CN115372188B - 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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- 238000012360 testing method Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000010410 layer Substances 0.000 claims abstract description 36
- 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
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 238000002474 experimental method Methods 0.000 claims abstract description 13
- 230000000087 stabilizing effect Effects 0.000 claims abstract description 13
- 239000011241 protective layer Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000005336 cracking Methods 0.000 claims abstract description 7
- 238000005260 corrosion Methods 0.000 claims abstract description 6
- 230000007797 corrosion Effects 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 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 9
- 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 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000000977 initiatory effect Effects 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000003486 chemical etching Methods 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 1
- 238000010998 test method Methods 0.000 abstract description 8
- 238000003466 welding Methods 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000007619 statistical method Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 230000032798 delamination Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a scratch method-based interface strength test method for a second-generation high-temperature superconducting tape, which comprises the steps of removing a copper stabilizing layer and a silver protective layer through chemical corrosion, exposing a superconducting layer and a basal layer below the silver protective layer, adhering and fixing the high-temperature superconducting tape on a nano scratch experiment table, and enabling one surface of the exposed superconducting layer to face upwards; carrying out nano scratch experiments by using a spherical pressure head through a slope loading mode, and determining interface stripping critical loadL c Coefficient of sliding friction between superconducting coating and ram𝜇The method comprises the steps of carrying out a first treatment on the surface of the Observing the scratch morphology through a microscope, confirming the occurrence position and the expansion area of the interface cracking, and determining the average scratch cracking width of the completely peeled scratch through a statistical methodd c The method comprises the steps of carrying out a first treatment on the surface of the And calculating the interface strength according to a Laugier formula. The scratch test is convenient and quick, and directly acts on the surface of the superconducting film, welding or bonding is not needed, the influence of non-interface elastoplastic deformation is effectively avoided, the repeatability of the 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 strip testing method; more particularly, the method specifically 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 interfacial peeling often occurs between layers, so that the use of the tape is seriously affected. At present, an anvil test method is mostly adopted to test the interface strength of a superconducting strip, but because the anvil test method needs to weld or bond samples in the experimental process, non-interface elastoplastic deformation inevitably occurs in the process of soldering tin overflow and non-uniformity and loading, the measured interface strength has larger difference from the actual situation, and the test result has larger discreteness.
Disclosure of Invention
The invention provides a scratch method-based interface strength testing method for a second-generation high-temperature superconducting tape, and aims to solve the problems that interface strength data detected by current experiments are large in discreteness and have large difference from actual conditions.
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 a high-temperature superconducting tape meeting the experimental requirement;
2) Dissolving and completely removing the copper stabilizing layer on the surface of the superconducting tape through chemical corrosion to expose the silver protecting layer below the copper stabilizing layer;
3) Dissolving and removing the silver protective layer on the surface of the superconducting tape through chemical corrosion, and exposing the superconducting layer below the silver protective layer;
4) The surface of the superconducting layer exposed upwards, and the high-temperature superconducting tape is stuck and fixed to a nano scratch experiment table;
scratch position determination: 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 strip for positioning;
scratch test parameter setting: a scratch test method is selected in a control computer, a slope loading mode is selected, the required scratch length (300 microns) is set, and the peak load is set.
Scratch test:
and the control computer gives a test starting instruction, and the sample stage moves to the position where the pressure head is placed down and stays at the determined scratch position.
Starting pre-scanning, enabling the pressure head to contact the surface of the sample with a very small load (about 1 mN), starting to lightly scratch the sample through the set scratch length to determine the surface roughness of the superconducting layer and the sliding friction coefficient of the superconducting layer and the pressure head, and positioning the scratch position;
starting slope loading etching scanning, returning the sample stage to the initial position of the pressure head after the pre-scanning is completed, starting scratch test according to the set peak load and scratch length, and finally determining the interface stripping critical loadL C ；
Scanning after starting, scanning the sample on the pressure head once again with a tiny load according to a preset scratch length after finishing the etching scanning, and determining the residual scratch depth after the scratching;
and finishing scratch test, wherein the three steps are automatically finished by an indentation instrument according to condition setting.
And observing the appearance of the scratch by using a microscope, taking down a sample to be tested after the scratch test is completed, pasting the sample to be tested to a microscope sample holder, and finding the position of the scratch under the microscope. The position and depth of the interfacial cracking are further confirmed by a microscope, and a scratch cracking area at the position of complete peeling occurs.
5) Calculating the interface strength according to the Laugier formulaσ strength ：
Wherein:L c is the critical load of the device, and the device is the critical load,𝜇is the sliding friction coefficient of the superconductive layer and the pressure head;d c scratch cracking width for complete peeling;υ s poisson's ratio for the substrate.
Further, soaking the superconductive strip in silver nitrate solution for at least 5 min, taking out, 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), a mixed solution of ammonia water, hydrogen peroxide and methanol solution is used for removing the silver protective layer through chemical corrosion.
Further, the volume ratio of the ammonia water, the hydrogen peroxide and the methanol solution is (3.8-4.2) (0.8-1.2); the experiment is as follows: 380-420 ml of ammonia water, 80-120 ml of hydrogen peroxide solution and 80-120 ml of methanol solution are respectively taken for each 15cm long superconducting tape with the copper layer removed.
As shown in FIG. 6, the scratch crack initiation width after complete peelingd c Can be determined by the post-experiment interface morphology. As the superconductive layer is a film coating, defects exist, and the width of the stripping area is uneven in the scratch experiment process, so that the stripping strength calculation result has more general meaningRepresentative of the pass, in the present methodd c The equivalent average width after complete peeling occurred was used. I.e. in the completely peeled area𝛺 d𝑒l Dividing the integral by the scratch length of the superconducting coating after complete peelingL s Thereby determining the equivalent average scratch onset widthd c ：
Wherein, the liquid crystal display device comprises a liquid crystal display device,L s is the scratch length of the superconducting coating after complete stripping,𝛺 d𝑒l the area of the region where complete delamination of the superconducting coating occurs, such as the coil-drawing region in the figure.
The invention has the beneficial effects that:
the test of the interface strength of the superconducting strip by the anvil test method requires welding or bonding of samples, and non-interface elastoplastic deformation inevitably occurs in the process of loading due to solder overflow and non-uniformity, so that the measured interface strength has a large difference from the actual situation and the test result has a large discreteness.
The scratch test is convenient and quick, and directly acts on the surface of the superconducting film, welding or bonding is not needed, the influence of non-interface elastoplastic deformation is effectively avoided, and the repeatability of the test result is high; 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 peeling failure area) obtained by the scratch experiment, and other undetermined parameters are not introduced; the average scratch cracking width obtained based on statistics reduces experimental errors and data discrete degrees caused by superconducting coatings and interface random defects, the data is more universal and representative, and the interface strength data discrete degree obtained based on Laugier formula calculation is low.
Drawings
FIG. 1 is a schematic flow chart of the present invention;
FIG. 2 is a schematic diagram of the scratch test of step 4) of the present invention;
FIG. 3 is a schematic diagram of the pre-scan, the etch scan and the post-scan of step 4) of the present invention;
FIG. 4 is a schematic illustration of scratch test peak load loading in accordance with an embodiment of the present invention;
FIG. 5 is a graph of the results of a scratch microscope observation in accordance with an embodiment of the present invention;
FIG. 6 is an equivalent scratch crack initiation width of the present inventiond c A computational schematic.
Detailed Description
The invention is further illustrated by the following examples:
experimental group:
cutting out 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. The result of the scratch penetration and normal load along with the scratch distance is shown in figure 4, and the result of the three experiments can be seen to have better repeatability. The critical load distribution was 122.64mN, 122.27mN, 119.57mN; effective peel area and equivalent average scratch onset width determined according to FIG. 5d c Calculation formula, determining equivalent stripping width 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。
in addition, the critical load can be determined by experimentsL c The scratch initiation width after complete delamination can be determined by post-experimental interface morphology (integrated as the average width over the complete delamination area), and specific values are shown in table 1, with the maximum relative error being calculated based on the relative error of the average of the test data. It can be seen that the test results of this experiment have low dispersion, and the relative errors are only 1.58% and 0.66%, respectively, regardless of the critical load or the scratch depth. Further, according to the Laugier formula, the calculated interface strength still keeps smaller discreteness, and the relative error is only 1.14%.
Table 1 test results of experimental group
Control group:
the prior art currently uses the anvil test to test the interface strength of the superconductive tape, and table 2 summarizes the interface strength test results using the conventional anvil test (and the modified anvil test). Because the test standards of the data sources are inconsistent, the statistical methods are inconsistent, and 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, the maximum relative error of the test result of the method is different from that of the table 1. It can be seen that the interface strength obtained by different research teams based on anvil cell measurement has great discreteness. In contrast, the test method provided by the research has better repeatability, and further shows the superiority of the experimental method of the research.
Table 2 different research teams based on anvil test method and test result pairs of the present 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 itsApplications, 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 is only a part of embodiments of the present invention, and it should be noted that it will be apparent to those skilled in the art that several modifications and substitutions can be made without departing from the technical principles of the present invention, and these modifications and substitutions should also be considered as the protection scope of the present invention.
Claims (7)
1. The second-generation high-temperature superconducting tape interface strength testing method based on the scratch method is characterized by comprising the following steps of:
1) Cutting the second-generation high-temperature superconducting tape meeting the experimental requirement;
2) Completely removing the copper stabilizing layer on the surface of the high-temperature superconducting tape, and exposing the silver protecting layer below the copper stabilizing layer;
3) Then completely removing the silver protective layer on the surface of the high-temperature superconductive strip, exposing the superconductive layer below the silver protective layer, and preventing the superconductive layer from being damaged when the silver protective layer is removed;
4) Adhering and fixing the high-temperature superconducting tape with the copper stabilizing layer and the silver protecting layer removed on a nano scratch experiment table, and enabling the surface of the superconducting layer exposed to face upwards;
pre-scanning, determining the surface roughness of the superconducting layer and the sliding friction coefficient of the superconducting layer and the pressure head, and positioning the scratch position;
slope loading and scanning, and setting peak load; performing scratch test according to a preset peak load to determine the critical load of interface strippingL c ；
Scanning afterwards, and determining the residual scratch depth after the scratch;
observing the morphology of the scratch by a microscope, and confirming the occurrence position, the expansion range and the scratch crack initiation width of the completely peeled scratch at the interfaced c ；
d c Adopting the equivalent average width after complete stripping; i.e. in the completely peeled area𝛺 d𝑒l Dividing the integral by the scratch length of the superconducting coating after complete peelingL s Thereby determining the equivalent average scratch onset widthd c ：
Wherein:L s is the scratch length of the superconducting coating after complete stripping,𝛺 d𝑒l the area of the fully stripped region for the superconducting coating;
5) Calculating the interface strength according to the Laugier formulaσ strength ：
Wherein:L c is the critical load of the device, and the device is the critical load,𝜇is the sliding friction coefficient of the superconductive layer and the pressure head;d c scratch cracking width for complete peeling;υ s is Poisson's ratio of the second generation high temperature superconductive tape basal layer.
2. The method for testing the interfacial strength of the second-generation high-temperature superconducting tape based on the scratch method according to claim 1, wherein in the step 2) and the step 3), the copper stabilizing layer and the silver protecting layer are removed by chemical etching dissolution.
3. The method for testing the interfacial strength of the second-generation high-temperature superconducting tape based on the scratch method according to claim 2, wherein in the step 2), the copper stabilizing layer is removed by chemical etching using a silver nitrate solution.
4. The method for testing the interfacial strength of the second-generation high-temperature superconducting tape based on the scratch method according to claim 3, wherein the high-temperature superconducting tape is soaked in silver nitrate solution for at least 5 minutes, and the copper stabilizing layer which is subjected to chemical reaction is cleaned by clean water after being taken out; and repeatedly soaking and cleaning for multiple times until the copper stabilizing layer is completely removed.
5. The method for testing the interfacial strength of the second-generation high-temperature superconducting tape based on the scratch method according to claim 2, wherein in the step 3), the silver protective layer is removed by chemical corrosion by using a mixed solution of ammonia water, hydrogen peroxide and methanol solution.
6. The method for testing the interfacial strength of the second-generation high-temperature superconducting tape based on the scratch method according to claim 5, wherein the ammonia water, the hydrogen peroxide and the methanol solution are mixed according to the volume ratio of (3.8-4.2) (0.8-1.2).
7. The method for testing the interfacial strength of a second-generation high-temperature superconducting tape based on a scratch method according to claim 1, wherein the indenter is a spherical indenter.
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| 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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