CN115372188A - Second-generation high-temperature superconducting tape interface strength testing method based on scratch method - Google Patents
Second-generation high-temperature superconducting tape interface strength testing method based on scratch method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 24
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- 238000002474 experimental method Methods 0.000 claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 claims abstract description 14
- 239000010949 copper Substances 0.000 claims abstract description 14
- 239000011241 protective layer Substances 0.000 claims abstract description 14
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 10
- 238000006748 scratching Methods 0.000 claims abstract description 8
- 230000002393 scratching effect Effects 0.000 claims abstract description 8
- 230000000977 initiatory effect Effects 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000010998 test method Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
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- 229910000831 Steel Inorganic materials 0.000 claims description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 239000003381 stabilizer Substances 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000003486 chemical etching Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
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- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
- G01N3/42—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid
- G01N3/46—Investigating hardness or rebound hardness by performing impressions under a steady load by indentors, e.g. sphere, pyramid the indentors performing a scratching movement
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0058—Kind of property studied
- G01N2203/0076—Hardness, compressibility or resistance to crushing
- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
- G01N2203/0082—Indentation characteristics measured during load
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/0641—Indicating or recording means; Sensing means using optical, X-ray, ultraviolet, infrared or similar detectors
- G01N2203/0647—Image analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/06—Indicating or recording means; Sensing means
- G01N2203/067—Parameter measured for estimating the property
- G01N2203/0682—Spatial dimension, e.g. length, area, angle
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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Abstract
The invention discloses a second-generation high-temperature superconducting tape interface strength testing method based on a scratching method, which comprises the steps of removing a copper stabilizing layer and a silver protective layer through chemical corrosion, exposing a superconducting layer and a substrate layer below the silver protective layer, sticking and fixing a high-temperature superconducting tape to a nano scratching experiment table, and enabling one surface exposed out of the superconducting layer to face upwards; developing a nano scratch experiment by using a spherical pressure head through a slope loading mode, and determining the critical load of interface peelingL c Coefficient of sliding friction of superconducting coating and indenter𝜇(ii) a Observing the appearance of the scratch through a microscope, confirming the position and the expansion area of the interface crack, and determining the average crack initiation width of the completely peeled scratch through a statistical methodd c (ii) a And calculating the interface strength according to a Laugier formula. The scratch test is convenient and quick, andthe method has the advantages that the method directly acts on the surface of the superconducting film, welding or bonding is not needed, the influence of non-interface elastic-plastic deformation is effectively avoided, the repeatability of a test result is high, and the dispersion of the calculated interface strength data is low.
Description
Technical Field
The invention belongs to the technical field of superconducting materials, and particularly relates to a superconducting tape testing method; more particularly, the invention relates to a second generation high temperature superconducting tape interface strength test method based on a scratch method.
Background
The second generation high temperature superconducting tape is a typical laminated composite material, and interlayer interface stripping often occurs, which seriously influences the use of the tape. At present, the anvil measurement method is mostly adopted to test the interface strength of the superconducting strip, but because the experimental process of the anvil measurement method needs to weld or bond a sample, and because the solder overflows and is non-uniform and the loading process inevitably generates non-interface elastic-plastic deformation, the measured interface strength has larger difference with the actual situation and the test result has larger discreteness.
Disclosure of Invention
The invention provides a second-generation high-temperature superconducting tape interface strength testing method based on a scratching method, and aims to solve the problems that the interface strength data detected by the existing experiment has large discreteness and is greatly different from the actual situation.
Therefore, the invention adopts the following technical scheme:
a second-generation high-temperature superconducting tape interface strength testing method based on a scratch method comprises the following steps:
1) Cutting the high-temperature superconducting tape meeting the experimental requirement;
2) Dissolving and completely removing the copper stabilizing layer on the surface of the high-temperature superconducting tape by chemical corrosion to expose the silver protective layer below the copper stabilizing layer;
3) Dissolving and removing the silver protective layer on the surface of the high-temperature superconducting strip through chemical corrosion, and exposing the superconducting layer below the silver protective layer;
4) The surface exposed out of the superconducting layer faces upwards, and the high-temperature superconducting tape is stuck and fixed to a nano scratch experiment table;
and (3) determining the position of the scratch: positioning a scratch test position through an optical microscope carried by a nano indentation instrument, and selecting a position with a uniform surface and positioned in the middle of the superconducting tape for positioning;
and (3) setting scratch test parameters: selecting a scratch testing method in a control computer, selecting a slope loading mode, setting the required scratch length (300 micrometers), and setting the peak load.
And (3) scratch testing:
and a test starting instruction is issued by controlling the computer, and the sample table moves to the pressure head to be placed and stays at the determined scratch position.
Starting pre-scanning, enabling an indenter to contact the surface of the sample with a very small load (about 1 mN), starting to slightly scratch the sample through a set scratch length to determine the surface roughness of the superconducting layer and the sliding friction coefficient of the superconducting layer and the indenter, and positioning the scratch position;
starting slope loading and engraving scanning, after pre-scanning is finished, returning the sample stage to the initial position of a pressure head, starting a scratch test according to the set peak load and scratch length, and finally determining the critical load of interface peelingL C ；
Scanning after starting, after finishing the carving scanning, scanning the sample once again by the pressure head with a micro load according to the preset scratch length, and determining the residual scratch depth after scratching;
and finishing the scratch test, wherein the three steps are automatically finished by an indentation instrument according to condition setting.
And observing the scratch appearance by using a microscope, taking down a sample to be tested after the scratch test is finished, sticking the sample to be tested to a microscope sample holder, and finding the scratch position under the microscope. The position and depth of the interface crack were further confirmed by a microscope, and the scratch crack region where the complete peeling occurred was confirmed.
5) Calculating the interface strength according to Laugier formulaσ strength ：
Wherein:L c is the critical load of the steel wire rope,𝜇the sliding friction coefficient of the superconducting layer and the pressure head is shown; d c the scratch crack width at the complete stripping part;υ s is the poisson's ratio of the substrate.
Further, soaking the high-temperature superconducting tape in a silver nitrate solution for at least 5 minutes, taking out the high-temperature superconducting tape, and cleaning the copper stabilizing layer subjected to chemical reaction by using clear water; and repeatedly soaking and cleaning for multiple times until the copper stabilizing layer is completely removed.
Further, in the step 3), the silver protective layer is removed by chemical corrosion by using a mixed solution of ammonia water, hydrogen peroxide and a methanol solution.
Further, the ammonia water, the hydrogen peroxide and the methanol solution are mixed according to the volume ratio of (3.8-4.2) to (0.8-1.2); during the experiment: 380-420 ml, 80-120 ml and 80-120 ml of ammonia water, hydrogen peroxide and methanol solution are respectively taken for each 15cm long superconducting strip with a copper layer removed.
As shown in FIG. 6, the scratch crack width after complete peelingd c Can be determined by the interface morphology after the experiment. Because the superconducting layer is a thin film coating, the defect exists, the width of a stripping area is not uniform in the scratching experiment process, and in order to ensure that the calculation result of the stripping strength has more general representativeness, in the methodd c The equivalent average width after full peeling occurred was used. I.e. in the completely peeled-off region𝛺 d𝑒l After integration, the length of the scratch is divided by the length of the complete peeling of the superconducting coatingL s To determine the equivalent average scratch crack initiation widthd c ：
Wherein the content of the first and second substances,L s the length of the scratch after the complete peeling of the superconducting coating,𝛺 d𝑒l the area where complete peeling-off of the superconducting coating occurs, such as the circled area in the figure.
The invention has the beneficial effects that:
the experiment for testing the interface strength of the superconducting tape by the anvil measurement method needs to weld or bond a sample, and the measured interface strength has larger difference from the actual condition and the test result has larger discreteness due to the overflow and the nonuniformity of soldering tin and the inevitable non-interface elastic-plastic deformation in the loading process.
The scratch test is convenient and quick, and the scratch test directly acts on the surface of the superconducting film without welding or bonding, thereby effectively avoiding the influence of non-interface elastoplastic deformation and having high test result repeatability; the Laugier formula based on the contact theory can directly calculate the interface strength according to the experimental results (such as friction coefficient, critical load and stripping failure area) obtained by a scratch experiment, and other undetermined parameters are not introduced; the average scratch crack width obtained based on statistics reduces experimental errors and data dispersion caused by the superconducting coating and random interface defects, the data is more general and representative, and the interface intensity data obtained by calculation based on a Laugier formula has low dispersion.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a schematic diagram of the scratch test in step 4) of the present invention;
FIG. 3 is a schematic diagram of the pre-scan, scribe-scan, and post-scan of step 4) of the present invention;
FIG. 4 is a schematic view of the scratch test peak load loading according to the embodiment of the present invention;
FIG. 5 is a drawing showing the result of observation by a scratch microscope according to the embodiment of the present invention;
FIG. 6 is an equivalent scratch initiation width of the present inventiond c And calculating a schematic diagram.
Detailed Description
The invention will be further illustrated with reference to specific examples:
experimental groups:
and intercepting a second-generation high-temperature superconducting tape with the length of 15cm, removing the copper stabilizing layer and the silver protective layer through chemical corrosion, and exposing the superconducting layer. Three independent and repeated experiments are carried out on the high-temperature superconducting tape under the same condition, the scratch penetration and the normal load result along with the scratch distance are shown in figure 4, and the results of the three experiments have better repeatability. The critical load distribution is 122.64mN, 122.27mN and 119.57mN; effective peel area and equivalent average scratch initiated crack width determined according to FIG. 5d c Calculating formula, determining the equivalent stripping widths to be 30.17 respectively𝜇m、30.01𝜇m、dc=30.39𝜇m。
The material parameters required based on the method are respectively as follows:
𝜇=0.2,υ s =0.34。
furthermore, the critical load can be determined experimentallyL c The scratch crack initiation width after complete peeling can be determined by the interface morphology after experiment (average width is calculated by integration in the complete peeling area), the specific values are shown in table 1, and the maximum relative error is counted based on the relative error of the average value of the test data. It can be seen that the test result of the experiment has low dispersion degree no matter the critical load or the scratch depth, and the relative error is only 1.58% and 0.66% respectively. Further according to a Laugier formula, the calculated interface strength still keeps small discreteness, and the relative error is only 1.14%.
Table 1 test results of the experimental groups
Control group:
in the prior art, the interface strength of the superconducting tape is mostly tested by using an anvil testing method, and table 2 summarizes the interface strength test results of the conventional anvil testing method (and the improved anvil testing method). Because the test standards of all data sources are inconsistent and the statistical method is inconsistent, the maximum relative error in the table 2 is counted based on the relative error of the average value of the maximum value and the minimum value in the test data, so the maximum relative error of the test result of the method is different from that in the table 1. It can be seen that interface strengths obtained by different research teams based on an anvil measurement method have great discreteness. Compared with the prior art, the test method provided by the research has better repeatability of results, and further shows the superiority of the experimental method of the research.
TABLE 2 test result pairs of different research teams based on anvil test method and method
Table 2 data sources:
[1] van der Laan D C, Ekin J W, Clickner C C, et al. Delamination strength of YBCO coated conductors under transverse tensile stress. Superconductor Science and Technology, 2007, 20(8): 765.
[2]Majkic G, Galstyan E, Zhang Y, et al. Investigation of delamination mechanisms in IBAD-MOCVD REBCO coated conductors. IEEE transactions on applied superconductivity, 2013, 23(3): 6600205.
[3] Shin H S, Gorospe A. Characterization of transverse tensile stress response of critical current and delamination behaviour in GdBCO coated conductor tapes by anvil test. Superconductor Science and Technology, 2013, 27(2): 025001.
[4]Dai K, Guo C, Zhu J, et al. A modified method to measure delamination strength of stabilizer free REBCO coated conductor under transverse tension. Physica C: Superconductivity and its Applications, 2021, 583: 1353850.
[5]Zhang X, Sun C, Liu C, et al. A standardized measurement method and data analysis for the delamination strengths of YBCO coated conductors. Superconductor Science and Technology, 2020, 33(3): 035005.
it should be noted that the above are only some embodiments of the present invention, and it should be noted that, for those skilled in the art, many modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (7)
1. A second-generation high-temperature superconducting tape interface strength testing method based on a scratch method is characterized by comprising the following steps:
1) Cutting a second-generation high-temperature superconducting tape with the size meeting the experimental requirement;
2) Completely removing the copper stabilizing layer on the surface of the high-temperature superconducting tape, and exposing the silver protective layer below the copper stabilizing layer;
3) Completely removing the silver protective layer on the surface of the high-temperature superconducting strip, exposing the superconducting layer below the silver protective layer, and preventing the superconducting layer from being damaged when the silver protective layer is removed;
4) The high-temperature superconducting tape with the copper stabilizing layer and the silver protective layer removed is fixedly adhered to a nano scratch experiment table, and one surface exposed out of the superconducting layer faces upwards;
pre-scanning, determining the surface roughness of the superconducting layer and the sliding friction coefficient of the superconducting layer and a pressure head, and positioning the scratch position;
slope loading and scale scanning, and setting peak load; performing scratch test according to the preset peak load, and determining the critical load of interface peelingL c ；
Post-scanning to determine the residual scratch depth after scratching;
observing the appearance of the scratch by a microscope, confirming the position and the extension range of the interface crack and confirming the crack initiation width of the completely peeled scratchd c ；
5) Calculating the interface strength according to Laugier formulaσ strength ：
Wherein:L c is the critical load of the steel wire rope,𝜇the sliding friction coefficient of the superconducting layer and the pressure head is shown;d c the scratch crack width at the complete stripping part;υ s the Poisson's ratio of the second generation high temperature superconducting tape substrate layer.
2. The method for testing the interfacial strength of a second-generation high-temperature superconducting tape according to claim 1, wherein the copper stabilizer layer and the silver protective layer are removed by chemical etching in the steps 2) and 3).
3. The second generation high temperature superconducting tape interfacial strength testing method based on scratch method as claimed in claim 2, wherein in said step 2), the copper stabilizer layer is chemically etched away using silver nitrate solution.
4. The second generation high temperature superconducting tape interfacial strength test method based on the scratch method as claimed in claim 3, wherein the high temperature superconducting tape is soaked in silver nitrate solution for at least 5 minutes, and after being taken out, the copper stable layer which is chemically reacted is cleaned with clear water; and repeatedly soaking and cleaning for many times until the copper stabilizing layer is completely removed.
5. The second-generation high-temperature superconducting tape interfacial strength testing method based on the scratching method according to claim 2, wherein in the step 3), the silver protective layer is chemically etched away by using a mixed solution of ammonia, hydrogen peroxide and a methanol solution.
6. The method for testing the interfacial strength of a second-generation high-temperature superconducting tape based on the scratch method as claimed in claim 5, wherein the volume ratio of the ammonia water, the hydrogen peroxide and the methanol solution is (3.8-4.2) to (0.8-1.2).
7. The second generation high temperature superconducting tape interfacial strength testing method based on the scratching method according to claim 1, wherein the indenter is a spherical indenter.
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| CN112649360A (en) * | 2021-01-07 | 2021-04-13 | 中国民航大学 | Method for testing bonding strength of silver coating |
| CN113270235A (en) * | 2021-05-12 | 2021-08-17 | 中国科学院合肥物质科学研究院 | Method for separating superconducting phase from silver-based copper oxide superconducting material |
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