CN115200518B - 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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CN115200518B
CN115200518B CN202210659495.3A CN202210659495A CN115200518B CN 115200518 B CN115200518 B CN 115200518B CN 202210659495 A CN202210659495 A CN 202210659495A CN 115200518 B CN115200518 B CN 115200518B
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anode
coating
thickness
titanium anode
uniformity
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CN115200518A (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 Xinneng 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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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a method for detecting the thickness and visualizing the uniformity of a titanium anode coating, which is characterized by comprising the following steps: s1: cleaning the titanium anode to be detected, and keeping the titanium anode to be detected on a dry surface; s2: testing the anode processed in the step S1 by using a handheld XRF, and measuring the anode at fixed points at fixed distances in the transverse and longitudinal directions respectively; s3: and (2) 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 map, so that the distribution condition of the thickness of the coating on the whole anode surface can be intuitively judged. The method for conveniently detecting the thickness and visualizing the uniformity of the titanium anode coating provided by the invention has the advantages that the information of the anode surface coating is rapidly obtained, the production is timely fed back, and the product quality is ensured; technicians can conduct 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 convenient titanium anode coating thickness detection and uniformity visualization method.
Background
In the production process of the electrolytic copper foil, the coating thickness of the titanium anode can directly influence the distribution of the power lines, and the more uniform the thickness is, the more uniform the current density distribution is, and the more uniform the cathode copper foil grows. It is therefore important to determine whether the distribution is uniform based on the coating thickness at a large number of test points, whether in the study of product inspection or failure analysis.
Common coating thickness measuring methods include weighing method, scanning electron microscope, metallographic microscope, chemical dissolution method, X-ray diffraction method, etc. The weighing method is used for estimating 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 during the early sample preparation by an electron microscope and a microscope method, the sample preparation is difficult, and the method is not suitable for large-batch data point test; with the development of modern analysis technology, an in-situ, nondestructive and convenient handheld type X-ray fluorescence spectrometer is already proposed, but is not applied in 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 convenient titanium anode coating thickness detection and uniformity visualization method, which can rapidly obtain anode surface coating information, timely feed back production and ensure product quality. In addition, technicians can conduct nondestructive analysis and research on the failed anode, process technology is improved timely, and product competitiveness is improved.
The technical scheme adopted for solving the technical problems is as follows: a method for conveniently detecting the thickness and visualizing the uniformity of a titanium anode coating comprises the following steps:
s1: cleaning the titanium anode to be detected, and keeping the titanium anode to be detected on a dry surface;
s2: testing the anode processed in the step S1 by using a handheld XRF, and measuring the anode at fixed points at fixed distances in the transverse and longitudinal directions respectively;
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 map.
Further, the titanium anode to be detected in the step S1 may be a finished product with a clean surface, or may be a spent titanium anode with a surface scale.
Further, the cleaning process in step S1 is directed to a surface-scaled spent titanium anode; the specific treatment method is that a chemical method is adopted to remove scale, and the spent titanium anode is soaked in an acidic or alkaline solution for a certain time, wherein the acidic solution can be hydrochloric acid or acetic acid, and the alkaline solution can be sodium hydroxide solution or sodium carbonate solution.
Further, the handheld XRF test 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: under the conditions that the analysis voltage is 40kV, the analysis current is 8uA, and the test time is 60s, carrying out spectrogram scanning on a standard sample, and adopting TiKa, irKa, taKa as an analysis line;
s23: regression is carried out on the test results of the standard samples according to a regression equation, and a regression correction curve is obtained; the regression equation is:
Figure BDA0003689941180000021
wherein C is i For measuring the content of the element C j A as the content of the interfering element ij To absorb the influence coefficient, R i To correct the absorption coefficient.
Further, in the step S2, the fixed-point measurement is numbered from left to right and from top to bottom at one side of the longitudinal end of the anode, and 30 to 60 measurement points are selected for each piece according to different specification sizes.
Further, in the step S3, the software used may be matlab, python or origin.
Further, in the step S3, the matrix performs spline curve interpolation operation first, and then a polynominal 2D function is selected for fitting to obtain a coating thickness function; finally, drawing a coating thickness contour line pattern on the surface of the anode plate by using a contourf function, so that the distribution condition of the coating thickness on the surface of the whole anode can be visually displayed; 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 beneficial effects of the invention are as follows: 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, single-point property, hysteresis and the like of the traditional detection are solved.
(2) According to the method, a large number of cloud data points are fitted to the contour patterns of the coating thickness on the surface of the whole anode plate, so that the requirements of visually judging whether the coating distribution is uniform and whether the product quality meets the standard are met, and the yield and the inspection efficiency are greatly increased.
(3) Specific coating systems can be established in a targeted way, and accuracy of results is guaranteed. Not only can control the product quality in the production process, but also can provide guiding opinion in the research of later failure analysis.
Drawings
FIG. 1 is a regression calibration curve of a standard sample according to the present invention.
FIG. 2 is a plot of the coating thickness as a function of the coating thickness obtained in example 1.
FIG. 3 is a contour plot of the coating thickness in example 1.
FIG. 4 is a plot of the coating thickness as a function of the coating thickness obtained in example 2.
Fig. 5 is a contour pattern of the coating thickness in example 2.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are merely illustrative of the invention and are not intended to limit the scope of the invention.
Example 1
A method for conveniently detecting the thickness and visualizing the uniformity of a titanium anode coating comprises the following steps:
s1: maintaining 1450 x 319 x 1mm of finished titanium anode on a dry surface;
s2: testing the anode processed in the step S1 by using an Ir-Ta/Ti method in handheld XRF, and selecting 40 test points in total in the transverse and longitudinal directions;
s3: and (2) storing the data obtained in the step (S2) as a matrix, firstly performing spline curve interpolation operation, and then selecting a polynominal 2D function for fitting to obtain a coating thickness function, as shown in FIG. 2. Finally, a contour pattern of the coating thickness on the anode plate surface is plotted using a contourf function, as shown in fig. 3. The thickness distribution of the surface coating of the finished titanium anode is uniform, and the finished titanium anode is a qualified product.
Figure BDA0003689941180000041
Example 2
A method for conveniently detecting the thickness and visualizing the uniformity of a titanium anode coating comprises the following steps:
s1: soaking 1510 x 253 x 6mm of reworked titanium anode in 2mol/L NaOH (aq) for 24 hours, washing and airing;
s2: testing the anode processed in the step S1 by using an Ir-Ta/Ti method in handheld XRF, and selecting 40 test points in total in the transverse and longitudinal directions;
s3: and (2) storing the data obtained in the step (S2) as a matrix, firstly performing spline curve interpolation operation, and then selecting a polynominal 2D function for fitting to obtain a coating thickness function, as shown in FIG. 4. Finally, a contour pattern of the coating thickness on the anode plate surface is plotted using a contourf function, as shown in fig. 5. The thickness distribution of the surface coating of the reworked titanium anode is extremely uneven, the range is wider, the edge loss is serious, the qualified copper foil cannot be continuously produced, and the failure is judged.
Figure BDA0003689941180000051
The above embodiments are only for illustrating the present invention, not for limiting the present invention, and various changes and modifications may be made by one of ordinary skill in the relevant art without departing from the spirit and scope of the present invention, and therefore, all equivalent technical solutions are also within the scope of the present invention, and the scope of the present invention is defined by the claims.

Claims (5)

1. A method for conveniently detecting the thickness and visualizing the uniformity of a titanium anode coating is characterized by comprising the following steps:
s1: cleaning the titanium anode to be detected, and keeping the titanium anode to be detected on a dry surface;
s2: testing the anode processed in the step S1 by using a handheld XRF, and measuring the anode at fixed points at fixed distances in the transverse and longitudinal directions respectively;
s3: 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 map, so that the distribution condition of the thickness of the coating on the whole anode surface can be intuitively judged;
the handheld XRF testing method in the step S2 is an Ir-Ta/Ti standard curve obtained through an empirical coefficient method; 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: under the conditions that the analysis voltage is 40kV, the analysis current is 8uA, and the test time is 60s, carrying out spectrogram scanning on a standard sample, and adopting TiKa, irKa, taKa as an analysis line;
s23: regression is carried out on the test results of the standard samples according to a regression equation, and a regression correction curve is obtained; the regression equation is:
Figure FDA0004065509030000011
wherein C is i For measuring the content of the element C j A as the content of the interfering element ij To absorb the influence coefficient, R i To correct the absorption coefficient;
in the step S3, the matrix firstly carries out spline curve interpolation operation, and then a polynominal 2D function is selected for fitting to obtain a coating thickness function; finally, drawing a coating thickness contour line pattern on the surface of the anode plate by using a contourf function, so that the distribution condition of the coating thickness on the surface of the whole anode can be visually displayed; 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 。
2. the method for detecting the thickness and visualizing the uniformity of the titanium anode coating convenient to use according to claim 1, wherein the method comprises the following steps: the titanium anode to be detected in the step S1 can be a finished product with a clean surface, and can also be a failure titanium anode with a scaled surface.
3. A method for detecting the thickness and visualizing the uniformity of a titanium anode coating convenient to use according to claim 1 or 2, which is characterized in that: the cleaning treatment in the step S1 is to a failure titanium anode with surface scaling; the specific treatment method is that a chemical method is adopted to remove scale, and the spent titanium anode is soaked in an acidic or alkaline solution for a certain time, wherein the acidic solution can be hydrochloric acid or acetic acid, and the alkaline solution can be sodium hydroxide solution or sodium carbonate solution.
4. The method for detecting the thickness and visualizing the uniformity of the titanium anode coating convenient to use according to claim 1, wherein the method comprises the following steps: in the step S2, the fixed-point measurement is numbered from left to right and from top to bottom at one side of the longitudinal end of the anode, and 30 to 60 measurement points are selected for each piece according to different specification sizes.
5. The method for detecting the thickness and visualizing the uniformity of the titanium anode coating convenient to use according to claim 1, wherein the method comprises the following steps: in the step S3, the software used may be matlab, python or origin.
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