A method for detecting the deoxidation property of flux for superconducting wire

Abstract

The present invention discloses a method for detecting the deoxidation property of a flux for a superconducting wire, comprising: configuring a plurality of different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentration: Each time a fixed length of WIC superconducting wire is welded, the WIC flux solution used for inlay welding is subjected to a Cu 2+ Ion composition detection obtains Cu of multiple WIC flux solutions with different colors 2+ Ion concentration results; Cu 2+ The ion concentration results in the corresponding color H + Ion consumption concentration; according to H + The color of the effective WIC flux solution is obtained by the ion consumption concentration. The present invention determines the effective H of the flux under different production conditions by calibrating the deoxidation property of the flux during the production of WIC superconducting wires. + The ion concentration can quickly and accurately characterize the deoxidation property of the flux.

Description

Technical Field

[0001] The invention relates to the technical field of welding detection, and in particular to a method for detecting the deoxidation of a flux for a superconducting wire. Background Art

[0002] NbTi / Cu superconducting wire (Wire In Channel, WIC) has the advantages of low cost and high stability of the prepared magnet. It is one of the main products of low-temperature superconducting wire and is widely used in superconducting magnets of magnetic resonance imaging (MRI) systems. WIC wire is prepared by inlay welding NbTi / Cu round wire and copper slot wire using solder. In the process, in order to obtain better surface quality, it is necessary to use flux treatment before tinning to remove the surface oxide layer, improve the fluidity and wettability of the flux, reduce the surface tension of the flux, and form a protective film after welding.

[0003] The flux used in WIC superconducting wire contains a certain amount of HCl, H ＋ Ions can destroy the oxide film on the copper surface to make the solder surface clean, which is beneficial to the wetting of the solder. At the same time, they can enhance the surface activity of the solder and the metal being soldered and reduce the surface tension of the solder. ＋ During use, the ions react with Cu to form Cu 2+ , the deoxidation property gradually decreases, the soldering effect becomes worse, the surface quality is affected, and finally it cannot be used. Therefore, the quality of the flux also determines the soldering effect. + Real-time monitoring of ion composition is extremely important.

[0004] The flux will undergo obvious color changes during use. When the flux comes into contact with copper, H + A substitution reaction occurs, replacing Cu 2+ , forming a CuCl2 melt, with Cu 2+ The ion concentration changes, forming [Cu(Cl4)] 2- and [Cu(H2O)4] 2+ Two ions, Cu 2+ Reacts with water, Cu 2+ +4H2O=[Cu(H2O)4] 2+ , the melt is blue; Cu 2+ With Cl - Reacts to form [Cu(Cl4)] 2- , the melt is yellow, and the two ions exist in the flux at the same time. 2+ The ion concentration is low, and the [Cu(H2O)4] 2+ Dominant, more blue in color, when Cu 2+ When the ion concentration is high, [Cu(Cl4)]2- Dominant, yellow in color, when the two ion concentrations are equal, the flux color is green.

[0005] Currently, the commonly used methods for detecting the acidity of solder flux are acid-base titration and automatic point titration. For the acid-base titration, the presence of two color-developing ions in the WIC superconducting wire flux will interfere with the phenolphthalein indicator, resulting in inaccurate detection. For the automatic point titration, the solder flux sample needs to be pre-treated, reagents prepared, and numerically titrated. It is not possible to draw conclusions efficiently and accurately for industrial applications and is not applicable. Summary of the invention

[0006] The embodiment of the present invention provides a method for detecting the deoxidizing property of a flux for superconducting wires, which is used to solve the problem that when using the acid-base titration method in the prior art, the presence of two color-developing ions in the flux for WIC superconducting wires will interfere with the phenolphthalein indicator, resulting in inaccurate detection, and the automatic point titration method requires the steps of pretreatment of the flux sample, reagent preparation, numerical titration, etc., and it is impossible to efficiently and accurately draw conclusions for industrial applications.

[0007] On the one hand, an embodiment of the present invention provides a method for detecting the deoxidation property of a flux for a superconducting wire, comprising:

[0008] Determine the H of the WIC flux solution that can completely remove the oxide layer on the surface of the copper slot wire sample + The ion concentration is effective H + Ion concentration;

[0009] Configure multiple different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentration;

[0010] A transparent WIC soldering flux solution is prepared to perform inlay welding of the copper slot wire and the NbTi / Cu round wire to obtain a WIC superconducting wire;

[0011] Each time a fixed length of the WIC superconducting wire is welded, the WIC flux solution used for inlay welding is subjected to a Cu treatment. 2+ Ion composition detection obtains Cu of multiple WIC flux solutions with different colors 2+ Ion concentration results;

[0012] According to the different colors of WIC flux solution Cu 2+ The ion concentration results are the H of the WIC flux solution of the corresponding color. + Ion consumption concentration;

[0013] According to the H +The ion consumption concentration gives the corresponding color of the WIC flux solution. + Ion concentration;

[0014] According to the effective H + Ion concentration and the corresponding color of the WIC flux solution + The ion concentration gives the color of the effective WIC flux solution;

[0015] The color of the effective WIC soldering flux solution is used as a standard color to perform a deoxidation test on the WIC soldering flux solution.

[0016] In a possible implementation, the configuration includes multiple different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentrations include:

[0017] A plurality of different H + Ion concentration of WIC flux solution H + Ion concentration isotropic setting.

[0018] In a possible implementation, according to the Cu content of the WIC flux solution of different colors 2+ The ion concentration results are the H of the WIC flux solution of the corresponding color. + Ion depletion concentrations include:

[0019] According to the WIC flux solution Cu 2+ Ion concentration calculation: The H displaced by the WIC flux solution in the displacement reaction + The amount of

[0020] According to the H + The amount of H of the WIC flux solution is determined by + Ion consumption concentration.

[0021] In a possible implementation, using the color of the effective WIC soldering flux solution as a standard color to perform a deoxidation test on the WIC soldering flux solution includes:

[0022] The different colors of WIC flux solutions are as described in H + The ion concentrations are arranged in order to obtain a color list;

[0023] According to the H + Ion concentration sorts the color of the effective WIC flux solution into the color list;

[0024] Determine the detected H of the WIC soldering flux solution according to the color list + Is the ion concentration lower than the H of the effective WIC flux solution? + Ion concentration.

[0025] The method for detecting the deoxidation property of a flux for a superconducting wire in the present invention has the following advantages:

[0026] The effective H of the flux under different production conditions was determined by calibrating the deoxidation performance of the flux in the production process of WIC superconducting wires of different specifications. + The ion concentration can quickly and accurately characterize the deoxidation strength of the flux, solving the complex problem of flux effectiveness detection in the production process of WIC superconducting wires. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0028] Figure 1 A schematic flow chart of a method for detecting the deoxidation performance of a soldering flux for superconducting wire provided in an embodiment of the present invention. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Figure 1 A schematic flow chart of a method for detecting the deoxidation property of a soldering flux for a superconducting wire provided in an embodiment of the present invention; an embodiment of the present invention provides a method for detecting the deoxidation property of a soldering flux for a superconducting wire, comprising:

[0031] Configure multiple different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentration;

[0032] A transparent WIC soldering flux solution is prepared to perform inlay welding of the copper slot wire and the NbTi / Cu round wire to obtain a WIC superconducting wire;

[0033] Each time a fixed length of the WIC superconducting wire is welded, the WIC flux solution used for inlay welding is subjected to a Cu treatment. 2+ Ion composition detection obtains Cu of multiple WIC flux solutions with different colors 2+ Ion concentration results;

[0034] According to the different colors of WIC flux solution Cu 2+ The ion concentration results are the H of the WIC flux solution of the corresponding color. + Ion consumption concentration;

[0035] According to the H + The ion consumption concentration gives the corresponding color of the WIC flux solution. + Ion concentration;

[0036] According to the effective H + Ion concentration and the corresponding color of the WIC flux solution + The ion concentration gives the color of the effective WIC flux solution;

[0037] The color of the effective WIC soldering flux solution is used as a standard color to perform a deoxidation test on the WIC soldering flux solution.

[0038] For example, different H + A WIC flux solution with a high ion concentration was used to treat a section of severely oxidized copper trough wire with the same length and phase at different H + The copper trough wire was immersed in a WIC flux solution with a high ion concentration for 3s to simulate the effect of the WIC flux solution on the copper trough wire.

[0039] Determine the H of the WIC flux solution that can completely remove the oxide layer on the surface of the copper slot wire sample + The ion concentration is effective H + Ion concentration.

[0040] Contains a certain amount of H + The newly prepared WIC flux solution is put into use. At this time, the flux is a transparent colorless liquid.

[0041] During the inlay welding process, the WIC flux solution was sampled for each WIC superconducting wire with a fixed distance of inlay welding to obtain different Cu 2+ Ionic concentration of WIC flux solution sample.

[0042] The collected WIC flux solution samples were subjected to Cu 2+ Ion composition detection, get the Cu corresponding to different colors of WIC flux solution2+ The ion concentration can be obtained by + ion concentration, thus obtaining the H + Ion concentration.

[0043] The effective H + The WIC flux solution with the same ion concentration is used as the standard sample. When the color of the WIC flux solution during the production process is darker than that of the standard sample, it means that the deoxidation property of the flux is not enough to meet the surface quality requirements of the WIC superconducting wire, and the WIC flux solution needs to be replaced in time.

[0044] In one possible embodiment, the H of the WIC flux solution that can completely remove the oxide layer on the surface of the copper slot wire sample is determined. + The ion concentration is effective H + Ion concentration; the configuration has multiple different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentration includes: a plurality of different H + Ion concentration of WIC flux solution H + The ion concentration is set in equal differences. The Cu content of the WIC flux solution of different colors is 2+ The ion concentration results are the H of the WIC flux solution of the corresponding color. + Ion consumption concentrations include: Cu based on the WIC flux solution 2+ Ion concentration calculation: The H displaced by the WIC flux solution in the displacement reaction + The amount of H replaced in the replacement reaction + The amount of H of the WIC flux solution is determined by + The deoxidation detection of the WIC soldering flux solution by using the color of the effective WIC soldering flux solution as the standard color comprises: + The ion concentrations are arranged in order to obtain a color list; according to the H + ion concentration, sorting the colors of the effective WIC soldering flux solution into the color list; determining the detected H of the WIC soldering flux solution according to the color list. + Is the ion concentration lower than the H of the effective WIC flux solution? + Ion concentration.

[0045] In a possible embodiment, different H2O2 mixtures such as 0.1 mol / L, 0.15 mol / L, 0.2 mol / L, 0.25 mol / L, 0.3 mol / L, 0.35 mol / L, 0.4 mol / L, 0.45 mol / L, and 0.5 mol / L were prepared respectively. + A WIC flux solution with a high ion concentration was used to take a 2.100×1.400mm copper slot wire sample with severe oxidation and place it at different H + The copper trough wire was immersed in a WIC flux solution with a high ion concentration for 3s to simulate the effect of the WIC flux solution on the copper trough wire.

[0046] Determine the WIC flux solution H that can completely remove the oxide layer on the surface of the copper slot wire sample + Ion concentration, when WIC flux solution contains H + When the ion concentration is 0.2 mol / L, the oxide layer on the surface of the copper slot wire sample can be completely removed, and the effective H + The ion concentration is 0.2mol / L.

[0047] Contains a certain amount of H + The newly prepared WIC flux solution is put into use. At this time, the WIC flux solution is a transparent colorless liquid.

[0048] During the inlay welding process, the WIC flux solution was sampled for every 10,000 meters of WIC superconducting wire welded to obtain different Cu 2+ Ionic concentration of WIC flux solution sample.

[0049] The collected WIC flux solution samples were subjected to Cu 2+ Ion composition detection to obtain the Cu corresponding to different colors of WIC flux solution 2+ The ion concentration can be obtained by + Ion concentration, thus obtaining WIC flux solution H + Ion concentration. For a 2.000×1.300mm WIC wire (using a 2.100×1.400mm copper slot wire), when the inlay welding is 180,000 meters, the H in the WIC flux solution sample is + The ion concentration is 0.213 mol / L. The sample is 2.000×1.300 mm WIC wire with effective H + Ionic concentration WIC flux solution standard.

[0050] H +The WIC flux solution sample corresponding to the ion concentration of 0.213 mol / L is used as the standard sample. When the color of the WIC flux solution during the production process is darker than that of the standard sample, it means that the deoxidation property of the WIC flux solution is not enough to meet the surface quality requirements of the WIC wire and needs to be replaced in time.

[0051] In a possible embodiment, different H2O2 mixtures such as 0.1 mol / L, 0.15 mol / L, 0.2 mol / L, 0.25 mol / L, 0.3 mol / L, 0.35 mol / L, 0.4 mol / L, 0.45 mol / L, and 0.5 mol / L were prepared respectively. + A WIC flux solution with a high ion concentration was used to take a 2.900×1.600mm copper trough wire sample with severe oxidation and place it at different H + The copper trough wire was immersed in a WIC flux solution with a high ion concentration for 3s to simulate the effect of the WIC flux solution on the copper trough wire.

[0052] Determine the WIC flux solution H that can completely remove the oxide layer on the surface of the copper slot wire sample + Ion concentration, when WIC flux solution contains H + When the ion concentration is 0.25mol / L, the oxide layer on the surface of the copper slot wire sample can be completely removed, and the effective H + The ion concentration is 0.25mol / L.

[0053] Contains a certain amount of H + The newly prepared WIC flux solution is put into use. At this time, the WIC flux solution is a transparent colorless liquid.

[0054] During the inlay welding process, the WIC flux solution was sampled for every 10,000 meters of WIC superconducting wire welded to obtain different Cu 2+ Ionic concentration of WIC flux solution sample.

[0055] The collected WIC flux solution samples were subjected to Cu 2+ Ion composition detection to obtain the Cu corresponding to different colors of WIC flux solution 2+ The ion concentration can be obtained by + Ion concentration, thus obtaining WIC flux solution H + Ion concentration. For 2.800×1.500mm WIC wire (using 2.900×1.600mm copper slot wire), when the inlay welding is 160,000 meters, the H in the WIC flux solution sample is + The ion concentration is 0.258 mol / L. The sample is 2.800×1.500 mm WIC wire with effective H + Ionic concentration WIC flux solution standard.

[0056] H + The WIC flux solution sample corresponding to the ion concentration of 0.258 mol / L is used as the standard sample. When the color of the WIC flux solution during the production process is darker than that of the standard sample, it means that the deoxidation property of the WIC flux solution is not enough to meet the surface quality requirements of the WIC wire and needs to be replaced in time.

[0057] In a possible embodiment, different H2O2 mixtures such as 0.1 mol / L, 0.15 mol / L, 0.2 mol / L, 0.25 mol / L, 0.3 mol / L, 0.35 mol / L, 0.4 mol / L, 0.45 mol / L, and 0.5 mol / L were prepared respectively. + A WIC flux solution with a high ion concentration was used to take a 3.900×1.800mm copper slot wire sample with severe oxidation and place it at different H + The copper trough wire was immersed in a WIC flux solution with a high ion concentration for 3s to simulate the effect of the WIC flux solution on the copper trough wire.

[0058] Determine the WIC flux solution H that can completely remove the oxide layer on the surface of the copper slot wire sample + Ion concentration, when WIC flux solution contains H + When the ion concentration is 0.35 mol / L, the oxide layer on the surface of the copper slot wire sample can be completely removed, and the effective H + The ion concentration is 0.35mol / L.

[0059] Contains a certain amount of H + The newly prepared WIC flux solution is put into use. At this time, the WIC flux solution is a transparent colorless liquid.

[0060] During the inlay welding process, the WIC flux solution was sampled for every 10,000 meters of WIC superconducting wire welded to obtain different Cu 2+ Ionic concentration of WIC flux solution sample.

[0061] The collected WIC flux solution samples were subjected to Cu 2+ Ion composition detection to obtain the Cu corresponding to different colors of WIC flux solution 2+ The ion concentration can be obtained by + Ion concentration, thus obtaining WIC flux solution H + Ion concentration. For 3.800×1.700mm WIC wire (using 3.900×1.800mm copper slot wire), when the inlay welding is 130,000 meters, the H in the WIC flux solution sample is +The ion concentration is 0.366 mol / L. The sample is 3.800×1.700 mm WIC wire with effective H + Ionic concentration WIC flux solution standard.

[0062] H + The WIC flux solution sample corresponding to the ion concentration of 0.366 mol / L is used as the standard sample. When the color of the WIC flux solution during the production process is darker than that of the standard sample, it means that the deoxidation property of the WIC flux solution is not enough to meet the surface quality requirements of the WIC wire and needs to be replaced in time.

[0063] Although the preferred embodiments of the present invention have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention.

[0064] Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A method for detecting the deoxidation property of a flux for superconducting wire, characterized in that: include: Determine the H of the WIC flux solution that can completely remove the oxide layer on the surface of the copper slot wire sample + The ion concentration is effective H + Ion concentration; Configure multiple different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentration; A transparent WIC soldering flux solution is prepared to perform inlay welding of the copper slot wire and the NbTi / Cu round wire to obtain a WIC superconducting wire; Each time a fixed length of the WIC superconducting wire is welded, the WIC flux solution used for inlay welding is subjected to a Cu treatment. 2+ Ion composition detection obtains Cu of multiple WIC flux solutions with different colors 2+ Ion concentration results; According to the different colors of WIC flux solution Cu 2+ The ion concentration results are the H of the WIC flux solution of the corresponding color. + Ion consumption concentration; According to the H + The ion consumption concentration gives the corresponding color of the WIC flux solution. + Ion concentration; According to the effective H + Ion concentration and the corresponding color of the WIC flux solution + The ion concentration gives the color of the effective WIC flux solution; The color of the effective WIC soldering flux solution is used as a standard color to perform a deoxidation test on the WIC soldering flux solution.

2. The method for detecting the deoxidation property of a soldering flux for a superconducting wire according to claim 1, characterized in that: The configuration has multiple different H + The effective H of the WIC flux solution was obtained by immersing a corresponding number of copper oxide slot wire samples of the same length and phase in the WIC flux solution with different ion concentrations. + Ion concentrations include: A plurality of different H + Ion concentration of WIC flux solution H + Ion concentration isotropic setting.

3. A method for detecting the deoxidation property of a soldering flux for a superconducting wire according to claim 2, characterized in that: According to the different colors of WIC flux solution Cu 2+ The ion concentration results are the H of the WIC flux solution of the corresponding color. + Ion depletion concentrations include: According to the WIC flux solution Cu 2+ Ion concentration calculation: The H displaced by the WIC flux solution in the displacement reaction + The amount of According to the H replaced in the replacement reaction + The amount of H of the WIC flux solution is determined by + Ion consumption concentration.

4. The method for detecting the deoxidation property of a soldering flux for a superconducting wire according to claim 1, characterized in that: The deoxidation detection of the WIC soldering flux solution using the color of the effective WIC soldering flux solution as a standard color comprises: The different colors of WIC flux solutions are as described in H + The ion concentrations are arranged in order to obtain a color list; According to the H + Ion concentration sorts the color of the effective WIC flux solution into the color list; Determine the detected H of the WIC soldering flux solution according to the color list + Is the ion concentration lower than the H of the effective WIC flux solution? + Ion concentration.

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