CN108910868A - A method of preparing graphene dendrite on an insulating substrate - Google Patents
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Abstract
The present invention relates to the methods that one kind prepares graphene dendrite on an insulating substrate, belong to technical field of microelectronic material, first clean insulating substrate, dry up;The quartz inner pipe outer wall in CVD tube furnace is placed the substrate into, tubular type stove evacuation is warming up to 200 DEG C~300 DEG C, is passed through hydrogen, and temperature is increased to constant temperature etched substrate surface at 800 DEG C~900 DEG C;It slowly heats up after hydrogen etching, is warming up to 1050~1080 DEG C, constant temperature is passed through carbon source and hydrogen, carries out graphene growth;Growth terminates, and stopping is passed through gas, is first cooled to 700 DEG C~800 DEG C, then Temperature fall is to room temperature.The form of graphene dendrite is dendroid, is distributed on the top of limb, by the intake to methane in preparation method, the control of the conditions such as ratio of methane and hydrogen realizes the structure that graphene is grown to dendritic crystalline on an insulating substrate.Dendritic crystalline graphene has more preferably mechanics and electric property compared to graphene net.
Description
Technical field
The invention belongs to technical field of microelectronic material, and in particular to one kind prepares graphene dendrite on an insulating substrate
Method.
Background technique
It is only monoatomic layer with honeycomb crystal structure made of sp2 hydridization close-packed arrays that graphene, which is as carbon atom,
The two-dimensional material of thickness.Highly directional pyrolysis is by mechanically pulling off by two scientists Geim and Novoselov of Britain within 2004
Graphite (HOPG) forms.Graphene is also the basic unit for constituting other materials, it can be rolled into the fullerene of zero dimension, curling
At one-dimensional carbon nanotube and it is stacked into three-dimensional graphite.The unique structure of graphene determines its unique property.Preferably
Electron mobility can achieve 200000cm to grapheme material at room temperature2/(V·s);High specific surface area;It is hot at room temperature
Conductance is 5000W/ (mK);High transparency, the light transmittance of single graphene is up to 97%;Intensity is high, is intensity highest in the world
Material, the properties such as these excellent excellent electricity, mechanics, optics and calorifics determine graphene in transparent electrode, field effect
The application such as transistor and energy storage device is answered above to have broad prospects.
By the exploration of scientists many years, the preparation method of graphene have been developed it is a variety of, including:Mechanical stripping
Method;Silicon carbide (SiC) epitaxial growth method;Oxidation-reduction method and chemical vapour deposition technique (Chemical vapor
deposition,CVD).Wherein, chemical vapour deposition technique becomes preparation because of the advantages that at low cost, process flow is simple and easy
Large area, an effective way of the graphene of high quality, cardinal principle are to utilize methane (CH4) etc. carbonaceous gas be carbon
Source, carbon source decomposition carries out chemical reaction and generates graphene at high temperature.
Dendrite refers to that is grown under a kind of nonequilibrium state is similar to dendritic crystal habit.Dendrite is very normal in nature
See, for example snowflake is exactly a kind of dendrite, many metals and alloy also will appear the form of dendrite.In Material Field, due to dendrite
Have many advantages, such as bigger specific surface area, conducts electricity very well and cause the concern of researcher in fields such as sensing, catalysis.
Graphene dendrite can regard a kind of derivative of graphene as.So far, also about the report of graphene dendrite
Seldom.Traditional graphene preparation is mostly to prepare based on the graphene of film-form, and the electric property etc. of the graphene of film-form
Aspect is weaker than graphene dendrite.
Chinese patent CM103172058A discloses a kind of preparation method of three-dimensional netted graphene, in graphite oxide solution
Both ends be inserted into electrode, for electrode apply positive negative pulse stuffing voltage after, graphite oxide will undergo positive pulse voltage on same electrode
Absorption, negative pulse voltage restore two processes, and graphite oxide particle is adsorbed and restores in electrode surface, and with tree form to
Upper growth, final accumulation form three-dimensional netted graphene.The patent be using graphite oxide be raw material, by signal generator to
Two end electrodes in graphite oxide apply positive negative pulse stuffing voltage to form graphite oxide reduction adsorption.Original used in this method
Material graphite oxide contains the elements such as hydrogen, oxygen, easily causes sample to pollute due to reacting insufficient during reduction, and oxygen
The structure of graphite is more complicated, and particle layer is thicker, and dendrite is easily packed together, and forms three-dimensional netted graphene.
Chinese patent CN103834993A discloses the preparation method and its graphene dendrite of a kind of graphene dendrite, in oxygen
After the both ends of graphite alkene solution apply square wave electrical signal, by regulating and controlling duty ratio, frequency, voltage, so that the electricity of actual use
Current density oversteps the extreme limit current density, and diffusion overpotential is suddenly poly- to be increased, and electrode nearby will be there is a serious shortage of graphene oxide particle, only
There is the attainable part crystal face of particle to continue to grow up with the dendrite of palpus shape, as graphene dendrite.This method is equally inevitable
Hydrogen, pollution of the impurity elements such as oxygen to graphene dendrite sample.
Chinese patent CN105417525A discloses the preparation method of dendritic crystalline three-dimensional grapheme, in CuSO4,NiSO4With
H2SO4Mixed solution in by working electrode of Cu deposit the lining that Cu cluster or CuNi cluster are deposited with this as graphene dendrite
Bottom cleans nano metal cluster in ultrapure water, filters out and is lyophilized, and the nano metal cluster after freeze-drying is placed in vacuum drying oven, first
Reduction treatment is carried out under atmosphere of hydrogen and experimental temperature, then the mixed gas progress of hydrogen and methane is passed through under experimental temperature
Graphene deposition processes, finally utilized (NH4)2SO4Solution or FeCl3Solution removes alloy substrates to get dendritic crystalline graphite is arrived
Alkene.The substrate of this method effect is metal substrate, needs to utilize chemical reagent for substrate etching in practical applications and utilize
For organic matter secondary transfer to insulating substrate, this method causes the damage and pollution of sample to a certain extent.
Summary of the invention
For above-mentioned problems of the prior art, it is an object of the present invention to provide one kind to make on an insulating substrate
The method of standby graphene dendrite.It is easy to operate using the method for process for preparing graphenes by chemical vapour deposition dendrite, and repeatability
Preferably, excellent graphene dendrite can be prepared.
In order to solve the above technical problems, the technical scheme is that:
A method of preparing graphene dendrite on an insulating substrate, the specific steps are:
1) insulating substrate is cleaned, is dried up;
2) 1) the middle substrate that dries up is put into the quartz inner pipe outer wall in CVD tube furnace, tubular type stove evacuation is warming up to
200 DEG C~300 DEG C, it is passed through hydrogen, temperature is increased to constant temperature etched substrate surface at 800 DEG C~900 DEG C;
3) it slowly heats up after hydrogen etching, is warming up to 1050~1080 DEG C, constant temperature is passed through carbon source and hydrogen, carries out graphite
Alkene growth;
4) growth terminates, and stopping is passed through gas, is first cooled to 700 DEG C~800 DEG C, then Temperature fall to room temperature to get stone
Black alkene dendrite.
Graphene dendrite is prepared in the application on an insulating substrate, and the form of graphene dendrite is dendroid, in limb
Top distribution, graphene is in the surface Si of substrate or SiO2Surface is initially formed ball-type, branch is grown on the top of ball-type, in branch
Grow up to dendroid on dry.The surface of hydrogen etched substrate combines carbon source preferably with substrate, and after methane decomposes, carbon source is in height
It is grown under temperature in substrate surface, after etching, carbon source and hydrogen are passed through simultaneously can be to avoid oxygen remaining in test to reality
The influence tested, and hydrogen can keep the slow decomposition of methane, improve the quality of graphene dendrite.In compared with the prior art
The graphene prepared on an insulating substrate is compared, and the application has prepared the graphene dendrite with dendritic shape, is had more preferable
Mechanics and electric property.Substrate, which is located at the placement location of quartz inner pipe outer wall compared with the prior art in CVD tube furnace, to be had
Better effect can adequately utilize methane, improve the utilization efficiency of methane, the graphene dendrite effect of generation is more preferable.
Preferably, insulating substrate is silicon wafer in the step 1), and the silicon wafer is the silicon chip surface with a thickness of 400-600 μm
For unformed SiO2The silicon wafer of layer, the SiO2Layer with a thickness of 100-400nm, SiO2Layer surface passes through polishing treatment, Si layers of table
Face is without polishing treatment.
It is further preferred that the silicon wafer is the SiO with a thickness of 450-550 μm2Layer with a thickness of 200-350nm.
Preferably, it is cleaned by ultrasonic in the step 1) using chemical, successively uses chemical acetone, second
Pure and mild deionized water is cleaned, and the time of cleaning is 8-12min;The time of cleaning is 9-11min.
Preferably, the vacuum degree pressure in the step 2) in CVD tube furnace is 10-5~10-4mbar。
Preferably, the purity of hydrogen is greater than 99.9% in the step 2), and hydrogen flowing quantity is 15~25sccm.
It is further preferred that hydrogen flowing quantity is 15~20sccm in step 2).
Preferably, the heating rate that 200~300 DEG C are warming up in the step 2) is 8-12 DEG C/min, it is warming up to 800~
900 DEG C of heating rate is 8-12 DEG C/min.
Preferably, the time that hydrogen constant temperature etches in the step 2) is 30~60min.
It is further preferred that the time of hydrogen constant temperature etching is 30~40min.
Preferably, heating rate is 4-6 DEG C/min, constant temperature 30 when increasing temperature in the step 3) to 1050~1080 DEG C
~120min, pressure are identical as the pressure in step 2).It is further preferred that 100~120min of constant temperature in the step 3).
Preferably, the carbon source being passed through in the step 3) is methane, and the purity of methane is greater than 99.9%, and the flow of methane is
15~60sccm;The ratio of the methane and hydrogen that are passed through is 2:3~4:1.
It is further preferred that the flow of methane is 25~40sccm.
Preferably, the rate of temperature fall that 700 DEG C~800 DEG C are cooled in the step 4) is 100~200 DEG C/min.
The graphene grown on an insulating substrate is prepared in the above-mentioned method for preparing graphene dendrite on an insulating substrate
Dendrite.
The above-mentioned graphene dendrite grown on an insulating substrate is preparing the application in microelectronic component.
Beneficial effects of the present invention:
1, experimental implementation is simple, and cost of material is low, and assay reproducibility is good;
2, direct deposition growing on an insulating substrate, shifts without chemical method, may be directly applied to field of electronic devices;
3, the application first carries out hydrogen etching on substrate, improves the structure of substrate surface, forms substrate surface certain
Then defect grows graphene on substrate again, keep the combination of substrate and graphene more close,
4, by the intake to methane in preparation method, the control of the conditions such as ratio of methane and hydrogen realizes graphite
Alkene is grown to the structure of dendritic crystalline on an insulating substrate;
5, the substrate of the application is located at quartz inner pipe outer wall in CVD tube furnace, and inventor has found in quartz inner pipe outer wall carbon
Source is easier to carry out depositing, and can obtain preferable deposition effect, it is easier to grow dendrite.
6, original method selection graphene oxide raw material for preparing graphene dendrite, graphene oxide structure is complex,
Three-dimensional netted graphene easy to form, dendritic crystalline graphene have more preferably mechanics and electric property compared to graphene net.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the experimental principle figure based on process for preparing graphenes by chemical vapour deposition dendrite;
Fig. 2 is the scanning electron microscope image of silicon substrate side graphene dendrite;
Fig. 3 is the SiO on silicon substrate2With the Raman spectral image of the surface Si graphene dendrite;
Fig. 4 is the Scanning Electron MIcrosope image of surface of silicon graphene dendrite;
Fig. 5 is the selected diffraction spot image of silicon substrate graphene dendrite sample.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
All appts in the present invention, raw material are commercial product
Below with reference to embodiment, the present invention is further described
As shown in Figure 1 it is the schematic illustration for preparing graphene dendrite on an insulating substrate of the application, substrate is placed
In tube furnace quartz inner pipe outer wall, methane and hydrogen and mixed gas enter in tube furnace, and methane decomposes, and Carbon deposition is in substrate
On, it is grown to serve as graphene dendrite.
Embodiment 1
A method of graphene dendrite being prepared, on an insulating substrate with SiO2For/Si substrate, including steps are as follows:
It (1) will be with a thickness of 500 μm of SiO2The ultrasonic cleaning of/Si substrate, drying.
(2) silicon substrate dried up in (1) is put into quartz inner pipe outer wall in CVD tube furnace, tubular type stove evacuation, vacuum pressure
Power is 10-5Mbar is warming up to 300 DEG C, 10 DEG C/min of heating rate, closes molecular pump;800 DEG C, constant temperature 30min are warming up to, is led to
Enter hydrogen and carries out hydrogen etching, hydrogen flowing quantity 15sccm;1050 DEG C are to slowly warm up to, heating rate is 5 DEG C/min, is passed through first
Alkane, the flow of methane are 30sccm, constant temperature 60min.Graphene branch can be obtained in the constantly decomposition of methane, deposition process
It is brilliant.
(3) after growing, tube furnace furnace box is slided, is naturally cooling to 600 DEG C, rate of temperature fall is 150 DEG C/min, later
It is slowly dropped to room temperature.
The pattern of graphene dendrite prepared by embodiment 1 in the side of substrate is dendroid, the SiO of substrate2Surface does not have
Dendritic crystalline graphene growth.It is illustrated in figure 2 pattern of the graphene dendrite in the side of substrate of the preparation of embodiment 1.
Embodiment 2
A method of graphene dendrite being prepared, on an insulating substrate with SiO2For/Si substrate, including steps are as follows:
It (1) will be with a thickness of 500 μm of SiO2The ultrasonic cleaning of/Si substrate, drying.
(2) silicon substrate dried up in (1) is put into quartz inner pipe outer wall in CVD tube furnace, tubular type stove evacuation, vacuum pressure
Power is 10-5Mbar is warming up to 300 DEG C, 10 DEG C/min of heating rate, closes molecular pump;800 DEG C, constant temperature 30min are warming up to, is led to
Enter hydrogen and carries out hydrogen etching, hydrogen flowing quantity 25sccm;1050 DEG C are to slowly warm up to, heating rate is 5 DEG C/min, is passed through first
Alkane, the flow of methane are 15sccm, constant temperature 30min.Graphene branch can be obtained in the constantly decomposition of methane, deposition process
It is brilliant.
After growth, tube furnace furnace box is slided, is naturally cooling to 600 DEG C, rate of temperature fall is 150 DEG C/min, Zhi Houhuan
Slowly it is down to room temperature.
As shown in figure 3, SiO of the graphene dendrite being prepared under conditions of embodiment 2 in substrate2The pattern on surface is
Spherical shape, it is spherical to grow dendrite arm above.In the side of substrate without dendritic growth.
Embodiment 3
A method of graphene dendrite being prepared, on an insulating substrate with SiO2For/Si substrate, including steps are as follows:
It (1) will be with a thickness of 500 μm of SiO2The ultrasonic cleaning of/Si substrate, drying.
(2) silicon substrate dried up in (1) is put into quartz inner pipe outer wall in CVD tube furnace, tubular type stove evacuation, vacuum pressure
Power is 10-5Mbar is warming up to 300 DEG C, 10 DEG C/min of heating rate, closes molecular pump;800 DEG C, constant temperature 30min are warming up to, is led to
Enter hydrogen and carries out hydrogen etching, hydrogen flowing quantity 15sccm;1050 DEG C are to slowly warm up to, heating rate is 5 DEG C/min, is passed through first
Alkane, the flow of methane are 25sccm, constant temperature 120min.Graphene can be obtained in the constantly decomposition of methane, deposition process
Dendrite.
(3) after growing, tube furnace furnace box is slided, is naturally cooling to 600 DEG C, rate of temperature fall is 150 DEG C/min, later
It is slowly dropped to room temperature.
SiO of the graphene dendrite being prepared under conditions of embodiment 3 in substrate2The pattern on surface is spherical shape, spherical
Dendrite arm is grown above.The pattern on the surface Si of substrate is spherical shape, spherical to grow dendrite arm above.It is in the side dendrite morphology of substrate
Dendroid.It is illustrated in figure 4 the pattern on the surface Si of the substrate of embodiment 3.
It is illustrated in figure 4 the Raman spectral image of graphene dendrite in insulating substrate prepared by embodiment 3, by can in figure
To obtain in SiO2There are three characteristic peaks of graphene with the sample Raman spectrum of Si, further proves that the substance is graphite
Alkene.
Embodiment 4
A method of graphene dendrite being prepared, on an insulating substrate with SiO2For/Si substrate, including steps are as follows:
It (1) will be with a thickness of 500 μm of SiO2The ultrasonic cleaning of/Si substrate, drying.
(2) silicon substrate dried up in (1) is put into quartz inner pipe outer wall in CVD tube furnace, tubular type stove evacuation, vacuum pressure
Power is 10-5Mbar is warming up to 300 DEG C, 10 DEG C/min of heating rate, closes molecular pump;800 DEG C, constant temperature 30min are warming up to, is led to
Enter hydrogen and carries out hydrogen etching, hydrogen flowing quantity 15sccm;1050 DEG C are to slowly warm up to, heating rate is 5 DEG C/min, is passed through first
Alkane, the flow of methane are 45sccm, constant temperature 40min.Graphene branch can be obtained in the constantly decomposition of methane, deposition process
It is brilliant.
(3) after growing, tube furnace furnace box is slided, is naturally cooling to 600 DEG C, rate of temperature fall is 150 DEG C/min, later
It is slowly dropped to room temperature.
Pattern of the prepared graphene dendrite in the side of substrate is dendroid, the SiO of substrate under this condition2Surface does not have
There is the growth of spherical graphite alkene.
Embodiment 5
A method of graphene dendrite being prepared, on an insulating substrate with SiO2For/Si substrate, including steps are as follows:
It (1) will be with a thickness of 500 μm of SiO2The ultrasonic cleaning of/Si substrate, drying.
(2) silicon substrate dried up in (1) is put into quartz inner pipe outer wall in CVD tube furnace, tubular type stove evacuation, vacuum pressure
Power is 10-5Mbar is warming up to 300 DEG C, 10 DEG C/min of heating rate, closes molecular pump;800 DEG C, constant temperature 30min are warming up to, is led to
Enter hydrogen and carries out hydrogen etching, hydrogen flowing quantity 15sccm;1050 DEG C are to slowly warm up to, heating rate is 5 DEG C/min, is passed through first
Alkane, the flow of methane are 60sccm, constant temperature 60min.Graphene branch can be obtained in the constantly decomposition of methane, deposition process
It is brilliant.
(3) after growing, tube furnace furnace box is slided, is naturally cooling to 600 DEG C, rate of temperature fall is 150 DEG C/min, later
It is slowly dropped to room temperature.
SiO of the prepared graphene dendrite in substrate under conditions of embodiment 52The pattern on surface is spherical, in spherical shape
Face grows dendrite arm.In the side of substrate without dendritic growth.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. the method that one kind prepares graphene dendrite on an insulating substrate, it is characterised in that:The specific steps are:
1) insulating substrate is cleaned, is dried up;
2) 1) the middle substrate that dries up is put into CVD tube furnace, tubular type stove evacuation is warming up to 200 DEG C~300 DEG C, is passed through hydrogen
Gas, temperature are increased to constant temperature etched substrate surface at 800 DEG C~900 DEG C;
3) it slowly heats up after hydrogen etching, is warming up to 1050~1080 DEG C, constant temperature is passed through carbon source and hydrogen, and it is raw to carry out graphene
It is long;
4) growth terminates, and stopping is passed through gas, is first cooled to 700 DEG C~800 DEG C, then Temperature fall to room temperature to get graphene
Dendrite.
2. according to the method described in claim 1, it is characterized in that:Insulating substrate is silicon wafer, the silicon wafer in the step 1)
It is with a thickness of 400-600 μm, silicon chip surface is unformed SiO2The silicon wafer of layer, the SiO2Layer with a thickness of 100-400nm,
SiO2Layer surface passes through polishing treatment, and Si layer surface is without polishing treatment;
Preferably, the silicon wafer is the SiO with a thickness of 450-550 μm2Layer with a thickness of 200-350nm.
3. according to the method described in claim 1, it is characterized in that:Ultrasound is carried out clearly using chemical in the step 1)
It washes, is successively cleaned with chemical acetone, ethyl alcohol and deionized water, the time of cleaning is 8-12min.
4. according to the method described in claim 1, it is characterized in that:Vacuum degree pressure in the step 2) in CVD tube furnace
It is 10-5~10-4mbar。
5. according to the method described in claim 1, it is characterized in that:200~300 DEG C of heating speed is warming up in the step 2)
Rate is 8-12 DEG C/min, and the heating rate for being warming up to 800~900 DEG C is 8-12 DEG C/min;The purity of hydrogen in the step 2)
Greater than 99.9%, hydrogen flowing quantity is 15~25sccm;The time that constant temperature etches in the step 2) is 30~60min;
Preferably, hydrogen flowing quantity is 15~20sccm in the step 2);
Preferably, the time that constant temperature etches in the step 2) is 30~40min.
6. according to the method described in claim 1, it is characterized in that:When increasing temperature in the step 3) to 1050~1080 DEG C
Heating rate is 4-6 DEG C/min, constant temperature 30min~120min, and pressure is identical as the pressure in step 2);
Preferably, 100~120min of constant temperature in the step 3).
7. according to the method described in claim 1, it is characterized in that:The carbon source being passed through in the step 3) is methane, methane
Purity is greater than 99.9%, and the flow of methane is 15~60sccm;The ratio of the methane and hydrogen that are passed through is 2:3~4:1;
Preferably, the flow of methane is 25~40sccm in the step 3).
8. according to the method described in claim 1, it is characterized in that:700 DEG C~800 DEG C of cooling is cooled in the step 4)
Rate is 100~200 DEG C/min.
It is given birth on an insulating substrate 9. the method for preparing graphene dendrite described in claim 1-8 on an insulating substrate is prepared
Long graphene dendrite.
10. the graphene dendrite as claimed in claim 9 grown on an insulating substrate is preparing the application in microelectronic component.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110176582A (en) * | 2019-05-10 | 2019-08-27 | 天津大学 | Preparation method of dendritic graphene/carbon nanotube composite structure |
CN114105491A (en) * | 2021-11-22 | 2022-03-01 | 广东墨睿科技有限公司 | Preparation method and application of graphene water condensation device |
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2018
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110176582A (en) * | 2019-05-10 | 2019-08-27 | 天津大学 | Preparation method of dendritic graphene/carbon nanotube composite structure |
CN110176582B (en) * | 2019-05-10 | 2022-04-01 | 天津大学 | Preparation method of dendritic graphene/carbon nanotube composite structure |
CN114105491A (en) * | 2021-11-22 | 2022-03-01 | 广东墨睿科技有限公司 | Preparation method and application of graphene water condensation device |
CN114105491B (en) * | 2021-11-22 | 2022-07-12 | 广东墨睿科技有限公司 | Preparation method and application of graphene water condensation device |
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