CN110186900A - A kind of test pond and its design method of the test metal erosion of coupling Raman spectrum - Google Patents

A kind of test pond and its design method of the test metal erosion of coupling Raman spectrum Download PDF

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Publication number
CN110186900A
CN110186900A CN201910500977.2A CN201910500977A CN110186900A CN 110186900 A CN110186900 A CN 110186900A CN 201910500977 A CN201910500977 A CN 201910500977A CN 110186900 A CN110186900 A CN 110186900A
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corrosion
pond
test
raman spectrum
coupling
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CN110186900B (en
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齐建涛
汪振文
刘伟
陈梦瑶
胡爽飞
丁一航
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China University of Petroleum East China
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • G01N17/006Investigating resistance of materials to the weather, to corrosion, or to light of metals
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Life Sciences & Earth Sciences (AREA)
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  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Environmental Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)

Abstract

The invention discloses the test ponds and its design method of a kind of coupling Raman spectrum test metal erosion, the peristaltic pump fixed time using constant volume and novel corrosion pond, etchant solution is pumped out from beaker, into corrosion pond, then after corrosion reaction occurring, it flows out, and then is transferred in the beaker of end with solution.This testing process can overcome conventional dead etchant solution to extend influence of the etchant solution environmental change to corrosion mechanism at any time, can expand the accuracy of more technology coupling measurement corrosion processes.It is worth noting that, the top half central design that novel corrosion pond is observed close to object lens halfpace shape concave inward structure, is conducive to the effective observed range for expanding object lens and metal to be measured, raising amplification factor provides more local corrosion information.In addition, the design of general corrosion pond is light and handy economical, it can be achieved that 3D printing forms.

Description

A kind of test pond and its design method of the test metal erosion of coupling Raman spectrum
Technical field
The present invention relates to a kind of test ponds of metal erosion, in particular to are suitable for a kind of coupling Raman spectrum and test metal The test pond and its design method of corrosion.
Background technique
The electrochemistry and physical message of local corrosion microcell are the important parameters for characterizing rate of metal corrosion, however due to office The limitation of the irregular and mesoscopic size of portion's corrosion area is so that measuring accuracy is limited.Raman spectroscopy is that one kind can be used for point The technology for analysing the information such as electrochemistry ingredient, the space structure of molecular scale, with accommodating, information is more, sample pretreatment is simple, water The features such as interference is small, non-intruding.It is detected with fortune in medicine by extensive, illicit drugs inspection, historical relic research, food detection, battery electricity Pole investigation of materials.In recent years, the research method of multidisciplinary mutually warm more technology couplings receives more and more concerns.For metal In the research of local corrosion, there has also been new progresses for the Corrosion monitoring of coupling Raman spectrum and optical microscopy.Ramya et al. is logical The chemical constituent of film layer when in-situ Raman has measured spot corrosion is crossed with the variation in reaction time.(S.Ramya,et.al.Applied Surface Science, 2018,428:1106-1118) Raman spectrum cooperation optical microscopy tool can be determined in spot corrosion position The corrosion product of body, and then clarified the etch-proof mechanism of surface layer element of the modified steel.However, the Raman corrosion that they propose Pond uses the form of built-in corrosive liquid, and this corrosion pond oxygen in long-time reaction process constantly consumes even depleted. This environment can not be matched with the true corrosive environment of metal, thus be not suitable for studying long-time metal erosion mechanism.
Summary of the invention
In order to overcome the drawbacks of corroding pond solution stand in tradition corrosion pond and change over time, also for the more technologies of realization Coupling Research metal erosion it is true and reliable, the invention proposes a kind of novel metal corrosion ponds and its design method.Using increasing Add etchant solution inlet and outlet, corrosion pond inner flow passage and corrode the two-part washer in pond or more, and the sealed connection in corrosion pond Equal part ways change the structure design in tradition corrosion pond, cooperate peristaltic pump and circuit design and then guarantee that more technology couplings are ground Study carefully the accuracy of metal erosion behavior.
To achieve the goals above, the present invention adopts the following technical scheme: operator is using constant volume and fixes time Peristaltic pump extracts etchant solution out from beaker, is transported in the novel corrosion pond for being placed on Raman test platform, and then occurs Dynamic Corrosion, and corrode the Raman spectrum above pond test microscope capture corrosion product spectral information, and etchant solution from The outlet of corrosion pond is output in terminal beaker.
Wherein, corrode a height of 70x 50x 10mm of long x wide x of top half (2) monnolithic case in pond;Central observation area For halfpace shape concave inward structure, depth 4mm, the long x wide in top is 18.5x 9.5mm and the long x wide in bottom is 14 x 8mm;This Outside, the left and right sides of upper part is lateral symmetry respectively opens the circular through hole (1.) that a diameter is 5mm, the long 19mm of through-hole;It is logical at this On the basis of hole, continue inwardly to make a call to the aperture (2.) that a diameter x length is 3x 4.5mm;It is 4mm's that surrounding, which longitudinally opens 8 diameters, Bolt hole;It is worth noting that, lower end surface, there are groove and runner, groove size is long 18 mm, both ends semicircle radius 5mm, recessed Groove width x depth is 1x 0.7mm;Central area of observation coverage two sides are symmetrically distributed with the semicircle orifice (4.) that radius x depth is 3x 3mm, at this The square hole (3.) for making a call to that one long x wide x depth is 1x 1x 1mm is continued up in hole, so guarantees the semicircle orifice and cross of lower end surface It connects to both through-holes of distribution, forms runner.
Corrode part (3) under pond in contrast.The a height of 70x 50x 12mm of the long x wide x of its monnolithic case;Surrounding is longitudinal Open the bolt hole that 8 diameters are 4mm.
The present invention has the advantage that
(1) the just metal erosion in the environment such as metal erosion pond analog long-time burn into different fluid state of solution flowing Mechanism has expanded the application range and accuracy of more technology coupling measurement technologies;
(2) the halfpace shape concave inward structure for the metal erosion pond top half that just solution flows is conducive to expand object lens and gold to be measured The effective observed range belonged to improves amplification factor, provides more local corrosion information;
(3) just the metal erosion pond of solution flowing can realize 3D printing, efficiently molding and cost economy.
Detailed description of the invention
Fig. 1 is the flow chart for coupling Raman spectrum test metal erosion.
Fig. 2 is the part drawing for corroding part on pond, wherein Fig. 2 a is the CAD X-Y scheme of top half;Fig. 2 b is the upper half Divide lower end surface X-Y scheme;Fig. 2 c is the cross-sectional view (position A-A in corresponding diagram 2b) at the lateral symmetry axis in top half lower end surface.
Fig. 3 is the part drawing for corroding part under pond, wherein Fig. 3 a and 3b are the CAD X-Y schemes for corroding pond lower half portion.
Fig. 4 is corrosion pond assembling figure.
Fig. 5 is the size table of corresponding diagram 2c mesoporous.
In figure: R2.5-M4 bolt radius, 2.5mm;R3-runner semicircle pore radius, 3mm;R5-groove semicircle inside radius, 5mm;R6-groove semicircle outer radius, 6mm
Specific embodiment
The present invention will be further explained below with reference to the attached drawings:
According to Fig. 2 and Fig. 3,3D printing metal erosion pond;
According to Fig. 4, ultra-thin coverslip (0.1mm is thick) is adhered in corrosion pond top half by 502 seccotines first Entreat the halfpace structural base of the area of observation coverage;Then utilize washer (diameter and thickness is respectively 16mm and 1mm) by the recessed of top half Slot filling, and then sheet metal to be measured is put among corrosion pond, it is finally symmetrically tightened using 8 M4 bolts, pond will be corroded up and down Connection;
The flow chart of entire test device is built in conjunction with Fig. 1.
The specific embodiment of coupling Raman spectrum test metal erosion is: operator is using constant volume and fixes time Peristaltic pump extracts etchant solution out from beaker, is transported in the novel corrosion pond for being placed on Raman test platform, and then occurs Dynamic Corrosion, and corrode the Raman spectrum above pond test microscope capture corrosion product spectral information, and etchant solution from The outlet of corrosion pond is output in terminal beaker.

Claims (5)

1. this patent is related to the test pond and its design method of a kind of coupling Raman spectrum test metal erosion, structure feature It is:
A. the top half center area of observation coverage is halfpace shape concave inward structure, by ultra-thin coverslip by halfpace sealed bottom, guarantees object It is plane that mirror, which observes Process of Metallic Corrosion aqueous solution,;(width x depth is in addition, the fluted structure in the lower end surface of top half 1x0.7mm) guarantee that ultra-thin solution flowing and the sealing in corrosion pond up and down can be achieved in embedded gasket (diameter x is with a thickness of 16x1mm) Property is good;It is worth noting that, central area of observation coverage two sides are symmetrically distributed with semicircle orifice (radius x depth is 3x3mm), in the hole It continues up and makes a call to a square hole (long x wide x depth is 1x1x1mm), so guarantee the semicircle orifice of lower end surface and leading to for cross direction profiles Both holes connect, and form runner.
B. lower half portion upper surface is plane, and the angle of lower end surface four is cube structure (17x17mm), i.e., prominent cross structure (with a thickness of 3mm) guarantees the stability for corroding pond on observation platform.
C. coupling part is bolted using 8 symmetrical M8, guarantees integral sealing effect.
D. above-mentioned corrosion pond cooperation peristaltic pump and pipe-line system can realize the purpose of more technology coupling measurement metal erosion.
2. the test pond and its design method of a kind of coupling Raman spectrum test metal erosion as described in claim 1, special Sign is that corrosion pond is divided into dismountable two parts up and down, is equipped with cooperation peristaltic pump and hose size at left and right sides of top half With the solution inlet and outlet of flow transformation, corrosion pond top half inside is equipped with runner and the corrosion pond center area of observation coverage has halfpace shape Concave inward structure and bottom is sealed using ultra-thin coverslip, in addition, the lower end surface of top half is fluted and gasket construction.
3. the test pond and its design method of a kind of coupling Raman spectrum test metal erosion as described in claim 1, special Sign is that corrosion pond lower half portion upper surface is plane, for placing metal sample and maintaining the level for being vertically connected with end face;It is rotten The lower end surface for losing pond lower half portion is cross structure, guarantees that corrosion pond is placed in the stability on observation platform.
4. the test pond and its design method of a kind of coupling Raman spectrum test metal erosion as described in claim 1, special Sign is that the peristaltic pump that entire test process is fixed time using constant volume and the solution of corrosion front and back are placed in head and end beaker And Raman spectrum can directly detect corrosion pond center area of observation coverage metal.
5. the test pond and its design method of a kind of coupling Raman spectrum test metal erosion as described in claim 1, special Sign is that the optical microscopy of different amplification can monitor and record the variation of corrosion process metal surface pattern and Raman spectrum Corrosion pond center area of observation coverage metal can be directly detected, and then metal erosion pattern, the corrosion product changed with etching time is provided Raman spectrum and etchant solution change of component multiple dimensioned corrosion information.
CN201910500977.2A 2019-06-11 2019-06-11 Test pool for testing metal corrosion by coupling Raman spectrum and design method thereof Active CN110186900B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110530786A (en) * 2019-09-05 2019-12-03 北京科技大学 A kind of device of in-situ observation steel surface local corrosion germinating process
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
CN113008887A (en) * 2021-02-10 2021-06-22 中国石油大学(华东) Corrosion cell system convenient for researching metal corrosion by coupling optical microscope and tow electrode technology and use method thereof
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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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110530786A (en) * 2019-09-05 2019-12-03 北京科技大学 A kind of device of in-situ observation steel surface local corrosion germinating process
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
CN113008887A (en) * 2021-02-10 2021-06-22 中国石油大学(华东) Corrosion cell system convenient for researching metal corrosion by coupling optical microscope and tow electrode technology and use method thereof
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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