CN113720703A - Method for researching mechanism of graphene for enhancing mechanical properties of asphalt - Google Patents

Method for researching mechanism of graphene for enhancing mechanical properties of asphalt Download PDF

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CN113720703A
CN113720703A CN202111083496.XA CN202111083496A CN113720703A CN 113720703 A CN113720703 A CN 113720703A CN 202111083496 A CN202111083496 A CN 202111083496A CN 113720703 A CN113720703 A CN 113720703A
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asphalt
graphene
test
matrix
sample
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许涛
徐子航
王海森
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Nanjing Forestry University
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Nanjing Forestry University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • G01N3/18Performing tests at high or low temperatures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/24Investigating strength properties of solid materials by application of mechanical stress by applying steady shearing forces
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/28Investigating ductility, e.g. suitability of sheet metal for deep-drawing or spinning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/32Investigating strength properties of solid materials by application of mechanical stress by applying repeated or pulsating forces
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01QSCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
    • G01Q60/00Particular types of SPM [Scanning Probe Microscopy] or microscopes; Essential components thereof
    • G01Q60/24AFM [Atomic Force Microscopy] or apparatus therefor, e.g. AFM probes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0001Type of application of the stress
    • G01N2203/0003Steady
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0001Type of application of the stress
    • G01N2203/0005Repeated or cyclic
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014Type of force applied
    • G01N2203/0016Tensile or compressive
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014Type of force applied
    • G01N2203/0025Shearing
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058Kind of property studied
    • G01N2203/0069Fatigue, creep, strain-stress relations or elastic constants
    • G01N2203/0071Creep
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0058Kind of property studied
    • G01N2203/0069Fatigue, creep, strain-stress relations or elastic constants
    • G01N2203/0073Fatigue

Abstract

The invention provides a method for researching a mechanical property enhancement mechanism of asphalt by graphene, belongs to the technical field of asphalt property enhancement, solves the problem of single limitation of mechanical property enhancement behavior evaluation between graphene and asphalt in the existing evaluation method, and is beneficial to further research on the graphene modified asphalt enhancement mechanism. According to the invention, firstly, high-temperature and low-temperature mechanical properties, fatigue characteristics and direct tensile tests are carried out on No. 70 matrix asphalt and graphene modified asphalt, and then the mechanical property index changes of the No. 70 matrix asphalt and the graphene modified asphalt are researched; then, by utilizing an atomic force microscope test and an X-ray diffraction test, the changes of the surface morphology information, the micro mechanical properties and the phase structure of the No. 70 matrix asphalt and the graphene modified asphalt are analyzed, the changes of the micro and macro mechanical property indexes before and after the No. 70 matrix asphalt is added with the graphene are comprehensively analyzed, and the mechanism of enhancing the mechanical property of the asphalt by the graphene is further disclosed.

Description

Method for researching mechanism of graphene for enhancing mechanical properties of asphalt
Technical Field
The invention provides a method for researching a mechanism of enhancing the mechanical property of asphalt by graphene, and belongs to the technical field of asphalt property enhancement.
Background
Roads are always regarded as static infrastructures, certain bearing capacity of the roads is mainly utilized, and with continuous release of artificial intelligence and information intelligence, the road construction also faces a brand new development direction. The cross-world emergence of graphene breaks through the conclusion that strictly bi-level crystal materials cannot exist independently and stably, and the graphene is applied to more and more fields due to excellent and unique physical properties of light, electricity, heat, force and the like.
Graphene is a honeycomb two-dimensional crystal structure formed by a layer of carbon atoms in a close arrangement, can be regarded as an infinite aromatic molecule, and is a basic constitutional unit of carbon materials such as graphite, carbon nano tubes, fullerene and the like; the two-dimensional nano material with special structure and excellent performance is applied to civil engineering, the performance of the civil engineering material can be comprehensively improved, and the application field of the graphene material is expanded.
In recent years, some scholars find that, when carrying out structural characterization on graphene modified asphalt, the lipophilicity of styrene-butadiene-styrene copolymer modifier (SBS) is increased by graphene, so that the modifier can be more fully dispersed in the asphalt; and the graphene has certain affinity to the asphalt, can be stripped or intercalated by hot asphalt, and if the graphene can be uniformly dispersed in the asphalt, various property indexes of the asphalt can be greatly changed or even comprehensively improved.
When the microscopic aging performance of the graphene-SBS composite modified asphalt is researched, the short-term aging of the graphene-SBS composite modified asphalt is caused by the oxidation of S ═ S double bonds, and the performance is weakened by the oxidation of S ═ S and C ═ C double bonds, and the long-term aging is more serious than the short-term aging, and the relative content of C ═ C is related to the mechanical performance of the modified asphalt. The graphene has obvious influence on the external force deformation resistance and the rutting resistance of the asphalt, and the formed net-shaped stable phase state corresponds to better storage stability and macroscopic mechanical property and has stronger external force resistance; in an infrared spectrum test, the addition of the graphene increases C ═ C, which is used as a high double bond energy and is a main source of the mechanical property of an asphalt sample.
In SBS modified asphalt, a small amount of graphene is introduced to achieve a good modification effect, and the synergistic effect between the graphene and the SBS modifier is presumed to improve the service performance of the asphalt. Researches have been made on adopting graphene/Carbon Nano Tube (CNTs) hybrid materials to compound and modify asphalt, and the two materials cooperate to construct a 1D-2D hybrid structure, so that the contact area of the nano materials in the asphalt is increased, and the accumulation and aggregation of the nano materials are reduced to the maximum extent; the graphene has a hardening effect on the SBS modified asphalt, slows down the loss of elastic components of the SBS modified asphalt, improves the anti-rutting capability, improves the high-temperature performance of the SBS modified asphalt, and weakens the low-temperature tensile strength; the addition of the graphene improves the shear modulus, the bulk modulus, the ductility and the mechanical property and the pavement performance of the asphalt composite material.
In previous researches, the research on the microscopic action mechanism of uniqueness between graphene and asphalt is not enough due to the lack of fine characterization of the intercalation structure between graphene and asphalt. Therefore, based on the characteristics of the layered structure of the graphene material, the mechanical property changes of the modified asphalt in the high-temperature and low-temperature states are recorded by adopting a research mode of combining macroscopic mechanical indexes and a microscopic action mechanism, and the macroscopic mechanical angle analysis is performed on the mechanical property enhancement of the graphene modified asphalt by combining the results of a direct tensile test; and finally, obtaining the surface appearance characteristics and mechanical information of the modified asphalt through microscopic performance tests, and further researching the enhancing mechanism of the graphene on the mechanical property of the asphalt.
Disclosure of Invention
(1) Technical problem
The invention provides a research method of a mechanical property enhancement mechanism of graphene to asphalt, and solves the problems that the existing mechanical property enhancement evaluation method of graphene to asphalt is single and the mechanical property enhancement mechanism of graphene to asphalt is difficult to reveal, so that the modification effect of graphene to asphalt is improved.
(2) Technical scheme
In order to improve the single limitation of the evaluation of the mechanical property enhancement behavior of the existing graphene modified asphalt, the enhancement mechanism of the graphene modified asphalt is further researched. According to the method, firstly, from the macroscopic mechanics angle, the high-temperature and low-temperature mechanical properties of the graphene modified asphalt are tested, a tensile test is carried out on an asphalt sample at the temperature of 25 ℃, and then the enhancement principles of the high-temperature and low-temperature mechanical properties and fatigue characteristics of the graphene modified asphalt are analyzed by combining the test result of a fatigue test; from the micro-mechanics perspective, the surface appearance information of the asphalt sample and the intercalation condition inside the modified asphalt are obtained, and the structural reason for enhancing the mechanical property of the graphene modified asphalt is analyzed. The technical scheme of the invention is as follows: selecting No. 70 matrix asphalt and graphene modified asphalt with the graphene doping amount accounting for 0.4% of the mass of the asphalt to perform mechanical property enhancement mechanism research, respectively performing a dynamic shear rheological test, a bending beam creep stiffness test, a force measurement ductility test and a fatigue characteristic test on an asphalt sample, and performing a direct tensile test on a standard asphalt sample at 25 ℃ based on mechanical parameters obtained by the tests to obtain macroscopic mechanical property indexes of the No. 70 matrix asphalt sample and the graphene modified asphalt sample; then, carrying out an X-ray diffraction test and an atomic force microscope test on the two asphalt samples to obtain the surface appearance information change and the phase structure change of the asphalt samples after adding the graphene; and finally, further researching a mechanical property enhancing mechanism of the graphene modified asphalt by combining mechanical parameters and structural form changes.
(3) Advantageous effects
With the rise of nano materials in this century, more and more researchers are beginning to apply nano materials to the relatively traditional traffic industry so as to improve the road performance of asphalt. After the graphene is added, the conventional performance of the modified asphalt is generally improved, and the high-temperature performance and the anti-rutting performance of the modified asphalt are greatly improved. The dispersion degree of the graphene in the asphalt greatly influences the improvement or the weakening of the comprehensive performance of the modified asphalt, and the doping amount and the microscopic dispersion degree of the graphene are closely related to the macroscopic mechanical property of the modified asphalt. The invention provides a method for researching a mechanical reinforcing mechanism of asphalt by graphene, which adopts high and low temperature mechanical properties, fatigue characteristics and direct tensile tests to research the mechanical property index changes of No. 70 matrix asphalt and graphene modified asphalt; collecting surface morphology information and phase structure changes of No. 70 matrix asphalt and graphene modified asphalt by using an atomic force microscope test and an X-ray diffraction test; and finally, from the perspective of a microscopic graphene-asphalt intercalation structure, comparing the change of macroscopic mechanical property indexes, and further researching a mechanism for enhancing the mechanical property of the asphalt by the graphene.
Detailed Description
The invention provides a method for researching a mechanism of enhancing the mechanical property of asphalt by graphene, which comprises the following specific implementation steps:
(1) selecting No. 70 matrix asphalt and modified asphalt with the graphene doping amount of 0.4% of the asphalt mass as samples, respectively testing the high-temperature performance of the No. 70 matrix asphalt and the high-temperature performance of the graphene modified asphalt by using a dynamic shear rheometer, wherein the test starting temperature is 40 ℃, the initial recording temperature is 46 ℃, the test temperatures are 46 ℃, 52 ℃, 58 ℃, 64 ℃, 70 ℃, 76 ℃ and 82 ℃, continuous sinusoidal alternating load is applied, a strain control mode is adopted, the rotation frequency is 10rad/s, and the complex modulus (G/S) of the two asphalt samples is obtained*) Phase angle (delta) and rutting factor (G)*/sin delta), and the rut factor is used as the evaluation index of the high-temperature performance of the asphalt;
(2) preparing No. 70 matrix asphalt and graphene modified asphalt into bending beam rheological test standard samples, performing a low-temperature crack resistance test by using a bending beam rheometer, inputting constant stress for continuous loading for 240s at the temperature of-12 ℃ and-18 ℃, recording stiffness moduli and creep rates of 8.0s, 15.0s, 30.0s, 60.0s, 120.0s and 240.0s in the test process, and evaluating the low-temperature crack resistance of the two asphalt samples by using the measured creep stiffness moduli and the measured creep rates;
(3) preparing No. 70 matrix asphalt and graphene modified asphalt into a standard sample for force ductility test, testing by adopting an asphalt ductility tester, stretching the sample at a stretching speed of 5cm/min at a temperature of 5 ℃, and measuring the maximum tensile force (F) of the two asphalt samples at the time of fracturemax) Maximum elongation displacement (D) and displacement corresponding to maximum tension (D)1) Respectively calculating tensile compliance (f) and yield strain energy (E) by adopting formulas I and II;
f=Fmax/D ①
E=Fmax/D ②
(4) carrying out a multi-stress creep recovery test on No. 70 matrix asphalt and graphene modified asphalt, testing the fatigue characteristics of the asphalt by using the same dynamic shear rheometer as that in the step (1), wherein the test temperature is 70 ℃, the test time is 1.0s and the test time is 9.0s under eight stress states of 0.1kPa, 0.5kPa, 1.0kPa, 1.5kPa, 2.0kPa, 2.5kPa, 3.0kPa and 3.2kPa, ten cycles are repeated, and the initial strain value (epsilon) of the stress level (sigma) in the loading stage is recorded0) Strain value (epsilon) at the end of the loading phasec) 10 th second test end strain (. epsilon.)r) Calculating the strain increment (epsilon) of two asphalt samples in the loading stage by adopting formulas (c), (c) and (c)1) 10 th second test end Strain increase value (. epsilon.)10) Average percent recovery (% R) and non-recoverable creep compliance (J)nr);
ε1=εc0
ε10=εr0
%R=[(ε110)/ε1]×100% ⑤
Jnr=(εr0)/σ ⑥
(5) Preparing No. 70 matrix asphalt and graphene modified asphalt into a standard sample for direct tensile test, adopting a universal material testing machine to stretch the sample at a tensile rate of 5mm/min at 25 ℃ until the sample is broken, and recording the peak tensile force (F) of the asphalt sample during the test, wherein the width of the sample is a mm, the thickness of the sample is b mm, and the peak tensile force (F) of the asphalt sample ish) Obtaining stress-strain relation curves of the substrate asphalt and the graphene modified asphalt, and calculating the tensile strength (T) of the two samples by adopting a formulas);
Ts=Fh/(a×b) ⑦
(6) Performing atomic force microscope test on No. 70 matrix asphalt and graphene modified asphalt, dripping a small amount of asphalt into the center of a glass slide to prepare a sample with the length and the width of 30mm, enabling the surface of the asphalt sample to be smooth and have no obvious pits, and selecting a scanning mode as a peak force mode to perform atomic force microscope test on the asphalt sampleThe 2kHz frequency is respectively used for carrying out force curve test on the surfaces of the matrix asphalt and the graphene modified asphalt to obtain the microscopic morphology and Young modulus (E) of the sample*) Adhesion (F)adh) Comparing the difference between the matrix asphalt and the graphene modified asphalt in terms of microstructure change, and analyzing the influence of graphene on the micromechanical property of the asphalt;
(7) carrying out an X-ray diffraction test on No. 70 matrix asphalt and graphene modified asphalt, setting the scanning speed to be 5 degrees/min and the scanning range to be 5-80 degrees, analyzing the change of the micro-phase structures of two asphalt samples before and after adding graphene, comparing the diffraction peak positions, the diffraction peak intensities and the peak areas of the matrix asphalt and the graphene modified asphalt, and analyzing the influence of an intercalation structure formed by the graphene and the asphalt on the mechanical property of the asphalt;
(8) the influence of the graphene on the high-low temperature performance, the fatigue property, the tensile strength, the micro mechanical property and the micro phase structure of No. 70 matrix asphalt is comparatively analyzed, the reinforcing effect of the graphene on the No. 70 matrix asphalt is comprehensively researched, and the reinforcing mechanism of the graphene on the mechanical property of the asphalt is disclosed.

Claims (1)

1. A method for researching a mechanism of enhancing the mechanical property of asphalt by graphene is characterized by comprising the following specific steps:
(1) selecting No. 70 matrix asphalt and modified asphalt with the graphene doping amount of 0.4% of the asphalt mass as samples, respectively testing the high-temperature performance of the No. 70 matrix asphalt and the high-temperature performance of the graphene modified asphalt by using a dynamic shear rheometer, wherein the test starting temperature is 40 ℃, the initial recording temperature is 46 ℃, the test temperatures are 46 ℃, 52 ℃, 58 ℃, 64 ℃, 70 ℃, 76 ℃ and 82 ℃, continuous sinusoidal alternating load is applied, a strain control mode is adopted, the rotation frequency is 10rad/s, and the complex modulus (G/S) of the two asphalt samples is obtained*) Phase angle (delta) and rutting factor (G)*/sin delta), and the rut factor is used as the evaluation index of the high-temperature performance of the asphalt;
(2) preparing No. 70 matrix asphalt and graphene modified asphalt into bending beam rheological test standard samples, performing a low-temperature crack resistance test by using a bending beam rheometer, inputting constant stress for continuous loading for 240s at the temperature of-12 ℃ and-18 ℃, recording stiffness moduli and creep rates of 8.0s, 15.0s, 30.0s, 60.0s, 120.0s and 240.0s in the test process, and evaluating the low-temperature crack resistance of the two asphalt samples by using the measured creep stiffness moduli and the measured creep rates;
(3) preparing No. 70 matrix asphalt and graphene modified asphalt into a standard sample for force ductility test, testing by adopting an asphalt ductility tester, stretching the sample at a stretching speed of 5cm/min at a temperature of 5 ℃, and measuring the maximum tensile force (F) of the two asphalt samples at the time of fracturemax) Maximum elongation displacement (D) and displacement corresponding to maximum tension (D)1) Respectively calculating tensile compliance (f) and yield strain energy (E) by adopting formulas I and II;
f=Fmax/D ①
E=Fmax/D ②
(4) carrying out a multi-stress creep recovery test on No. 70 matrix asphalt and graphene modified asphalt, testing the fatigue characteristics of the asphalt by using the same dynamic shear rheometer as that in the step (1), wherein the test temperature is 70 ℃, the test time is 1.0s and the test time is 9.0s under eight stress states of 0.1kPa, 0.5kPa, 1.0kPa, 1.5kPa, 2.0kPa, 2.5kPa, 3.0kPa and 3.2kPa, ten cycles are repeated, and the initial strain value (epsilon) of the stress level (sigma) in the loading stage is recorded0) Strain value (epsilon) at the end of the loading phasec) 10 th second test end strain (. epsilon.)r) Calculating the strain increment (epsilon) of two asphalt samples in the loading stage by adopting formulas (c), (c) and (c)1) 10 th second test end Strain increase value (. epsilon.)10) Average percent recovery (% R) and non-recoverable creep compliance (J)nr);
ε1=εc0
ε10=εr0
%R=[(ε110)/ε1]×100% ⑤
Jnr=(εr0)/σ ⑥
(5) Preparing No. 70 matrix asphalt and graphene modified asphalt into a standard sample for direct tensile test, adopting a universal material testing machine to stretch the sample at a tensile rate of 5mm/min at 25 ℃ until the sample is broken, and recording the peak tensile force (F) of the asphalt sample during the test, wherein the width of the sample is a mm, the thickness of the sample is b mm, and the peak tensile force (F) of the asphalt sample ish) Obtaining stress-strain relation curves of the substrate asphalt and the graphene modified asphalt, and calculating the tensile strength (T) of the two samples by adopting a formulas);
Ts=Fh/(a×b) ⑦
(6) Performing atomic force microscope test on No. 70 matrix asphalt and graphene modified asphalt, dripping a small amount of asphalt into the center of a glass slide to prepare a sample with the length and the width of 30mm, making the surface of the asphalt sample smooth and without obvious pits, selecting a scanning mode as a peak force mode, and performing force curve test on the surfaces of the matrix asphalt and the graphene modified asphalt respectively at the frequency of 2kHz to obtain the micro morphology and Young modulus (E) of the sample*) Adhesion (F)adh) Comparing the difference between the matrix asphalt and the graphene modified asphalt in terms of microstructure change, and analyzing the influence of graphene on the micromechanical property of the asphalt;
(7) carrying out an X-ray diffraction test on No. 70 matrix asphalt and graphene modified asphalt, setting the scanning speed to be 5 degrees/min and the scanning range to be 5-80 degrees, analyzing the change of the micro-phase structures of two asphalt samples before and after adding graphene, comparing the diffraction peak positions, the diffraction peak intensities and the peak areas of the matrix asphalt and the graphene modified asphalt, and analyzing the influence of an intercalation structure formed by the graphene and the asphalt on the mechanical property of the asphalt;
(8) the influence of the graphene on the high-low temperature performance, the fatigue property, the tensile strength, the micro mechanical property and the micro phase structure of No. 70 matrix asphalt is comparatively analyzed, the reinforcing effect of the graphene on the No. 70 matrix asphalt is comprehensively researched, and the reinforcing mechanism of the graphene on the mechanical property of the asphalt is disclosed.
CN202111083496.XA 2021-09-15 2021-09-15 Method for researching mechanism of graphene for enhancing mechanical properties of asphalt Pending CN113720703A (en)

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