CN110061219A - A kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber - Google Patents
A kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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Abstract
The invention discloses a kind of electrostatic spinning preparation methods of self-supporting SnTe/C nanofiber.First by SnCl2·2H2N,N-Dimethylformamide solvent is added in O, and magnetic agitation obtains colourless transparent solution to being completely dissolved;Then tellurium powder is added in colourless transparent solution, magnetic agitation obtains finely dispersed black suspension;As polyacrylonitrile and a small amount of polymethyl methacrylate are added in black suspension, continue to stir to get sticky electrostatic spinning precursor solution, it is transferred them in plain injector for medical purpose again, the spinning on electrostatic spinning apparatus, gained nano-fiber material is received with glass plate, and high temperature cabonization after being dried in vacuo to material, obtain final product SnTe/C nanofiber.Gained SnTe/C of the invention is uniform nanofiber, and diameter is about 100 ~ 300 nm, and has excellent chemical property.
Description
Technical field
The present invention relates to the preparation of self-supporting electrode material, in particular to a kind of electrostatic of self-supporting SnTe/C nanofiber
Spinning preparation method.
Background technique
By the development of many decades, battery technology is gradually mature, and the battery of high-energy density and long circulation life has become
Important energy-storage system at this stage.And as new science and technology constantly enters people's lives, people to science and technology there has also been new requirement,
Wearable battery starts to become trend in recent years, this necessarily brings the update of battery technology.The essence of battery is material
Material, constantly discovering for new material is important thrust that battery industry continues to develop, wherein two-dimensional material, that is, the transition metal being layered
Chalcogenide, graphene etc. are a kind of material of representative, have unique property due to the lesser nanostructure of size.Its
In, it is a kind of that the fusing point of SnTe, which is 780 DEG C, space group Fm3m, and the forbidden bandwidth of block SnTe is 0.18 eV at room temperature
Important narrow band gap (direct band gap) semiconductor, and the high density of SnTe makes it possess higher volume and capacity ratio, is recognized
To be the promising negative electrode material of lithium/sodium-ion battery.
Electrospinning process is a kind of special fiber fabrication process, by conducting polymer fluid atomizing in forceful electric power is had a meeting, an audience, etc. well under one's control
At the thread with nanostructure, nanofiber is solidified into longer injection route.This method is lower to environmental requirement,
Easy to operate, resulting materials have biggish specific surface area and porosity, are the effective ways that new energy field prepares basic material.
All required reagents are added in the present invention simultaneously during electrostatic spinning, and nano-fiber material obtained by spinning is obtained through one-step calcination
Final product, process is simple and environmentally-friendly, product safely cleaning, is a kind of excellent spinning mode of innovative energy-saving.
Summary of the invention
The purpose of the present invention is to provide a kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber, utilization is quiet
The method of Electrospun is prepared for a kind of SnTe/C material of self-supporting, and nanofibrous structures can effectively inhibit tin base cathode
Volume expansion of the material in charge and discharge process;The speciality of its self-supporting becomes application of the material in self-supporting battery can
Can, it is a kind of lithium/sodium ion negative electrode material of great prospect.
The technical solution of the present invention is as follows:
A kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber, includes the following steps:
(1) by SnCl2·2H2O is added in solvent n,N-Dimethylformamide, and magnetic agitation obtains colourless to after being completely dissolved
Transparent solution;
(2) tellurium powder is added into step (1) acquired solution, continues magnetic agitation, obtains finely dispersed black suspension;
(3) polyacrylonitrile and polymethyl methacrylate are added into suspension obtained by step (2), continues magnetic agitation,
Sufficiently dissolution, obtains sticky black ESD spinning precursor solution;
(4) electrostatic spinning presoma liquid relief obtained by step (3) is subjected to Static Spinning with electrostatic spinning machine into flat needle applicator
Silk, gained nanofiber are collected with glass plate;
(5) after the nanofiber drying collected to step (4), collection nanofiber, which is placed in inert gas, to be carbonized, and obtains
The SnTe/C material of self-supporting;
Further, in step (1), SnCl2·2H2The mass fraction of O in the solution is 12.6 ~ 25.88%.
Further, in step (2), the amount ratio of the tellurium powder of addition and n,N-Dimethylformamide be 3 ~ 6 mmol:4 ~
6ml。
Further, in step (3), the polyacrylonitrile average molecular weight of addition is 150000 further SnCl2·
2H2O, tellurium powder, polyacrylonitrile, polymethyl methacrylate mass ratio be 3 ~ 6:1 ~ 2:1.6 ~ 5: 0.5 ~ 1.5.
Further, in step (4), spinning parameter are as follows: voltage be 15 ~ 20 kV, micro-injection flow rate pump be 0.2 ~
0.8 mL/h, syringe needle internal diameter are 0.8 ~ 1.2 mm, and receiving the distance i.e. spacing of spinning nozzle and receiver board is 15 ~ 22 cm, spinning
Instrument internal temperature is 20 ~ 40 DEG C.
Further, dry to be dried in vacuo in step (5), temperature is 60 ~ 110 DEG C.
Further, it in step (5), is carbonized in N2It is carried out under atmosphere, detailed process are as follows: with the heating speed of 2 ~ 5 DEG C/min
Rate is raised to 550 ~ 700 DEG C from room temperature, keeps the temperature 1 ~ 6 h, be then cooled to room temperature with the rate of temperature fall of 2 ~ 5 DEG C/min.
The present invention has following technical effect that
The present invention is prepared for a kind of SnTe/C material of self-supporting using electrospinning process easy to operate, during the spinning process
SnCl is added2With the common spinning of tellurium powder, equally distributed solid-state tellurium powder and SnCl in tube furnace inert atmosphere2It directly reacts, warp
One-step calcination is crossed, resulting materials are uniform nano-fiber material, and distribution of fiber diameters has good in 100 ~ 300 nm
Flexibility and excellent chemical property, can be used for self-supporting battery, be a kind of cathode of great prospect of lithium/sodium-ion battery
Material.
Detailed description of the invention
Fig. 1 is the x-ray diffraction pattern of SnTe/C prepared by the embodiment of the present invention 3.
Fig. 2 is the SnTe/C self-supporting nanofiber for preparing in 650 DEG C of high temperature cabonizations of the embodiment of the present invention 3 as cathode material
Material, lithium piece are to be assembled into button cell to electrode.At 20 ~ 25 DEG C, in the voltage range of 0.01 ~ 2.5 V, 200 mA
g-1Current density under carry out charge-discharge test charging and discharging curve figure.
Fig. 3 is that (amplification factor is for the scanning electron microscope (SEM) photograph of self-supporting SnTe/C nanofiber prepared by the embodiment of the present invention 3
15000 times).
Fig. 4 is that self-supporting SnTe/C nanofiber prepared by the embodiment of the present invention 3 is electric as sodium-ion battery self-supporting
The photo of pole.
Specific embodiment
The present invention will be further described combined with specific embodiments below, but the present invention is not limited thereto.
Embodiment 1
The n,N-Dimethylformamide solution of 5 mL is placed in the salable vial of 10 mL at room temperature, is added into solution
1.354 g SnCl2·2H2O(6mmol it) is sufficiently stirred to obtain colourless transparent solution;0.766g tellurium powder (6mmol) is added, after
It is continuous to stir to get black suspension;0.5 g polyacrylonitrile and 0.2 g polymethyl methacrylate are added into black suspension,
6 h of magnetic agitation is sticky uniformly to solution, obtains electrostatic spinning presoma;The electrostatic spinning presoma of brand-new is injected into plain head
In syringe, spinning is carried out with electrostatic spinning machine, nanofiber obtained by spinning is collected with glass plate, spinning parameter are as follows: voltage is
18 kV, micro-injection flow rate pump are 0.4 mL/h, and syringe needle internal diameter is 1.2 mm, receive distance (between spinning nozzle and receiver board
Away from) it is 15 cm, spinning instrument internal temperature is 25 DEG C.By collecting nanofibers obtained by spinning in porcelain boat, it is placed in vacuum oven
60 DEG C of 6 h of drying;High temperature cabonization is carried out under nitrogen protection to the nanofiber after drying, specifically: with the heating of 5 DEG C/min
Rate is raised to 750 DEG C from room temperature, keeps the temperature 8 h, be cooled to room temperature later with the rate of temperature fall of 5 DEG C/min, obtain SnTe/C, because
Carburizing temperature is excessively high, and carbonization time is too long, and resulting materials lose self-supporting.
Embodiment 2
The n,N-Dimethylformamide solution of 5 mL is placed in the salable vial of 10 mL at room temperature, is added into solution
0.903 g SnCl2·2H2O(4mmol it) is sufficiently stirred to obtain colourless transparent solution;Add 0.511 g(4mmol) tellurium powder, after
It is continuous to stir to get black suspension;0.5 g polyacrylonitrile and 0.1 g polymethyl methacrylate are added into black suspension,
6 h of magnetic agitation is sticky uniformly to solution, obtains electrostatic spinning presoma;The electrostatic spinning presoma of brand-new is injected into plain head
In syringe, spinning is carried out with electrostatic spinning machine, nanofiber obtained by spinning is collected with glass plate, spinning parameter are as follows: voltage is
16 kV, micro-injection flow rate pump are 0.2 mL/h, and syringe needle internal diameter is 1.2 mm, receive distance (between spinning nozzle and receiver board
Away from) it is 19 cm, spinning instrument internal temperature is 35 DEG C.By collecting nanofibers obtained by spinning in porcelain boat, it is placed in vacuum oven
60 DEG C of 6 h of drying;High temperature cabonization is carried out under nitrogen protection to the nanofiber after drying, specifically: with the heating of 5 DEG C/min
Rate is raised to 500 DEG C from room temperature, keeps the temperature 4 h, be cooled to room temperature later with the rate of temperature fall of 5 DEG C/min, it is incomplete to obtain carbonization
SnTe/C be carbonized not complete enough, resulting materials are led because of the reasons such as carbonization time is shorter and other process conditions are not enough suitable for
It is electrically poor.
Embodiment 3
The n,N-Dimethylformamide solution of 5 mL is placed in the salable vial of 10 mL at room temperature, is added into solution
0.677 g SnCl2·2H2O(3mmol it) is sufficiently stirred to obtain colourless transparent solution;0.383g tellurium powder (3mmol) is added, after
It is continuous to stir to get black suspension;0.5 g polyacrylonitrile and 0.1 g polymethyl methacrylate are added into black suspension
(pore creating material), 6 h of magnetic agitation is sticky uniformly to solution, obtains electrostatic spinning presoma;By the electrostatic spinning presoma of brand-new
It injects in flat needle applicator, carries out spinning with electrostatic spinning machine, nanofiber obtained by spinning is collected with glass plate, spinning parameter
Are as follows: voltage be 18 kV, micro-injection flow rate pump be 0.4 mL/h, syringe needle internal diameter be 1.2 mm, receive distance (spinning nozzle with connect
Receive the spacing of plate) it is 15 cm, spinning instrument internal temperature is 25 DEG C.By collecting nanofibers obtained by spinning in porcelain boat, it is placed in true
60 DEG C of 6 h of drying of empty drying box;High temperature cabonization is carried out under nitrogen protection to the nanofiber after drying, specifically: with 5 DEG C/
The heating rate of min is raised to 650 DEG C from room temperature, keeps the temperature 4 h, later with the rate of temperature fall of 5 DEG C/min be cooled to room temperature to get
Final product SnTe/C.
Embodiment 4
The n,N-Dimethylformamide solution of 5 mL is placed in the salable vial of 10 mL at room temperature, is added into solution
0.9 g SnCl2·2H2O(4mmol it) is sufficiently stirred to obtain colourless transparent solution;Add 0.51g(4mmol) tellurium powder, continues to stir
It mixes to obtain black suspension;0.5 g polyacrylonitrile is added into black suspension, 6 h of magnetic agitation is sticky uniformly to solution, obtains
To electrostatic spinning presoma;The electrostatic spinning presoma of brand-new is injected in flat needle applicator, is spun with electrostatic spinning machine
Silk, spinning gained nanofiber are collected with glass plate, spinning parameter are as follows: voltage is 15 kV, and micro-injection flow rate pump is 0.4
ML/h, syringe needle internal diameter are 1.2 mm, and receiving distance (spacing of spinning nozzle and receiver board) is 15 cm, and spinning instrument internal temperature is
25℃.By collecting nanofibers obtained by spinning in porcelain boat, it is placed in 60 DEG C of 6 h of drying of vacuum oven;To the nanometer after drying
Fiber carries out high temperature cabonization under nitrogen protection, specifically: with the heating rate of 5 DEG C/min, 700 DEG C are raised to from room temperature, heat preservation 3
H is cooled to room temperature later to get the production compared with small specific surface product is possessed because being not added with pore creating material with the rate of temperature fall of 5 DEG C/min
Object SnTe/C, the material is opposite lower storage sodium capacity.
Embodiment 5
The n,N-Dimethylformamide solution of 5 mL is placed in the salable vial of 10 mL at room temperature, is added into solution
1.354 g SnCl2·2H2O(6mmol it) is sufficiently stirred to obtain colourless transparent solution;Add 0.765g(6mmol) tellurium powder, after
It is continuous to stir to get black suspension;0.5 g polyacrylonitrile is added into black suspension, 6 h of magnetic agitation is sticky to solution
It is even, obtain electrostatic spinning presoma;The electrostatic spinning presoma of brand-new is injected in flat needle applicator, with electrostatic spinning machine into
Row spinning, spinning gained nanofiber are collected with glass plate, spinning parameter are as follows: voltage is 12 kV, and micro-injection flow rate pump is
0.6 mL/h, syringe needle internal diameter are 2.0 mm, and receiving distance (spacing of spinning nozzle and receiver board) is 15 cm, temperature inside spinning instrument
Degree is 25 DEG C.By collecting nanofibers obtained by spinning in porcelain boat, it is placed in 60 DEG C of 6 h of drying of vacuum oven;After drying
Nanofiber carries out high temperature cabonization under nitrogen protection, specifically: with the heating rate of 5 DEG C/min, 700 DEG C are raised to from room temperature,
3 h are kept the temperature, are cooled to room temperature later with the rate of temperature fall of 5 DEG C/min, the non-uniform SnTe/C of fiber thickness are obtained, due to spinning
Parameter setting is unreasonable to cause spinning fibre thickness different, does not have intact fibre structure, resulting materials electric conductivity after firing
It is poor.
3 products obtained therefrom of embodiment is used for all kinds of characterizations, characterization result is as follows.
Shown in Fig. 1, by can be seen that prepared by embodiment 3 with the standard card PDF 46-1210 of SnTe comparison
The characteristic diffraction peak of SnTe/C and SnTe is very identical, and crystallinity is high, substantially free of impurities peak, it was demonstrated that the main component of the material
For SnTe.
Shown in Fig. 2, for SnTe/C self-supporting nanofiber prepared by embodiment 3 as negative electrode material, sodium piece is to electrode, group
Dress up button cell.At 20 ~ 25 DEG C, in the voltage range of 0.01 ~ 2.5 V, 200 mA g-1Current density under carry out
The charging and discharging curve figure of charge-discharge test.First discharge specific capacity is 716.5 mAh g-1, charge specific capacity is 429.2 mAh
g-1, coulombic efficiency is 59.9% for the first time, and charge and discharge platform is clear.Prove that the self-supporting material has excellent electrochemistry cyclicity
Energy.
Shown in Fig. 3, (amplification factor is the scanning electron microscope (SEM) photograph of self-supporting SnTe/C nanofiber prepared by embodiment 3
15000 times), nanofiber diameter is uniform in figure, and about between 100 ~ 300 nanometers, fiber surface is smooth, completely without obvious hair
Thorn, defect have more completely classical spinning fibre structure.
Shown in Fig. 4, self-supporting SnTe/C nanofiber prepared by embodiment 3 is as lithium ion battery self-supporting electrode
Photo.The electrode thickness is uniform, and surfacing has preferable flexibility.It proves that the electrode material has and realizes self-supporting battery
Possibility.
Claims (8)
1. a kind of electrostatic spinning preparation method of self-supporting SnTe/C nanofiber, which comprises the steps of:
(1) by SnCl2·2H2O is added in solvent n,N-Dimethylformamide, and magnetic agitation obtains colourless to after being completely dissolved
Transparent solution;
(2) tellurium powder is added into step (1) acquired solution, continues magnetic agitation, obtains finely dispersed black suspension;
(3) polyacrylonitrile and polymethyl methacrylate are added into suspension obtained by step (2), continues magnetic agitation,
Sufficiently dissolution, obtains sticky black ESD spinning precursor solution;
(4) electrostatic spinning presoma liquid relief obtained by step (3) is subjected to Static Spinning with electrostatic spinning machine into flat needle applicator
Silk, gained nanofiber are collected with glass plate;
(5) after the nanofiber drying collected to step (4), collection nanofiber, which is placed in inert gas, to be carbonized, and obtains
The SnTe/C material of self-supporting.
2. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that step
(1) in, SnCl2·2H2The mass fraction of O in the solution is 12.6 ~ 25.88%.
3. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that step
(2) in, the tellurium powder of addition and the amount ratio of n,N-Dimethylformamide are 3 ~ 6 mmol:4 ~ 10ml.
4. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that step
(3) in, the polyacrylonitrile average molecular weight of addition is 150000.
5. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that SnCl2·
2H2O, tellurium powder, polyacrylonitrile, polymethyl methacrylate mass ratio be 3 ~ 6:1 ~ 2:1.6 ~ 5: 0.5 ~ 1.5.
6. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that step
(4) in, spinning parameter are as follows: voltage be 15 ~ 20 kV, micro-injection flow rate pump be 0.2 ~ 0.8 mL/h, syringe needle internal diameter be 0.8 ~
1.2 mm, receiving the distance i.e. spacing of spinning nozzle and receiver board is 15 ~ 22 cm, and spinning instrument internal temperature is 20 ~ 40 DEG C.
7. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that step
(5) dry to be dried in vacuo in, temperature is 60 ~ 110 DEG C.
8. the electrostatic spinning preparation method of self-supporting SnTe/C nanofiber according to claim 1, which is characterized in that step
(5) it in, is carbonized in N2It is carried out under atmosphere, detailed process are as follows: with the heating rate of 2 ~ 5 DEG C/min, be raised to 550 ~ 700 from room temperature
DEG C, 1 ~ 6 h is kept the temperature, is then cooled to room temperature with the rate of temperature fall of 2 ~ 5 DEG C/min.
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