CN114436250A - Method for preparing graphene through liquid-phase stripping - Google Patents
Method for preparing graphene through liquid-phase stripping Download PDFInfo
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- CN114436250A CN114436250A CN202011213669.0A CN202011213669A CN114436250A CN 114436250 A CN114436250 A CN 114436250A CN 202011213669 A CN202011213669 A CN 202011213669A CN 114436250 A CN114436250 A CN 114436250A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000007791 liquid phase Substances 0.000 title claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 13
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 12
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 12
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 21
- 239000010439 graphite Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000004299 exfoliation Methods 0.000 claims description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 239000000138 intercalating agent Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
Abstract
The invention relates to a method for preparing graphene by liquid-phase stripping, which comprises the following steps: dissolving polyvinylpyrrolidone in anhydrous alcohol to obtain 0.1mg/L alcohol mixture; mixing flake graphite powder with concentrated ammonia water (25-28%) or ammonium bicarbonate according to a weight ratio of 3-5: 1 to obtain a graphite powder mixture; and finally, mixing the mixture of the graphite powder and the alcohol mixture according to the weight ratio of 0.5-1.5%, loading the mixture into a closed container, carrying out ultrasonic treatment for more than 20 hours, standing for more than 20 hours, and taking the upper layer mixed solution to obtain the liquid-phase graphene.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and relates to a method for preparing graphene through liquid phase stripping.
Background
Graphene is a two-dimensional carbon nanomaterial with hexagonal and honeycomb lattices formed by carbon atoms through sp 2 hybridized orbits, and the special monoatomic layer structure of graphene determines that the graphene has rich and novel physical properties, has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
The requirement for a large amount of high-quality graphene materials with complete structures requires improvement of the existing graphene preparation process level, and realization of large-scale, low-cost and controllable synthesis and preparation of graphene, so that the large-scale preparation of graphene has important scientific and practical significance, although some methods are developed at present, industrial production is difficult to meet, or certain defects exist, the preparation methods need to be further researched and perfected, and therefore, the technology for preparing high-quality graphene in a large scale is one of bottlenecks which restrict the high-quality graphene materials from entering practical application.
Common methods for producing graphene powder include mechanical exfoliation, redox, Chemical Vapor Deposition (CVD), and liquid phase exfoliation.
The micro-mechanical stripping method has the advantages of simplicity, difficult generation of structural defects, low yield, small area, difficult accurate control, low efficiency, difficult scale preparation, unsuitability for large-scale industrial production, and generally only application in basic research of laboratories, so that the development and application of the material cannot be met; the crystal epitaxial growth method requires that a growth substrate has certain crystal face orientation, has high requirements on equipment and vacuum conditions, and the graphene film adopting the method is uneven in thickness and is tightly adhered to the substrate, so that the performance of the graphene is greatly influenced; the Chemical Vapor Deposition method (Chemical Vapor Deposition CVD) is a method for industrially preparing a semiconductor thin film material on a large scale, but the method has high preparation cost and low production efficiency; the graphene oxide reduction method is the hottest method for preparing graphene at present, graphene oxide is obtained by ultrasonic stripping after graphite is oxidized by a strong oxidant, and finally oxygen-containing functional groups are reduced and removed by a reducing agent.
The liquid phase stripping method is to strip graphite in a solvent by using a specific solvent or a surfactant and an ultrasonic method, and compared with a micro-mechanical stripping and epitaxial growth method, the liquid phase stripping method is an effective method which is expected to realize low-cost large-scale preparation of graphene.
The graphene dispersion liquid obtained by the liquid phase stripping method has a complete graphene structure and high quality; and the graphene can be transferred to other substrates for preparing graphene devices, and can also be reacted or blended with other substances in a dispersion liquid for preparing graphene composite materials, so that the method for preparing graphene in a modeling manner by using a liquid phase stripping method is considered to be the most possible industrialized method, and the obtained graphene has a complete structure and is free from defects.
The liquid phase stripping method for preparing the graphene dispersion liquid shows unique advantages in the aspects of large-scale preparation, high graphene quality, easy functionalization, wide raw material, low cost and the like, but before the liquid phase stripping method for preparing the graphene dispersion liquid is industrially produced, some problems still need to be solved: the stability problem of the graphene dispersion liquid, the effect problem of the intercalation agent and the problem of environmental pollution.
Disclosure of Invention
Of the above three problems, the stability problem of the graphene dispersion is the most important problem among them, and this problem is usually to adjust the surface energy of graphene by adding a surfactant.
The preparation of graphene by exfoliation needs to overcome the van der waals force between graphite layers, and the dispersion of graphite in liquid is a direct and effective way to reduce the van der waals force, which makes the liquid phase exfoliation method possible to be industrialized.
To achieve the aim, through comparison of different surfactants, polyvinylpyrrolidone is found to be an ideal surfactant for dispersing and stabilizing graphene.
In order to peel off the layered graphite, an intercalator with a molecular diameter slightly larger than the interlayer spacing of the graphite needs to be selected, particularly, atoms with very strong coordination capacity are required in the intercalator molecules, so that the intercalator molecules can be inserted into the interlayer of the layered graphite, the nitrogen atom has a small radius, the outer layer has redundant empty tracks, and the coordination capacity of the intercalator is super strong.
The method utilizes polyvinylpyrrolidone as a dispersing agent, ammonia water or ammonium bicarbonate as an intercalating agent, and disperses graphite powder into graphene under the action of ultrasonic waves.
The flake graphite, alcohol, polyvinylpyrrolidone, ammonia water and ammonium bicarbonate in the adopted raw materials are all environment-friendly substances.
The purpose of the invention can be realized by the following technical scheme:
a method for preparing graphene through liquid phase stripping is characterized by comprising the following steps:
1) dissolving polyvinylpyrrolidone in anhydrous alcohol to obtain 0.1mg/L alcohol mixture;
2) mixing flake graphite powder with a particle size of more than 800 meshes with concentrated ammonia water (25-28%) or ammonium bicarbonate according to a weight ratio of 3-5: 1 to obtain a graphite powder mixture;
3) mixing the mixture of graphite powder and the alcohol mixture according to the weight ratio of 1%, loading the mixture into a closed container, performing ultrasonic dispersion treatment for more than 20 hours, standing for more than 20 hours, and taking the upper layer mixed solution to obtain the liquid-phase graphene.
The invention dissolves polyvinylpyrrolidone in alcohol solution to obtain dispersant, the solid content of polyvinylpyrrolidone is 95-100%, K value is 81-96, the ethanol content of absolute alcohol is more than or equal to 99.7%, the dispersant has approximate surface energy with graphite, and no agglomeration phenomenon is generated in the similar surface energy solution after graphite powder is dispersed by ultrasonic wave.
According to the invention, ammonia molecules, water molecules or carbon dioxide molecules decomposed from concentrated ammonia water or ammonium bicarbonate are used as an intercalation agent, the crystalline flake graphite powder is crystalline flake graphite with a particle size of more than 800 meshes, the concentrated ammonia water is analytically pure ammonia water with a particle size of 25-28%, the ammonium bicarbonate is in a food grade, and the weight ratio of the graphite powder to the concentrated ammonia water or ammonium bicarbonate is 3-5: 1.
The weight ratio of the mixture of the graphite powder to the alcohol mixture is 0.5-1.5%.
The graphite powder dispersion liquid is filled in a closed container, ultrasonic dispersion treatment is carried out for more than 20 hours, and the intercalation agent is timely inserted into the graphite sheet layer in the ultrasonic dispersion process to disperse the graphite sheet layer.
And (3) obtaining a dispersion liquid of the graphene after ultrasonic treatment for 20 hours, wherein the dispersion liquid can not be layered even standing for 20 hours, taking the dispersion liquid, naturally volatilizing the liquid, and detecting by using SEM (scanning electron microscope) to find that the phenomena of bending, folding and perspective lower layer of a graphite sheet layer occur, so that the graphene is confirmed.
The prepared graphene can be directly added into aqueous and oily substances or can be directly mixed into powdery substances.
Compared with the prior art, the invention has the following characteristics:
1) the material prepared by the invention is simple and easy to obtain and has low cost;
2) the preparation equipment is simple and low in price;
3) the raw materials, the preparation process and the application of the invention have no pollution to the environment;
4) the method can obtain a large amount of graphene, and is easy to realize industrial production;
5) the graphene prepared by the method is easy to use.
The invention can realize effective stripping of graphite flakes, and the obtained graphite flakes have the advantages of excellent performance, good quality, good compatibility with media such as water and the like, excellent dispersibility and wide application prospect.
Drawings
Fig. 1 is a scanning electron microscope image of graphene prepared in example 1.
Fig. 2 is a scanning electron microscope image of graphene prepared in example 2.
Fig. 3 is a scanning electron microscope image of graphene prepared in example 3.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
Example 1:
1) dissolving polyvinylpyrrolidone in anhydrous alcohol to obtain 0.1mg/L alcohol mixture;
2) mixing 1000-mesh crystalline graphite powder and ammonium bicarbonate according to the weight ratio of 5:1 to obtain a graphite powder mixture;
3) mixing the mixture of graphite powder and the alcohol mixture according to the weight ratio of 1%, loading the mixture into a closed container, performing ultrasonic dispersion treatment for 30 hours, standing for 48 hours, and taking the upper layer mixed solution to obtain the liquid-phase graphene.
The upper layer mixture is dropped on the copper foil to naturally volatilize the liquid, and then the liquid is observed by a scanning electron microscope, as shown in fig. 1, the scanning electron microscope image of the graphene prepared in the example 1 is shown, and as can be seen from the image, the obtained product is in a corrugated sheet structure, which indicates that the graphite is successfully peeled to form the graphene.
Example 2:
1) dissolving polyvinylpyrrolidone in anhydrous alcohol to obtain 0.1mg/L alcohol mixture;
2) mixing 1000-mesh crystalline graphite powder and ammonium bicarbonate according to the weight ratio of 4:1 to obtain a graphite powder mixture;
3) mixing the mixture of graphite powder and the alcohol mixture according to the weight ratio of 1%, loading the mixture into a closed container, performing ultrasonic dispersion treatment for 50 hours, standing for 20 hours, and taking the upper layer mixed solution to obtain the liquid-phase graphene.
When the upper layer mixture is dropped on the copper foil to naturally volatilize the liquid, and then the liquid is observed by a scanning electron microscope, as shown in fig. 2, the scanning electron microscope image of the graphene prepared in the example 2 is shown, the obtained product is in a corrugated sheet structure, and large graphite sheets are attached to the concave-convex grooves with the thickness of about 1 μm, which indicates that the graphite is successfully peeled to form the graphene.
Example 3:
1) dissolving polyvinylpyrrolidone in anhydrous alcohol to obtain 0.1mg/L alcohol mixture;
2) mixing 1000-mesh flake graphite powder with 28% ammonia water according to the weight ratio of 4:1 to obtain a graphite powder mixture;
3) mixing the mixture of graphite powder and the alcohol mixture according to the weight ratio of 1%, loading the mixture into a closed container, performing ultrasonic dispersion treatment for 20 hours, standing for 20 hours, and taking the upper layer mixed solution to obtain the liquid-phase graphene.
After the upper layer mixture is dropped onto the copper foil to naturally volatilize the liquid, the scanning electron microscope is used for observation, as shown in fig. 3, a scanning electron microscope image of the graphene prepared in the embodiment 3 is shown, and as can be seen from the image, the grooves of the substrate can be seen through the graphite sheet layer by using the scanning electron microscope, which indicates that the graphite is successfully exfoliated into the graphene.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art.
It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty.
Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (9)
1. A method for preparing graphene through liquid phase stripping is characterized by comprising the following steps:
1) dissolving polyvinylpyrrolidone in anhydrous alcohol to obtain 0.1mg/L alcohol mixture;
2) mixing flake graphite powder with concentrated ammonia water (25-28%) or ammonium bicarbonate according to a weight ratio of 3-5: 1 to obtain a graphite powder mixture;
3) mixing the mixture of graphite powder and the alcohol mixture according to the weight ratio of 0.5-1.5%, loading the mixture into a closed container, performing ultrasonic dispersion treatment for more than 20 hours, standing for more than 20 hours, and taking the upper layer mixed solution to obtain the liquid-phase graphene.
2. The method for preparing graphene by liquid phase exfoliation according to claim 1, wherein in step 1), the polyvinylpyrrolidone has a solid content of 95-100% and a K value of 81-96.
3. The method for preparing graphene through liquid-phase exfoliation according to claim 1, wherein in the step 1), the ethanol content of the absolute alcohol is not less than 99.7%.
4. The method for preparing graphene by liquid phase exfoliation according to claim 1, wherein in the step 2), the crystalline flake graphite powder is crystalline flake graphite with a particle size of 800 meshes or more.
5. The method for preparing graphene through liquid phase exfoliation according to claim 1, wherein in the step 2), the concentrated ammonia water is 25-28% of analytically pure ammonia water, and the ammonium bicarbonate is food grade.
6. The method for preparing graphene through liquid-phase exfoliation according to claim 1, wherein in the step 2), the weight ratio of graphite powder to concentrated ammonia water or ammonium bicarbonate is 3-5: 1.
7. The method for preparing graphene by liquid phase exfoliation according to claim 1, wherein in the step 3), the weight ratio of the mixture of graphite powder and the alcohol mixture is 0.5-1.5%.
8. The method for preparing graphene by liquid-phase exfoliation according to claim 1, wherein in the step 3), the graphite powder dispersion liquid is filled in a closed container and subjected to ultrasonic dispersion treatment for more than 20 hours.
9. The method for preparing graphene by liquid-phase exfoliation according to claim 1, wherein in the step 3), the mixture after the ultrasonic treatment is left to stand for more than 20 hours, and the upper-layer mixture is taken to obtain the liquid-phase graphene.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172053A (en) * | 2011-12-20 | 2013-06-26 | 中国科学院微电子研究所 | Method for preparing graphene through phase peeling of graphite by using mixed solvent |
| CN103449420A (en) * | 2013-08-22 | 2013-12-18 | 中国科学院金属研究所 | High-quality graphene dispersion method and film preparation method |
| CN105800603A (en) * | 2016-04-22 | 2016-07-27 | 华侨大学 | Method for quickly preparing high-quality graphene |
| CN105836734A (en) * | 2016-03-16 | 2016-08-10 | 中国科学院山西煤炭化学研究所 | Rapid preparation method for high-quality graphene |
| KR20160101556A (en) * | 2015-02-17 | 2016-08-25 | 주식회사 엘지화학 | Method for preparation of highly concentrated graphene dispersion |
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- 2020-11-04 CN CN202011213669.0A patent/CN114436250A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172053A (en) * | 2011-12-20 | 2013-06-26 | 中国科学院微电子研究所 | Method for preparing graphene through phase peeling of graphite by using mixed solvent |
| CN103449420A (en) * | 2013-08-22 | 2013-12-18 | 中国科学院金属研究所 | High-quality graphene dispersion method and film preparation method |
| KR20160101556A (en) * | 2015-02-17 | 2016-08-25 | 주식회사 엘지화학 | Method for preparation of highly concentrated graphene dispersion |
| CN105836734A (en) * | 2016-03-16 | 2016-08-10 | 中国科学院山西煤炭化学研究所 | Rapid preparation method for high-quality graphene |
| CN105800603A (en) * | 2016-04-22 | 2016-07-27 | 华侨大学 | Method for quickly preparing high-quality graphene |
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Application publication date: 20220506 |