosion micro-area information is overcome. However, the existing in-situ Raman test method is only suitable for detecting metal corrosion at a specific temperature, and cannot detect corrosion conditions at different temperatures.
Disclosure of Invention
The invention provides an in-situ heating Raman-electrochemical reaction device, aiming at solving the problem that the existing in-situ Raman testing method is only suitable for detecting metal corrosion at specific temperature and cannot detect corrosion conditions at different temperatures.
The invention relates to an in-situ heating type Raman-electrochemical reaction device which comprises a first beaker, a second beaker, a peristaltic pump, a Raman optical microscope, a Raman test pool, an in-situ heating table, an air bag and an external power supply voltage controller, wherein the first beaker is connected with the first beaker; the device comprises a first beaker, a gas bag, a Raman test pool, a liquid outlet, a liquid inlet, a liquid outlet and a liquid outlet, wherein the first beaker is communicated with a liquid inlet of a peristaltic pump through a pipeline, the liquid outlet of the peristaltic pump is communicated with an inlet of the gas bag through a pipeline, an outlet of the gas bag is communicated with a liquid inlet of the Raman test pool through a pipeline, the liquid outlet of the Raman test pool is communicated with a second beaker through a pipeline, a Raman optical microscope is arranged above the Raman test pool, an in-situ heating table is arranged at the lower part of the Raman test pool, and the in-situ heating table is connected with an external power supply voltage controller through a pipeline.
The invention has the beneficial effects that:
the in-situ heating Raman-electrochemical reaction device designed by the invention overcomes the defects of the traditional corrosion cell in metal corrosion rate measurement, improves the accuracy of corrosion rate test, can realize dynamic and differential detection of local corrosion of metal at different temperatures by using the in-situ heating table, can better understand the degradation mechanism of the material from the perspective of the material structure, is beneficial to optimizing the material structure and solves the instability of the material structure. The temperature can be changed rapidly and accurately in the corrosion test process, and dynamic and differential detection of local corrosion of metal at different temperatures can be realized.
Drawings
FIG. 1 is a schematic structural diagram of an in-situ heating Raman-electrochemical reaction device;
FIG. 2 is a schematic view of a first heater chip;
fig. 3 is a schematic structural view of a second heat patch.
Detailed Description
The technical solution of the present invention is not limited to the following embodiments, but includes any combination of the embodiments, and the following embodiments are described with reference to the accompanying drawings.
The first embodiment is as follows: the in-situ heating type Raman-electrochemical reaction device in the embodiment is composed of a first beaker 1, a second beaker 2, a peristaltic pump 3, a Raman optical microscope 4, a Raman test pool 5, an in-situ heating table 6, an air bag 7 and an external power supply voltage controller 8; the utility model discloses a Raman test device, including a Raman test pool 5, a first beaker 1, a gasbag 7, a Raman test pool 5, a normal position heating table 6, an external power supply voltage controller 8, a pipeline, a Raman optical microscope 4, a normal position heating table 6, a Raman optical microscope, a peristaltic pump 3, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a peristaltic.
In the present embodiment, the raman test cell 5 is composed of an upper half and a lower half; a central observation area is arranged in the center of the upper half part, the central observation area is of a trapezoidal inwards concave structure, the depth of the inwards concave structure is 4mm, and the bottom of the trapezoidal table is sealed through an ultrathin cover glass; the lower end surface of the upper half part is provided with a groove structure, and the groove structure is provided with a lining gasket; the length of the upper half part is 70mm, the width of the upper half part is 50mm, and the height of the upper half part is 10 mm; the lower half part is 70mm in length, 50mm in width and 12mm in height; the width of the groove structure is 1mm, and the depth of the groove structure is 0.7 mm; the diameter of the lining gasket is 16mm, and the thickness of the lining gasket is 1 mm; the left side and the right side of the upper part are transversely symmetrically provided with a circular through hole with the diameter of 5mm respectively, and the length of the through hole is 19 mm; on the basis of the through hole, a small hole with the diameter multiplied by the length of 3 multiplied by 4.5mm is continuously punched inwards; the periphery of the frame is longitudinally provided with 8 bolt holes with the diameter of 4 mm; semicircular holes with the radius multiplied by the depth of 3 multiplied by 3mm are symmetrically distributed at two sides of the central observation area, a square hole with the length multiplied by the width multiplied by the depth of 1 multiplied by 1mm is continuously drilled upwards in the hole, so that the semicircular holes at the lower end surface are communicated with the through holes which are transversely distributed, and a flow channel is formed. And 8 bolt holes with the diameter of 4mm are longitudinally arranged on the periphery of the symmetrical lower half part. The water solution of the objective lens in the metal corrosion process can be ensured to be a plane, the flow of the ultrathin solution can be realized by the embedded gasket, the overall sealing performance is good, and the stability of the Raman test pool is ensured.
The present embodiment incorporates an air bag that reduces the backflow phenomenon caused by the pulses of the peristaltic pump, accommodates the bubbles generated during the pulsation process, and also allows the gas to be discharged through the filter port. The hose section behind the bladder still has air that will enter the raman test cell along the tubing, so the length of tubing connecting the bladder and raman cell should be minimized.
Because a certain amount of gas exists in the Raman test cell pipe section, a suction injector can be added behind the pipe section behind the Raman test cell to reduce the air quantity of the part for evacuation. It should be noted that the time of the air extraction must be strictly controlled during the experiment to avoid excessive air extraction, and when the liquid enters the raman cell and forms a narrow flow channel in the cell, it flows out directly through the flow channel, and the liquid cannot completely fill the raman cell.
The front pipe section of the Raman test pool is additionally provided with the air bag and the exhaust pipe, so that the influence of pulsating fluid and gas in the front pipe on an experiment can be eliminated, the influence of the gas in the Raman test pool on the experiment can be effectively reduced by additionally arranging the vacuumizing at the rear section of the Raman test pool, and the air bag and the exhaust pipe can be mutually supplemented, so that the influence on the experiment due to the existence of the gas is further reduced.
The embodiment couples the Raman needle tip enhancement technology and the electrochemical corrosion, realizes in-situ detection, and well overcomes the defect of the traditional corrosion cell in measuring the metal corrosion rate.
The testing process of the embodiment can not damage the interface between the original sample and the corrosive environment, and is a nondestructive testing technology.
This embodiment heats through external power supply voltage control resistance to realize the quick and accurate change of temperature in the corrosion test process, and then realize the developments and the difference detection of metal local corrosion under the different temperatures.
The embodiment utilizes the peristaltic pump to control the flow of the solution in the hose, thereby realizing the stable flow of the corrosive solution.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the Raman optical microscope 4 consists of a micrometer screw, a piezoelectric ceramic positioning module, a fine adjustment table, an AD/DC voltage module, a stepping motor and a PID control system. The rest is the same as the first embodiment.
The peristaltic pump driven by the stepping motor in the embodiment can be accurately controlled, and the rotation angle of the pump head has the advantage of high flow resolution.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the Raman test cell 5 consists of an upper half part and a lower half part; the lower end surface of the upper half part is provided with a groove structure, and the groove structure is provided with a lining gasket; the bottom surface of the lower half part is provided with an annular runway-shaped sealing groove for additionally installing a rubber sealing ring. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: a transparent hard plastic sheet is additionally arranged at the top sight hole position of the upper half part, the size of the transparent hard plastic sheet is 30 mm multiplied by 20mm, and the thickness of the transparent hard plastic sheet is 0.2 mm. The rest is the same as one of the first to third embodiments.
This embodiment requires that the plastic sheet surface is clean, and the light transmissivity is good. First, the plastic sheet was attached to the top of the raman cell trough with 502 glue, and then the perimeter of the plastic sheet was sealed with a sealing glue to ensure that the seal was watertight under pressure.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and a quartz glass sheet with the thickness of 0.1mm is additionally arranged on the bottom surface of the lower half part, and the size of the glass sheet is 7 multiplied by 14 mm. The rest is the same as one of the first to fourth embodiments.
The glass sheet is required to be well attached to the Raman test pool, is positioned inside the sealing ring and is not broken. The glass sheet is fixed at the bottom of the Raman battery tank by tweezers, and then the four sides of the Raman battery tank are sealed by sealant, so that the sealing is ensured to be completely matched with the bottom of the Raman test tank and keep parallel, and the blocking of flow channels at two sides is prevented.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the heating mode of the in-situ heating table 6 is resistance heating. The rest is the same as one of the first to fifth embodiments.
In the present embodiment, the local temperature is increased by resistance heating. Throughout the system, it is desirable that the temperature of the rack remain constant while the temperature of the heated surface platform rises rapidly. By controlling the magnitude of the current, the temperature of the heating platform can be controlled rapidly and dynamically.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the in-situ heating table 6 is provided with a first heating sheet and a second heating sheet; the first heating plate and the second heating plate are arranged side by side, and a distance of 100 mu m is formed between the first heating plate and the second heating plate; the minimum distance from the in-situ heating table 6 to the lower bottom surface of the Raman test cell 5 is 10 μm; the substrate of the in-situ heating table 6 is of a thinning structure, and the thickness of the substrate is 10 micrometers. The rest is the same as one of the first to sixth embodiments.
The substrate behind the heating zone is designed into a partially thinned structure, and the thickness of the thinned zone is 10 μm; dimension of 10 μm from edge
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the material of the mechanical support substrate of the in-situ heating platform 6 is single crystal Si, and the material of the insulating layer is Si2And O, selecting Cr as a metal adhesion layer material of the heating table. The rest is the same as one of the first to seventh embodiments.
Example (b):
an in-situ heating Raman-electrochemical reaction device consists of a first beaker 1, a second beaker 2, a peristaltic pump 3, a Raman optical microscope 4, a Raman test pool 5, an in-situ heating table 6, an air bag 7 and an external power supply voltage controller 8; the utility model discloses a Raman test device, including a Raman test pool 5, a first beaker 1, a gasbag 7, a Raman test pool 5, a normal position heating table 6, an external power supply voltage controller 8, a pipeline, a Raman optical microscope 4, a normal position heating table 6, a Raman optical microscope, a peristaltic pump 3, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a Raman optical microscope, a peristaltic pump, a peristaltic. The main material of the raman test cell is polylactic acid (PLA), which is available through 3D printers. Polylactic acid is also called polylactide (polylactide), which belongs to polyester engineering plastics. Polylactic acid is polymerized by using lactic acid as a main raw material. The lactic acid has wide sources, is green and can be regenerated. The product is biodegradable, has good thermal stability, good solvent resistance and good biocompatibility, and has transparency, luster, heat resistance and hand feeling after being processed. Has certain antibacterial, flame retardant and ultraviolet ray resistant performance. Is an ideal recyclable green polymer engineering material.
Claims (8)
1. An in-situ heating Raman-electrochemical reaction device is characterized in that: the in-situ heating Raman-electrochemical reaction device consists of a first beaker (1), a second beaker (2), a peristaltic pump (3), a Raman optical microscope (4), a Raman test pool (5), an in-situ heating table (6), an air bag (7) and an external power supply voltage controller (8); the utility model discloses a Raman test device, including first beaker (1), peristaltic pump (3), gasbag (7), raman test pond (5), normal position heating table (6) are connected with external power supply voltage controller (8) through the pipeline, the inlet of first beaker (1) through pipeline and peristaltic pump (3) is linked together, the liquid outlet of peristaltic pump (3) is linked together through the import of pipeline and gasbag (7), the inlet of the export of gasbag (7) through pipeline and Raman test pond (5) is linked together, the liquid outlet of Raman test pond (5) is linked together through pipeline and second beaker (2), the top of Raman test pond (5) sets up Raman optical microscope (4), the lower part of Raman test pond (5) is provided with normal position heating table (6), normal position heating table (6) are connected with external power supply voltage controller (8) through the pipeline.
2. The in-situ heating type raman-electrochemical reaction device according to claim 1, wherein: the Raman optical microscope (4) is composed of a micrometer caliper, a piezoelectric ceramic positioning module, a fine adjustment table, an AD/DC voltage module, a stepping motor and a PID control system.
3. The in-situ heating type raman-electrochemical reaction device according to claim 1, wherein: the Raman test pool (5) consists of an upper half part and a lower half part; the lower end surface of the upper half part is provided with a groove structure, and the groove structure is provided with a lining gasket; the bottom surface of the lower half part is provided with an annular runway-shaped sealing groove for additionally installing a rubber sealing ring.
4. The in-situ heating type raman-electrochemical reaction device according to claim 3, wherein: a transparent hard plastic sheet is additionally arranged at the top sight hole position of the upper half part, the size of the transparent hard plastic sheet is 30 mm multiplied by 20mm, and the thickness of the transparent hard plastic sheet is 0.2 mm.
5. The in-situ heating type raman-electrochemical reaction device according to claim 3, wherein: and a quartz glass sheet with the thickness of 0.1mm is additionally arranged on the bottom surface of the lower half part, and the size of the glass sheet is 7 multiplied by 14 mm.
6. The in-situ heating type raman-electrochemical reaction device according to claim 1, wherein: the heating mode of the in-situ heating table (6) is resistance heating.
7. The in-situ heating type raman-electrochemical reaction device according to claim 1, wherein: the in-situ heating table (6) is provided with a first heating sheet and a second heating sheet; the first heating plate and the second heating plate are arranged side by side, and a distance of 100 mu m is formed between the first heating plate and the second heating plate; the minimum distance from the in-situ heating table (6) to the lower bottom surface of the Raman test cell (5) is 10 mu m; the substrate of the in-situ heating table (6) is of a thinning structure, and the thickness of the substrate is 10 micrometers.
8. The in-situ heating type raman-electrochemical reaction device according to claim 1, wherein: the mechanical support substrate material of the in-situ heating table (6) is selected from single crystal Si, and the insulating layer material is selected from Si2And O, selecting Cr as a metal adhesion layer material of the heating table.
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| CN202111293479.9A CN113916765A (en) | 2021-11-03 | 2021-11-03 | In-situ heating type Raman-electrochemical reaction device |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204405549U (en) * | 2014-12-29 | 2015-06-17 | 东北大学 | Melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell |
| CN105136771A (en) * | 2015-08-21 | 2015-12-09 | 山东大学 | Multifunctional gas high-pressure in situ Raman test cell and application thereof |
| CN106990094A (en) * | 2017-05-11 | 2017-07-28 | 华东理工大学 | The situ Raman Spectroscopy measuring method and measurement apparatus of vaporization at high temperature corrosivity fused salt |
| CN110186900A (en) * | 2019-06-11 | 2019-08-30 | 中国石油大学(华东) | A kind of test pond and its design method of the test metal erosion of coupling Raman spectrum |
| CN112014308A (en) * | 2020-09-07 | 2020-12-01 | 中国石油大学(华东) | Raman-enhanced electrochemical corrosion cell and control method thereof |
-
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- 2021-11-03 CN CN202111293479.9A patent/CN113916765A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204405549U (en) * | 2014-12-29 | 2015-06-17 | 东北大学 | Melten salt electriochemistry original position Raman spectral measurement microscopic heating stand and sample cell |
| CN105136771A (en) * | 2015-08-21 | 2015-12-09 | 山东大学 | Multifunctional gas high-pressure in situ Raman test cell and application thereof |
| CN106990094A (en) * | 2017-05-11 | 2017-07-28 | 华东理工大学 | The situ Raman Spectroscopy measuring method and measurement apparatus of vaporization at high temperature corrosivity fused salt |
| CN110186900A (en) * | 2019-06-11 | 2019-08-30 | 中国石油大学(华东) | A kind of test pond and its design method of the test metal erosion of coupling Raman spectrum |
| CN112014308A (en) * | 2020-09-07 | 2020-12-01 | 中国石油大学(华东) | Raman-enhanced electrochemical corrosion cell and control method thereof |
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