CN115290748A - System and method for detecting metal anodic oxidation behavior based on additional sound wave emission signal - Google Patents
System and method for detecting metal anodic oxidation behavior based on additional sound wave emission signal Download PDFInfo
- Publication number
- CN115290748A CN115290748A CN202210877330.3A CN202210877330A CN115290748A CN 115290748 A CN115290748 A CN 115290748A CN 202210877330 A CN202210877330 A CN 202210877330A CN 115290748 A CN115290748 A CN 115290748A
- Authority
- CN
- China
- Prior art keywords
- anodic oxidation
- time
- acoustic
- sample
- curve
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000003647 oxidation Effects 0.000 title claims abstract description 101
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 21
- 239000002184 metal Substances 0.000 title claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 43
- 239000003792 electrolyte Substances 0.000 claims description 15
- 238000002048 anodisation reaction Methods 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000002071 nanotube Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 238000013480 data collection Methods 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims 3
- 229910017855 NH 4 F Inorganic materials 0.000 claims 1
- 230000003247 decreasing effect Effects 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 11
- 230000000877 morphologic effect Effects 0.000 abstract description 2
- 230000006399 behavior Effects 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- 239000007788 liquid Substances 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000011897 real-time detection Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
-
- 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
- G01N21/84—Systems specially adapted for particular applications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/14—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object using acoustic emission techniques
-
- 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
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/8405—Application to two-phase or mixed materials, e.g. gas dissolved in liquids
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Acoustics & Sound (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)
Abstract
The invention discloses a system and a method for detecting metal anodic oxidation behavior based on an external sound wave emission signal, and aims to solve the problem that the existing anodic oxidation method is adopted to form a nano structure on an anode and needs to be observed and determined by a scanning electron microscope. The method for detecting the metal anodic oxidation behavior comprises the following steps: 1. the anode of the potentiostat is connected with the anodic oxidation sample, the cathode of the potentiostat is connected with the Pt electrode, and the back of the anodic oxidation sample is provided with an acoustic sensor; 2. carrying out an anodic oxidation test, and collecting acoustics, current signals and the pH of a system; 3. respectively drawing a time-current curve, a time-pH curve and a time-peak frequency curve; 4. and (4) estimating the micro morphology of the anodized sample after the anodic oxidation treatment through the test curve obtained in the third step. The invention directly judges the micro-nano structure prepared by anodic oxidation from data such as acoustic characteristics, electrochemical behavior and the like, and can save the step of observing and confirming the morphological characteristics by using a high-power electron microscope.
Description
Technical Field
The invention belongs to the technical field of metal or alloy material morphology analysis, and particularly relates to a prediction method for detecting anodic oxidation behavior and anodic oxidation micro morphology based on an external sound wave emission signal.
Background
The process of forming oxide film with special nanometer structure on the surface of sample by anode oxidation method with metal or alloy sample as anode is one method of preparing metal oxide base nanometer structure on the surface of metal material. The prepared special nano structure of the metal oxide has wide and excellent application prospect in the fields of magnetic medical treatment, energy battery electrodes, catalysis and the like. The specific nanostructure of metal-based oxides has a great influence on applications in different fields, and generally, only a surface array with relatively complete and ordered structure and at the nano level has excellent application potential, because the nanostructure with complete structure has larger surface area than an array with disordered structure. However, when oxide nanostructures are prepared on different metal-based surfaces, the desired nanostructures, such as nanotube-shaped or nanopore-shaped structures, can be prepared only under certain process conditions. In the current scientific research experiment, the special, complete and orderly nano array needs to be observed by a scanning electron microscope or related microscopic morphology under ultrahigh multiple on the surface of a sample after an anodic oxidation test to determine whether the process condition can be successfully prepared to obtain the required special nano array structure. For practical testing and potential future applications, observing the microscopic morphology of a sample with a high-power electron microscope requires both more testing time investment and increased testing and application costs for each sample to be examined.
In the nonlinear acoustic research, if bubbles are doped in a liquid (electrolyte in anodic oxidation), the received acoustic characteristic data is changed due to the obvious difference of physical properties such as density, acoustic impedance and the like between gas and liquid. When the amplitude of the incident sound wave is small, the change of the received acoustic signal is mainly in the sound velocity and the frequency dispersion of the sound absorption coefficient; when the incident sound wave is a large-amplitude sound wave, the propagation of the sound wave can cause the forced vibration of the bubbles to cause sound scattering, and the sound scattering is expressed as a strong nonlinear acoustic characteristic and has a very large difference with the bubble-free liquid. By utilizing the strong nonlinear acoustic characteristic of the bubble-containing liquid, the bubble-containing liquid can be combined with the generation and release specificity of bubbles in the anodic oxidation process to serve as a detection method for monitoring the anodic oxidation behavior. In the current electrochemical anode oxidation real-time detection method, no detection means for detecting the polarization state of the anode electrode in real time on line by using a nonlinear acoustic wave method is available.
Disclosure of Invention
The invention aims to solve the problem that the existing method of anodic oxidation requires a scanning electron microscope to observe and determine the nanostructure formed on the anode, and provides an acoustic signal characteristic which is based on the acoustic characteristics of bubbles in the anodic oxidation process and is used for representing the metal oxide nanotube structure generated by anodic oxidation by using an additional acoustic wave emission signal in combination with a current characteristic parameter in the anodic oxidation process.
The invention relates to a system for detecting metal anodic oxidation behavior based on an external sound wave emission signal, which comprises a potentiostat, a current data acquisition device, an acoustic emission signal acquisition device, a pH detector and a high-speed camera display device, wherein an anodic oxidation sample and a Pt electrode are placed in an electrolytic bath, the electrolytic bath is filled with electrolyte, the anode of the potentiostat is connected with the anodic oxidation sample, the cathode of the potentiostat is connected with the Pt electrode, the potentiostat is connected with the current data acquisition device, the back of the anodic oxidation sample is connected with an acoustic sensor, the acoustic sensor is connected with the acoustic emission signal acquisition device, the high-speed camera display device is connected with a mobile high-speed camera, and the mobile high-speed camera extends into the electrolytic bath and detects the bubble generation and growth conditions of the anodic oxidation sample.
The method for detecting the metal anodic oxidation behavior based on the additional acoustic emission signal is realized according to the following steps:
1. electrolyte is filled into an electrolytic cell, the anode of a constant potential rectifier is connected with an anodic oxidation sample, the cathode of the constant potential rectifier is connected with a Pt electrode, an acoustic sensor is arranged on the back of the anodic oxidation sample, and the acoustic sensor is used for detecting the acoustic characteristics of the electrolyte;
2. starting a constant potential rectifier to carry out an anodic oxidation test, and collecting acoustic and current signals and the pH of a system through an acoustic emission signal collecting device, a current data collecting device and a pH detector when micro bubbles are observed to be generated on the surface of an anodic oxidation sample in the anodic oxidation test;
3. drawing a time-current curve by taking the reaction time as an abscissa and the current data as an ordinate; drawing a time-pH curve by taking the reaction time as an abscissa and the pH as an ordinate; drawing a time-peak frequency curve by taking the reaction time as an abscissa and the peak frequency of the acoustic signal as an ordinate;
4. and (4) estimating the micro morphology of the anodized sample after the anodic oxidation treatment through the time-current curve, the time-pH curve and the time-peak frequency curve obtained in the third step.
The invention utilizes the real-time test phenomenon data in the on-line real-time monitoring anodic oxidation process, comprises monitoring means such as bubble acoustic characteristics, electrochemical behaviors, real-time high-speed camera shooting, micro-area pH and the like, integrates all real-time test monitoring data characteristics, corresponds to the microscopic nano-morphology observed by a high-power electron microscope, establishes the real-time acoustic characteristics, the electrochemical behaviors and the micro-area pH change mapping chart in the anodic oxidation process, and realizes the relationship construction of the process conditions, the real-time detection data chart and the nano-array microstructure, thereby directly judging the microstructure of the nano-structure prepared by anodic oxidation from the data such as the acoustic characteristics, the electrochemical behaviors and the like, omitting the step of observing and confirming the morphology characteristics by the high-power electron microscope, and creating conditions for shortening the test period and reducing the test cost.
The invention aims to provide a method for monitoring additional acoustic wave emission signals and current characteristic parameters in the anodic oxidation process in real time on line so as to represent whether the anodic oxidation generates a metal oxide nanotube nano structure or not, and realize the construction of the relationship of process conditions, a real-time detection data map and a nano array microstructure, so that the microstructure of the nano structure prepared by the anodic oxidation can be directly judged from data such as acoustic characteristics, electrochemical behaviors and the like, the step of observing and confirming the morphological characteristics by using a high-power electron microscope can be omitted, and conditions are created for shortening the test period and reducing the test cost.
Drawings
FIG. 1 is a schematic diagram of a system for detecting metal anodization behavior based on an applied acoustic emission signal in accordance with the present invention;
FIG. 2 is a graph of time-current during anodization in the third step of the example;
FIG. 3 is a graph of time versus pH during anodization in step three of the example;
FIG. 4 is a graph of time-peak frequency during anodization in step three of the example;
FIG. 5 is a surface microscopic topography (left) and a cross-sectional microscopic topography (right) of the anodized nanopore structure of the iron-based material obtained in the example.
Detailed Description
The first embodiment is as follows: the system for detecting the metal anodic oxidation behavior based on the external sound wave emission signal comprises a potentiostat 1, a current data acquisition device 2, an acoustic emission signal acquisition device 3, a pH detector 4 and a high-speed camera display device 5, wherein an anodic oxidation sample 9 and a Pt electrode 8 are placed in an electrolytic tank, electrolyte is filled in the electrolytic tank, the positive electrode of the potentiostat 1 is connected with the anodic oxidation sample 9, the negative electrode of the potentiostat 1 is connected with the Pt electrode 8, the potentiostat 1 is connected with the current data acquisition device 2, the back surface of the anodic oxidation sample is connected with an acoustic sensor 6, the acoustic sensor 6 is connected with the acoustic emission signal acquisition device 3, the high-speed camera display device 5 is connected with a high-speed moving camera 7, and the moving high-speed camera 7 extends into the electrolytic tank and detects the bubble generation and growth conditions of the anodic oxidation sample.
The embodiment provides an on-line real-time detection method for characterizing the electrochemical activity of an electrode and the degree of anodic oxidation of the electrode and judging the performance of a prepared nano array by using an Acoustic Emission (Acoustic Emission) technology.
The second embodiment is as follows: the present embodiment is different from the first embodiment in that an acoustic peak frequency signal is collected by the acoustic sensor 6.
The Acoustic sensor used in this embodiment is of model number WD FS63, physical acoustics Corporation.
The third concrete implementation mode: the method for detecting the metal anodic oxidation behavior based on the additional acoustic wave emission signal is implemented according to the following steps:
1. electrolyte is filled into an electrolytic cell, the anode of a potentiostat 1 is connected with an anodic oxidation sample 9, the cathode of the potentiostat 1 is connected with a Pt electrode 8, an acoustic sensor 6 is arranged on the back of the anodic oxidation sample, and the acoustic characteristics of the electrolyte are detected by using the acoustic sensor 6;
2. starting the potentiostat 1 to carry out an anodic oxidation test, and collecting acoustic and current signals and the pH of a system through the acoustic emission signal collection device 3, the current data collection device 2 and the pH detector 4 when micro bubbles are observed to be generated on the surface of an anodic oxidation sample 9 in the anodic oxidation test;
3. drawing a time-current curve by taking the reaction time as a horizontal coordinate and the current data as a vertical coordinate; drawing a time-pH curve by taking the reaction time as an abscissa and the pH as an ordinate; drawing a time-peak frequency curve by taking the reaction time as an abscissa and the peak frequency of the acoustic signal as an ordinate;
4. and (4) estimating the micro morphology of the anodized sample after the anodic oxidation treatment through the time-current curve, the time-pH curve and the time-peak frequency curve obtained in the third step.
The fourth concrete implementation mode: the difference between the present embodiment and the third embodiment is that in the first step, the anodized sample 9 is first subjected to ultrasonic cleaning treatment with acetone and alcohol-free ethanol solution.
The fifth concrete implementation mode: this embodiment differs from the third or fourth embodiment in that the anodized sample 9 described in step one is an iron-based material, a titanium-based material, a zinc-based material, or an aluminum-based material.
The sixth specific implementation mode is as follows: this embodiment mode andthe difference between the third and fifth embodiments is that the electrolyte in the first step contains NH with the mass fraction of 0.3% -0.8% in the glycol solution 4 F。
The seventh embodiment: the difference between the third embodiment and the sixth embodiment is that in the second anodic oxidation test, the anodic oxidation voltage is controlled to be 40V-90V, and the treatment time is controlled to be 1 min-5 min.
The specific implementation mode eight: the difference between the present embodiment and the third to seventh embodiments is that in the fourth step, when the pH value of the system is maintained at 7.85 ± 0.1 during the anodization test, the current curve decreases to 0.08 ± 0.01A in the first 20s of the anodization test and then slightly increases to 0.1 to 0.12A, the acoustic activity level in the first 80s of the anodization test in the time-peak frequency curve is higher than that in the later period of the test, and more than 90% of data points of the frequency peak in the first 80s of the anodization test are in the range of 0.1 to 0.3MHz, it is predicted that a regular nanotube array microstructure is formed on the surface of the anodized sample 9.
The acoustic activity level in the first 80s of the anodic oxidation test is higher than that in the later period of the test, which means that acoustic data points generated in the first 80s account for 80% -88% of all data points of the whole anodic oxidation test (180 s).
In the embodiment, the curve characteristics of the regular nano array generated after anodic oxidation are obtained by summarizing the time-current curve, the time-pH curve and the time-peak frequency curve, the characteristic range corresponds to a specific (nano tube array) micro-morphology structure, and the micro-morphology characteristics of the sample can be judged based on the characteristic range.
The specific implementation method nine: the present embodiment is different from the eighth embodiment in that in the four-step time-current curve, the current steadily increased and remained at 0.15A or less after 20s of the anodic oxidation test.
The embodiment is as follows: the method for detecting the metal anodic oxidation behavior based on the additional acoustic wave emission signal is implemented according to the following steps:
1. cutting a pure iron-based anodic oxidation sample into slices with the same size as the platinum electrode, grinding the slices by 600#, 1000#, and 2000# abrasive paper, sequentially performing ultrasonic treatment on the polished anodic oxidation sample by acetone and ethanol solution, and drying the polished anodic oxidation sample by blowing nitrogen to obtain a cleaned anodic oxidation sample, wherein the size of the pure iron-based anodic oxidation sample is 1.5cm x 1.5cm;
2. 20mL of anodic oxidation electrolyte containing 1.3 mol of H in ethylene glycol solution was prepared 2 O and NH with the mass fraction of 0.5 percent 4 F；
3. The electrolyte is filled into an electrolytic cell, the anode of a potentiostat 1 is connected with an anodic oxidation sample 9, the cathode of the potentiostat 1 is connected with a Pt electrode 8, and a PCI-2 data acquisition system and AEwin E4.30 software are used for measuring and preparing acoustic characteristic signals of the electrolyte at the sampling frequency of 2 MHz;
4. starting a potentiostat 1 to perform an anodic oxidation test, wherein the anodic oxidation voltage is 90V, the processing time of anodic oxidation is 180s respectively, simultaneously starting a high-speed camera device 5, a current data acquisition device 2 and a pH detector 4, and acquiring acoustics, the surface bubble morphology of a sample, a current signal and the pH of a system through an acoustic emission signal acquisition device 3, the high-speed camera device 5, the current data acquisition device 2 and the pH detector 4; data acquisition uses a PCI-2 data acquisition system and AEwin E4.30 software to acquire acoustic data at a sampling rate of 2MHz, acquired acoustic signals pass through a preamplifier in 60dB through AE output signals, a signal detection threshold is adjusted to 31dB, and the preamplifier is embedded with a band-pass filter with a frequency range of f =0.02-1 MHz;
5. after 150s of anodic oxidation, the constant potential rectifier automatically stops running, deionized water and ethanol are used for washing the sample after the anodic oxidation test, nitrogen is used for drying the sample, and then a scanning electron microscope is used for observing the microscopic morphology of the sample;
6. drawing a time-current curve by taking the reaction time as an abscissa and the current data as an ordinate; drawing a time-pH curve by taking the reaction time as an abscissa and the pH as an ordinate; drawing a time-acoustic signal curve by taking the reaction time as an abscissa and the peak frequency as an ordinate;
7. and (4) estimating the micro morphology of the anodized sample after the anodic oxidation treatment through the time-current curve, the time-pH curve and the time-peak frequency curve obtained in the third step.
In the sixth step of this example, when the pH value of the system is maintained at 7.85 ± 0.1 during the anodization test, the current curve decreases to 0.08 ± 0.01A in the first 20s of the anodization test and then slightly increases to 0.1 to 0.12A, the acoustic activity level in the first 80s of the anodization test in the time-peak frequency curve is higher than that in the later period of the test, and more than 90% of data points of the frequency peak in the first 80s of the anodization test are in the range of 0.1 to 0.3MHz, it is predicted that a regular nanotube array microstructure is formed on the surface of the anodized sample 9.
The test summary shows that when a relatively regular nanotube microstructure is obtained in the anodic oxidation process, the acoustic activity level is relatively high in the early stage and the middle stage of anodic oxidation, and the frequency peak is probably in the range of 0.1-0.3 MHz. In experiments that did not produce a regular nanotube array microstructure, the high level of acoustic activity was more likely to occur in the mid-late stage of anodization, and the frequency peaks correspond to lower than in the case of regular nanotube array structures.
Claims (9)
1. The system for detecting the metal anodic oxidation behavior based on the external sound wave emission signal is characterized by comprising a potentiostat (1), a current data acquisition device (2), an acoustic emission signal acquisition device (3), a pH detector (4) and a high-speed camera display device (5), wherein an anodic oxidation sample (9) and a Pt electrode (8) are placed in an electrolytic cell, electrolyte is filled in the electrolytic cell, the anode of the potentiostat (1) is connected with the anodic oxidation sample (9), the cathode of the potentiostat (1) is connected with the Pt electrode (8), the potentiostat (1) is connected with the current data acquisition device (2), the back of the anodic oxidation sample is connected with an acoustic sensor (6), the acoustic sensor (6) is connected with the acoustic emission signal acquisition device (3), the high-speed camera display device (5) is connected with a mobile high-speed camera (7), and the mobile high-speed camera (7) extends into the electrolytic cell and detects the bubble generation and growth conditions of the anodic oxidation sample.
2. The system for detecting the anodic oxidation behaviour of metals based on an applied acoustic emission signal according to claim 1, characterised in that the acoustic peak frequency signal is acquired by means of an acoustic sensor (6).
3. The method for detecting the metal anodic oxidation behavior based on the external sound wave emission signal is characterized by being realized according to the following steps:
1. electrolyte is filled into an electrolytic cell, the anode of a constant potential rectifier (1) is connected with an anodic oxidation sample (9), the cathode of the constant potential rectifier (1) is connected with a Pt electrode (8), an acoustic sensor (6) is arranged on the back of the anodic oxidation sample, and the acoustic sensor (6) is used for detecting the acoustic characteristics of the electrolyte;
2. starting a constant potential rectifier (1) to carry out an anodic oxidation test, and collecting acoustics, current signals and the pH of a system through an acoustic emission signal collection device (3), a current data collection device (2) and a pH detector (4) when micro bubbles are observed to be generated on the surface of an anodic oxidation sample (9) in the anodic oxidation test;
3. drawing a time-current curve by taking the reaction time as an abscissa and the current data as an ordinate; drawing a time-pH curve by taking the reaction time as an abscissa and the pH as an ordinate; drawing a time-peak frequency curve by taking the reaction time as an abscissa and the peak frequency of the acoustic signal as an ordinate;
4. and (4) estimating the micro morphology of the anodized sample after anodic oxidation treatment by using the time-current curve, the time-pH curve and the time-peak frequency curve obtained in the third step.
4. The method for detecting anodic oxidation behavior of metals based on applied acoustic emission signals according to claim 3, characterized in that in step one, the anodic oxidation sample (9) is first subjected to ultrasonic cleaning treatment with acetone and alcohol-free ethanol solution.
5. The method for detecting anodic oxidation behavior of metals based on applied acoustic emission signals according to claim 3, characterized in that the anodic oxidation samples (9) in step one are iron-based materials, titanium-based materials, zinc-based materials or aluminum-based materials.
6. The method according to claim 3, wherein the electrolyte in the first step is a glycol solution containing 0.3-0.8 wt% NH 4 F。
7. The method for detecting the anodic oxidation behavior of a metal based on an applied acoustic emission signal according to claim 3, wherein the anodic oxidation voltage is controlled to be 40V to 90V in the step two anodic oxidation test, and the treatment time is controlled to be 1min to 5min.
8. The method for detecting the anodic oxidation behavior of a metal based on an applied acoustic emission signal according to claim 3, wherein in the fourth step, when the pH value of the system is maintained at 7.85 ± 0.1 during the anodic oxidation test, the current curve is slightly increased to 0.1-0.12A after the current curve is decreased to 0.08 ± 0.01A in the first 20s of the anodic oxidation test, the acoustic activity level in the first 80s of the anodic oxidation test in the time-peak frequency curve is higher than that in the later period of the test, and more than 90% of data points of the frequency peak in the first 80s of the anodic oxidation test are in the range of 0.1-0.3MHz, the surface of the anodic oxidation sample (9) is predicted to form a regular nanotube array microstructure.
9. The method of claim 8, wherein the time-current curve of the step four is characterized in that after 20s of the anodization test, the current rises steadily and remains below 0.15A.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210877330.3A CN115290748B (en) | 2022-07-25 | 2022-07-25 | System and method for detecting metal anodic oxidation behavior based on external acoustic wave emission signal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210877330.3A CN115290748B (en) | 2022-07-25 | 2022-07-25 | System and method for detecting metal anodic oxidation behavior based on external acoustic wave emission signal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115290748A true CN115290748A (en) | 2022-11-04 |
| CN115290748B CN115290748B (en) | 2024-06-21 |
Family
ID=83824148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210877330.3A Active CN115290748B (en) | 2022-07-25 | 2022-07-25 | System and method for detecting metal anodic oxidation behavior based on external acoustic wave emission signal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115290748B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006017741A (en) * | 2000-11-17 | 2006-01-19 | Amikku:Kk | Acoustic diagnosing using pulse electromagnetic force and measuring apparatus and its diagnosing and measuring method |
| CN102288536A (en) * | 2011-07-01 | 2011-12-21 | 中国科学院金属研究所 | Electrochemical corrosion testing device for realizing multiple types of in-situ monitoring |
| CN103123314A (en) * | 2012-12-19 | 2013-05-29 | 中国原子能科学研究院 | Stress corrosion monitoring system |
| CN111366487A (en) * | 2020-03-31 | 2020-07-03 | 北京科技大学 | Probe for monitoring stress corrosion cracking and monitoring and predicting method |
| CN112782256A (en) * | 2019-11-06 | 2021-05-11 | 中国石油化工股份有限公司 | Multi-parameter probe for corrosion monitoring and corrosion detection system |
| CN115235877A (en) * | 2021-04-23 | 2022-10-25 | 中国石油化工股份有限公司 | Corrosion state monitoring system and stress corrosion state evaluation method and device |
-
2022
- 2022-07-25 CN CN202210877330.3A patent/CN115290748B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006017741A (en) * | 2000-11-17 | 2006-01-19 | Amikku:Kk | Acoustic diagnosing using pulse electromagnetic force and measuring apparatus and its diagnosing and measuring method |
| CN102288536A (en) * | 2011-07-01 | 2011-12-21 | 中国科学院金属研究所 | Electrochemical corrosion testing device for realizing multiple types of in-situ monitoring |
| CN103123314A (en) * | 2012-12-19 | 2013-05-29 | 中国原子能科学研究院 | Stress corrosion monitoring system |
| CN112782256A (en) * | 2019-11-06 | 2021-05-11 | 中国石油化工股份有限公司 | Multi-parameter probe for corrosion monitoring and corrosion detection system |
| CN111366487A (en) * | 2020-03-31 | 2020-07-03 | 北京科技大学 | Probe for monitoring stress corrosion cracking and monitoring and predicting method |
| CN115235877A (en) * | 2021-04-23 | 2022-10-25 | 中国石油化工股份有限公司 | Corrosion state monitoring system and stress corrosion state evaluation method and device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115290748B (en) | 2024-06-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Macpherson et al. | Combined scanning electrochemical− atomic force microscopy | |
| CN105297107B (en) | A kind of method of cyclic voltammetric electrodeposited nanocrystalline platinum nickel/titanium dioxide nanotube electrode | |
| Edwards et al. | Nanoscale electrochemical kinetics & dynamics: the challenges and opportunities of single-entity measurements | |
| CN102249183B (en) | CuO/TiO2 nanotube array and preparation method and application method thereof | |
| Hao et al. | Nanopipette-based electroplated nanoelectrodes | |
| Han et al. | Single molecular catalysis of a redox enzyme on nanoelectrodes | |
| Defnet et al. | Temporally-resolved ultrafast hydrogen adsorption and evolution on single platinum nanoparticles | |
| CN200953007Y (en) | Non-damage micrometering system utilizing multielectrode measurement | |
| CN1945300A (en) | Electrochemical supermicro electrode combining method and its super micro combined electrode and preparing process | |
| CN106119750A (en) | Laser-impact and differential arc oxidation are combined in Mg alloy surface and prepare biological coating method | |
| Li et al. | Correlating corrosion to surface grain orientations of polycrystalline aluminum alloy by scanning electrochemical cell microscopy | |
| Orlikowski et al. | Instantaneous impedance monitoring of aluminum alloy 7075 corrosion in borate buffer with admixed chloride ions | |
| Vieira et al. | Nanoimpact Electrochemistry to Quantify the Transformation and Electrocatalytic Activity of Ni (OH) 2 Nanoparticles: Toward the Size–Activity Relationship at High Throughput | |
| Li et al. | Controlling surface contact, oxygen transport, and pitting of surface oxide via single-channel scanning electrochemical cell microscopy | |
| CN115290748B (en) | System and method for detecting metal anodic oxidation behavior based on external acoustic wave emission signal | |
| CN110331427A (en) | A kind of porous silicon-silver nanoparticle pine-tree structure and preparation method thereof | |
| Liao et al. | Magnetic field effects on electrochemical dissolution behavior and surface quality of electrochemical machining of Ti-48Al-2Cr-2Nb alloy | |
| CN101303325A (en) | Method for preparing platinum nanometer perforated electrodes with electrodeposition | |
| Legerstee et al. | Scanning probe microscopy facility for operando study of redox processes on lithium ion battery electrodes | |
| CN108754580B (en) | The surface modified stainless steel of in-situ deposition nanometer pt a kind of and its application | |
| CN111999357A (en) | Preparation method of nano silver wire array sensor and application of nano silver wire array sensor in ascorbic acid biomolecule determination | |
| Zhu et al. | Nonenzymatic glucose sensor based on Pt-Au-SWCNTs nanocomposites | |
| CN107703203A (en) | A kind of heavy metal analysis device and its detection method | |
| Yang et al. | Direct determination of uric acid in human serum samples using polypyrrole nanoelectrode ensembles | |
| CN112795963B (en) | Method for simply and rapidly preparing ultramicro electrode array |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |