CN107731551B - A method of high-quality carbon electrode is manufactured using laser etching techniques rapid, high volume - Google Patents
A method of high-quality carbon electrode is manufactured using laser etching techniques rapid, high volume Download PDFInfo
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- CN107731551B CN107731551B CN201711136458.XA CN201711136458A CN107731551B CN 107731551 B CN107731551 B CN 107731551B CN 201711136458 A CN201711136458 A CN 201711136458A CN 107731551 B CN107731551 B CN 107731551B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000010329 laser etching Methods 0.000 title claims abstract description 7
- 239000005011 phenolic resin Substances 0.000 claims abstract description 27
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000010330 laser marking Methods 0.000 claims abstract description 9
- 238000000608 laser ablation Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 12
- 238000007711 solidification Methods 0.000 claims description 9
- 230000008023 solidification Effects 0.000 claims description 9
- 229920003169 water-soluble polymer Polymers 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims description 2
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 9
- 230000008859 change Effects 0.000 abstract description 3
- 238000002484 cyclic voltammetry Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 description 10
- 239000010439 graphite Substances 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 229910052697 platinum Inorganic materials 0.000 description 5
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 3
- 229960004011 methenamine Drugs 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- RCHKEJKUUXXBSM-UHFFFAOYSA-N n-benzyl-2-(3-formylindol-1-yl)acetamide Chemical compound C12=CC=CC=C2C(C=O)=CN1CC(=O)NCC1=CC=CC=C1 RCHKEJKUUXXBSM-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012956 testing procedure Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention provides a kind of methods for manufacturing high-quality carbon electrode using laser etching techniques rapid, high volume, with macromolecular water-soluble phenolic resin, alkaline curing agent, laser marking machine and smearable conductive substrates.The present invention reduces electrode preparation time, time cost is substantially reduced, and raw materials used price is extremely cheap, preparation method is simple.Carbon electrode prepared by the present invention is practically free of any impurity, is the porous carbon structure of high-purity.Laser ablation can choose diversified figure, different mark speed and power, and then can change the cyclic voltammetry curve of electrode, and the carbon electrode of the electrode that the property of can choose preparation needs, preparation has good spike potential poor.It due to the flow behavior before macromolecular water-soluble phenolic resin curing, can be cured in the substrate of any materials, and the phenolic resin film after solidifying also has certain flexibility, this provides possibility to prepare flexible electrode circuit.
Description
Technical field
The present invention relates to a kind of methods that rapid, high volume prepares high-quality carbon electrode, and in particular to uses macromolecular water-soluble phenolic aldehyde
Resin, alkaline curing agent, laser marking machine and arbitrarily can be applied conductive substrates.
Background technique
Electrode is the core of electrochemical field, and the material for being usually used in making electrode has platinum, gold, carbon, mercury etc..Wherein platinum electrode
As a kind of most common electrode material, there is chemical property to stablize, hydrogen overpotential is small, and the platinum of high-purity is easy to get, and holds
The advantages that easy processing.But the low mutability of the mechanical strength of platinum electrode, and price is very expensive.The metal material the same for same platinum
For material gold, the disadvantage as solid electrode maximum is exactly that hardness is lower, it is difficult to effectively be encapsulated, i.e. electrode fabrication fiber crops
It is tired, and golden material construction is also costly.And mercury electrode is since itself is easy to dissolve, so being not suitable for being used to observe in electrolyte to change
Close the oxidation reaction of object.In conclusion metal electrode generally has at high price, difficult problem is made.Therefore, electric conductivity compared with
Good, the stable carbon of chemical property is just widely used for substitution noble metal and uses as electrode material.Glass-carbon electrode is using most wide
General carbon electrode, but require before each use of glass-carbon electrode by polishing cleaning and activation process repeatedly.Wherein appoint
What step goes wrong, and can all influence the reproducibility of electrochemical process.Meanwhile in polishing cleaning process, need to consume a large amount of
Manpower and material resources, such as use the grinding agents such as a large amount of aluminium oxide and acidic activated electrolyte.Polishing cleaning electrode is consumed
Time occupied the significant portion in electro-chemical test.Meanwhile its price of the glass-carbon electrode of commercialization is still not cheap enough,
Especially in being chemically modified electrode testing procedure, it is difficult to carry out more electrode control experiments of big batch.
There is the problems such as above manufacture is difficult, expensive, reproducibility is low for traditional electrode, develops a kind of rapid, high volume
It prepares electrode material and the technology for solving traditional electrode disadvantage is particularly important.The chemical cooperated reaction process of laser-is international
On new development in recent years manufacture functional material important means, can be used for manufacturing various electrochemical capacitances and battery material.And swash
The hot corrasion of light can be combined with the heat chemistry transition process of polymer, form the glassy state carbon materials with porous structure
Material.Therefore, the laser of suitable presoma and suitable power and wavelength is selected, then may be with excellent by polymer conversion
The carbon electrode of chemical property.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing high-quality carbon electrode using laser etching techniques rapid, high volume.
Technical solution of the present invention:
A method of high-quality carbon electrode being manufactured using laser etching techniques rapid, high volume, steps are as follows:
(1) curing agent is dissolved in ethyl alcohol, ultrasound stirs curing agent and water soluble polymer phenolic resin to abundant dissolution
It mixes to be uniformly mixed;Wherein, curing agent accounts for the 3%~30% of water soluble polymer PF resin concentration;
(2) phenolic resin containing curing agent is applied in conductive substrates, and is allowed to apply and puts down, film thickness is 20~300
Micron;Under the conditions of not destroying the temperature of phenolic resin characteristic, it is abundant to be allowed to solidification for dry solidification;
(3) the macromolecule phenolic resin film after solidification is placed under laser marking machine, selects suitable laser power and figure
Shape carries out laser ablation.
The mark speed that the laser marking machine is selected is 0~4000mm/s, laser power is 0~100%, frequency is
1~20KHZ;The high-quality carbon electrode of high-purity is obtained after etching.
The curing agent is alkali compounds, specially methenamine, sodium carbonate, ammonium hydroxide, sodium hydroxide or triethylamine.
Effect and benefit of the invention: the present invention prepares electrode using laser ablation, to industrialize a large amount of fast and low-costs
The high-quality carbon electrode for preparing provide a kind of general method of feasibility.One, it The present invention reduces electrode preparation time, drops significantly
Low time cost, and raw materials used price is extremely cheap, and preparation method is simple.Two, carbon electrode prepared by the present invention is several
Any impurity is not contained, is the porous carbon structure of high-purity, and porous carbon includes micropore, mesoporous and macropore.Three, laser incising
Erosion can choose diversified figure, different mark speed and power, and then can change the cyclic voltammetry curve of electrode,
The carbon electrode of the electrode that the property of can choose preparation needs, preparation has good spike potential poor, about 60~80mv or so.Four, by
Flow behavior before macromolecular water-soluble phenolic resin curing can be cured in the substrate of any materials, such as: wood
Plate, metal, oxidation film etc., and the phenolic resin film after solidifying also has certain flexibility, this is prepares flexible electrode circuit
Provide possibility.
Detailed description of the invention
Fig. 1 is flexible graphite substrate carbon electrode schematic diagram.
In figure: 1 flexible graphite substrate (does not smear phenolic resin);2 phenolic resin films: the porous carbon electrodes of 3 laser ablations.
Specific embodiment
Below in conjunction with attached drawing and technical solution, further the present invention will be described in detail.
A method of high-quality carbon electrode is prepared using laser etching techniques rapid, high volume, the specific steps are as follows:
Embodiment 1
(1) CorelDRAW software design electrode pattern is used.
(2) water soluble phenol resin 5.66g is weighed, takes 0.453g methenamine in a small amount of ethyl alcohol, ethyl alcohol will be dissolved in
Methenamine is mixed with phenolic resin, and it is abundant that stirring is allowed to mixing for 10 minutes.
(3) flexible conducting substrate is produced.Compressed graphite paper is adhered on the flexible heat resistant plastic foil with glue.Then will
(2) the water soluble polymer phenolic resin containing urotropine firming agent prepared is uniformly applied on graphite paper, film thickness
It is 50 microns.
(4) the graphite-based bottom plate for being coated with water soluble polymer phenolic resin is put into baking oven, 80 degrees Celsius of dryings 12 are small
When, it is cured to phenolic resin sufficiently in conductive substrates.
(5) the graphite substrate of the phenolic resin after solidification is placed in laser marking to write down, is using mark speed
300mm/s, power 30%, frequency 15KHZ laser carry out laser ablation, obtain the high-quality carbon electrode of spike potential difference 73mv.
Embodiment 2
(1) CorelDRAW software design electrode pattern is used.
(2) water soluble phenol resin 7.06g is weighed, takes 0.565g triethylamine in a small amount of ethyl alcohol, the three of ethyl alcohol will be dissolved in
Ethamine is mixed with phenolic resin, and it is abundant that stirring is allowed to mixing for 15 minutes.
(3) polymer graphite conductive paper is adhered in the PET plastic substrate with glue.Then containing (2) preparation
The water soluble polymer phenolic resin of triethylamine curing agent is uniformly applied on graphite paper, and film thickness is 75 microns.
(4) the graphite-based bottom plate for being coated with water soluble polymer phenolic resin is placed in oven and dried solidification, 70 degrees Celsius
It is 18 hours dry, it is cured to phenolic resin sufficiently in conductive substrates.
(5) the graphite substrate of the phenolic resin after solidification is placed in laser marking to write down, is using mark speed
400mm/s, power 35%, frequency 20KHZ laser carry out laser ablation, obtain the high-quality carbon electrode of spike potential difference 80mv.
(6) step (5) are repeated and sets the flow work for laser marking machine, conductive substrates are placed in roller transfer band
On, it can the high-quality carbon electrode of rapid, high volume manufacture.
Claims (1)
1. a kind of method for manufacturing high-quality carbon electrode using laser etching techniques rapid, high volume, which is characterized in that steps are as follows:
(1) curing agent is dissolved in ethyl alcohol, ultrasound to abundant dissolution, by curing agent and the stirring of water soluble polymer phenolic resin with
It is uniformly mixed;Wherein, curing agent accounts for the 3%~30% of water soluble polymer PF resin concentration;
(2) phenolic resin containing curing agent is applied in conductive substrates, and is allowed to apply and puts down, film thickness is 20~300 microns;
Under the conditions of not destroying the temperature of phenolic resin characteristic, it is abundant to be allowed to solidification for dry solidification;
(3) the macromolecule phenolic resin film after solidification is placed under laser marking machine, select suitable laser power and figure into
Row laser ablation;
The curing agent is sodium carbonate, ammonium hydroxide, sodium hydroxide or triethylamine;
The mark speed that the laser marking machine is selected is 0~4000mm/s, laser power is 0~100%, frequency be 1~
20KHZ;The high-quality carbon electrode of high-purity is obtained after etching.
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Families Citing this family (5)
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CN111217351B (en) * | 2018-11-26 | 2022-11-08 | 中国科学院大连化学物理研究所 | Method for preparing magnetic porous carbon by laser ablation method |
CN110518256A (en) * | 2019-08-06 | 2019-11-29 | 大连理工大学 | A method of it is composite porous using laser pyrolysis rapid, high volume manufacture high-test metal/carbon |
CN112723855B (en) * | 2019-10-14 | 2022-03-04 | 武汉大学 | Laser engraving preparation method and application of graphene-ceramic composite electrode array |
CN111354576B (en) * | 2020-03-03 | 2022-05-17 | 华东理工大学 | Fabric-based flexible supercapacitor and manufacturing method thereof |
CN112349914A (en) * | 2020-10-26 | 2021-02-09 | 深圳大学 | Carbon sponge electrode for vanadium redox flow battery, preparation method and battery |
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---|---|---|---|---|
CN1393397A (en) * | 2001-07-02 | 2003-01-29 | 中国科学院山西煤炭化学研究所 | Process for preparing phenolic resin-carbon material used as negative electrode of Li-ion battery |
CN105322224A (en) * | 2014-07-29 | 2016-02-10 | 福特全球技术公司 | Batteries prepared by spinning |
CN106164018A (en) * | 2014-02-13 | 2016-11-23 | 莫里斯兄弟控股有限公司 | For the method manufacturing three-dimensional body |
-
2017
- 2017-11-16 CN CN201711136458.XA patent/CN107731551B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1393397A (en) * | 2001-07-02 | 2003-01-29 | 中国科学院山西煤炭化学研究所 | Process for preparing phenolic resin-carbon material used as negative electrode of Li-ion battery |
CN106164018A (en) * | 2014-02-13 | 2016-11-23 | 莫里斯兄弟控股有限公司 | For the method manufacturing three-dimensional body |
CN105322224A (en) * | 2014-07-29 | 2016-02-10 | 福特全球技术公司 | Batteries prepared by spinning |
Non-Patent Citations (1)
Title |
---|
Direct synthesis of graphitic mesoporous carbon from green phenolic resins exposed to subsequent UV and IR laser irradiations;Mihai Sopronyi等;《Scientific RepoRts》;20161221;第6卷;第1-13页 |
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