CN115200518A - Convenient titanium anode coating thickness detection and uniformity visualization method - Google Patents

Convenient titanium anode coating thickness detection and uniformity visualization method Download PDF

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CN115200518A
CN115200518A CN202210659495.3A CN202210659495A CN115200518A CN 115200518 A CN115200518 A CN 115200518A CN 202210659495 A CN202210659495 A CN 202210659495A CN 115200518 A CN115200518 A CN 115200518A
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thickness
coating
titanium anode
anode
uniformity
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CN115200518B (en
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白璐怡
冯庆
杨瑞锋
王小龙
郝小军
柴作强
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Xian Taijin Industrial Electrochemical Technology Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
    • G01B15/02—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons for measuring thickness
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • C23G1/106—Other heavy metals refractory metals
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/20—Other heavy metals
    • C23G1/205—Other heavy metals refractory metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a convenient titanium anode coating thickness detection and uniformity visualization method, which is characterized by comprising the following steps of: s1: cleaning the titanium anode to be detected, and keeping the titanium anode dry; s2: testing the anode processed in the step S1 by using a handheld XRF, and measuring the anode at fixed intervals and fixed points in the transverse and longitudinal directions; s3: and (3) storing the data obtained in the step (S2) as a matrix, performing interpolation fitting on the data by using software, and then drawing a 3D contour diagram, wherein the distribution condition of the coating thickness of the whole anode surface can be visually judged. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating rapidly obtains the information of the anode surface coating, feeds back production in time and ensures the product quality; technicians can perform nondestructive analysis and research on the failed anode, timely improve the process technology and improve the product competitiveness.

Description

Convenient titanium anode coating thickness detection and uniformity visualization method
Technical Field
The invention relates to the technical field of titanium anode coating thickness detection, in particular to a method for conveniently detecting the titanium anode coating thickness and visualizing the uniformity of the titanium anode coating thickness.
Background
In the production process of the electrolytic copper foil, the thickness of the coating of the titanium anode can directly influence the distribution of electric lines, and the more uniform the thickness of the coating, the more uniform the current density distribution, and the more uniform the growth of the cathode copper foil. Therefore, whether the distribution is uniform or not is judged according to the coating thickness of a large number of test points in the finished product inspection or failure analysis research.
Common coating thickness measuring methods include a weighing method, a scanning electron microscope, a metallographic microscope, a chemical dissolution method, an X-ray diffraction method and the like. The weighing method is to estimate the average thickness of the coating, the accuracy is not high, and the uniformity of distribution cannot be judged; the surface coating is easy to collapse and difficult to prepare samples by electron microscope and microscope methods in the early stage, and is also not suitable for large-scale data point tests; with the development of modern analysis technology, an in-situ, nondestructive and convenient handheld type spectrometer is provided, but the spectrometer is not applied to the field due to the complexity of a titanium anode coating system.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for conveniently detecting the thickness of a titanium anode coating and visualizing the uniformity of the titanium anode coating, so that the information of the anode surface coating is quickly obtained, the production is fed back in time, and the product quality is ensured. In addition, technicians can perform nondestructive analysis and research on the failed anode, timely improve the process technology and improve the product competitiveness.
The technical scheme adopted by the invention for solving the technical problem is as follows: a convenient titanium anode coating thickness detection and uniformity visualization method comprises the following steps:
s1: cleaning the titanium anode to be detected, and keeping the titanium anode dry;
s2: testing the anode processed in the step S1 by using a handheld XRF, and measuring the anode at fixed intervals and fixed points in the transverse and longitudinal directions;
s3: and (3) storing the data obtained in the step (S2) as a matrix, performing interpolation fitting on the data by using software, and then drawing a 3D contour diagram.
Further, the titanium anode to be detected in step S1 may be a finished product with a clean surface, or may be a failed titanium anode with a scaled surface.
Further, the cleaning treatment in step S1 is a failed titanium anode for surface fouling; the specific treatment method is that a chemical method is adopted to remove scale, and the failed titanium anode is soaked in an acidic or alkaline solution for a certain time, wherein the acidic solution can be hydrochloric acid and acetic acid, and the alkaline solution can be a sodium hydroxide solution and a sodium carbonate solution.
Further, the handheld XRF testing method in the step S2 is an Ir-Ta/Ti standard curve obtained by an empirical coefficient method.
Further, the establishment of the Ir-Ta/Ti standard curve comprises the following steps:
s21: preparing a series of standard substances with different coating thicknesses;
s22: performing spectrogram scanning on a standard sample under the conditions that the analysis voltage is 40kV, the analysis current is 8uA, and the test time is 60s, and adopting TiKa, irKa and TaKa as analysis lines;
s23: the test result of each standard sample is regressed according to a regression equation to obtain a regression correction curve; the regression equation is:
Figure BDA0003689941180000021
wherein, C i To be measured for the element content, C j As content of interfering elements, a ij For absorption coefficient of influence, R i To correct the absorption coefficient.
Further, in the step S2, the distance fixed point measurement is performed by numbering from left to right and from top to bottom on the side of the longitudinal end of the anode, and 30 to 60 measurement points are selected for each piece according to different specifications and sizes.
Further, in the step S3, the software used may be matlab, python or origin.
Further, in the step S3, the matrix first performs spline interpolation operation, and then selects a polymonomial 2D function for fitting to obtain a coating thickness function; finally, drawing a contour line graph of the coating thickness of the surface of the anode plate by using a contourf function, and visually displaying the distribution condition of the coating thickness of the whole anode surface; the coating thickness function is: z = Z 0 +A 1 x+A 2 x 2 +A 3 x 3 +B 1 y+B 2 y 2 +B 3 y 3 。
The invention has the beneficial effects that: compared with the prior art, the convenient titanium anode coating thickness detection and uniformity visualization method provided by the invention has the following advantages:
(1) The problems of destructiveness, singleness, hysteresis and the like of the traditional detection are solved.
(2) The contour line graph of the coating thickness of the whole anode plate surface is fitted according to a large number of cloud data points, the requirements of visually judging whether the coating is uniformly distributed and whether the product quality reaches the standard are met, and the yield and the inspection efficiency are greatly increased.
(3) The method can be used for establishing a specific coating system in a targeted way, and the accuracy of the result is ensured. Not only can control the product quality in the production process, but also can provide guiding opinions in the research of later failure analysis.
Drawings
FIG. 1 is a regression calibration curve of a standard sample in the present invention.
FIG. 2 is a function of the coating thickness obtained in example 1.
FIG. 3 is a plot of the thickness contour of the coating in example 1.
FIG. 4 is a function of the coating thickness obtained in example 2.
FIG. 5 is a plot of the thickness contours of the coatings of example 2.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
A method for conveniently detecting the thickness of a titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating comprises the following steps:
s1: maintaining 1450 x 319 x 1mm finished titanium anode dry surface;
s2: testing the anode processed in the step S1 by using an Ir-Ta/Ti method in a handheld XRF, and selecting 40 test points in total in the transverse and longitudinal directions;
s3: and (3) storing the data obtained in the step (S2) as a matrix, firstly performing spline interpolation operation, and then selecting a polymonomial 2D function for fitting to obtain a coating thickness function, as shown in figure 2. Finally, the contour of the coating thickness on the surface of the anode plate was plotted using the contourf function, as shown in FIG. 3. The coating thickness distribution of the finished product titanium anode surface coating is uniform, and the finished product titanium anode is a qualified product.
Figure BDA0003689941180000041
Example 2
A convenient titanium anode coating thickness detection and uniformity visualization method comprises the following steps:
s1: soaking 1510 x 253 x 6mm reworked titanium anodes in 2mol/L NaOH (aq) for 24h, washing and airing;
s2: testing the anode processed in the step S1 by using an Ir-Ta/Ti method in a handheld XRF, and selecting 40 test points in total in the transverse and longitudinal directions;
s3: and (3) storing the data obtained in the step (S2) as a matrix, firstly performing spline interpolation operation, and then selecting a polymonomial 2D function for fitting to obtain a coating thickness function, as shown in figure 4. Finally, the contour of the coating thickness on the surface of the anode plate was plotted using the contourf function, as shown in FIG. 5. It can be seen that the coating thickness distribution of the repaired titanium anode surface is extremely uneven, the range is wide, the edge loss is serious, qualified copper foil cannot be continuously produced, and failure is judged.
Figure BDA0003689941180000051
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.

Claims (8)

1. A convenient titanium anode coating thickness detection and uniformity visualization method is characterized by comprising the following steps:
s1: cleaning the titanium anode to be detected, and keeping the titanium anode on the dry surface;
s2: testing the anode processed in the step S1 by using a handheld XRF, and measuring the anode at fixed intervals and fixed points in the transverse and longitudinal directions;
s3: and (3) storing the data obtained in the step (S2) as a matrix, performing interpolation fitting on the data by using software, and then drawing a 3D contour diagram, wherein the distribution condition of the coating thickness of the whole anode surface can be visually judged.
2. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating as claimed in claim 1, wherein the method comprises the following steps: the titanium anode to be detected in the step S1 may be a finished product with a clean surface, or may be a failed titanium anode with a scale formed on the surface.
3. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating as claimed in claim 1 or 2, wherein the method comprises the following steps: the cleaning treatment in the step S1 is to deal with the failed titanium anode with surface scaling; the specific treatment method is that a chemical method is adopted for descaling, and the failed titanium anode is soaked in an acidic or alkaline solution for a certain time, wherein the acidic solution can be hydrochloric acid and acetic acid, and the alkaline solution can be a sodium hydroxide solution and a sodium carbonate solution.
4. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating as claimed in claim 1, wherein the method comprises the following steps: the handheld XRF testing method in the step S2 is an Ir-Ta/Ti standard curve obtained by an empirical coefficient method.
5. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating as claimed in claim 4, wherein the method comprises the following steps: the establishment of the Ir-Ta/Ti standard curve comprises the following steps:
s21: preparing a series of standard substances with different coating thicknesses;
s22: performing spectrogram scanning on a standard sample under the conditions that the analysis voltage is 40kV, the analysis current is 8uA and the test time is 60s, and adopting TiKa, irKa and TaKa as analysis lines;
s23: the test result of each standard sample is regressed according to a regression equation to obtain a regression correction curve; the regression equation is:
Figure FDA0003689941170000021
wherein, C i To be measured for the element content, C j As content of interfering elements, a ij For absorption coefficient of influence, R i To correct the absorption coefficient.
6. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating as claimed in claim 1, wherein the method comprises the following steps: in the step S2, the distance fixed-point measurement is performed by numbering from left to right and from top to bottom on the side of the longitudinal end of the anode, and 30 to 60 measurement points are selected for each piece according to different specifications and sizes.
7. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness of the titanium anode coating as claimed in claim 1, wherein the method comprises the following steps: in step S3, the software used may be matlab, python, or origin.
8. The method for conveniently detecting the thickness of the titanium anode coating and visualizing the uniformity of the thickness as claimed in claim 1, wherein the method comprises the following steps: in the step S3, the matrix is firstly subjected to spline interpolation operation, and then a polymodal 2D function is selected for fitting to obtain a coating thickness function; finally, drawing a contour line graph of the coating thickness of the surface of the anode plate by using a contourf function, and visually displaying the distribution condition of the coating thickness of the whole anode surface; the coating thickness function is:
Z＝Z 0 +A 1 x+A 2 x 2 +A 3 x 3 +B 1 y+B 2 y 2 +B 3 y 3 。
CN202210659495.3A 2022-06-13 2022-06-13 Convenient titanium anode coating thickness detection and uniformity visualization method Active CN115200518B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN116516436A (en) * 2023-07-03 2023-08-01 深圳市欣茂鑫实业有限公司 Coating control method and system based on micro-arc oxidation

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Publication number Priority date Publication date Assignee Title
CN116516436A (en) * 2023-07-03 2023-08-01 深圳市欣茂鑫实业有限公司 Coating control method and system based on micro-arc oxidation
CN116516436B (en) * 2023-07-03 2023-08-29 深圳市欣茂鑫实业有限公司 Coating control method and system based on micro-arc oxidation

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