CN107253709A - A kind of lignite derives the preparation method and application of carbon material - Google Patents
A kind of lignite derives the preparation method and application of carbon material Download PDFInfo
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- CN107253709A CN107253709A CN201710404868.1A CN201710404868A CN107253709A CN 107253709 A CN107253709 A CN 107253709A CN 201710404868 A CN201710404868 A CN 201710404868A CN 107253709 A CN107253709 A CN 107253709A
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- lignite
- carbon material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
Derive the preparation method of carbon material and its in DSSC to the application in electrode the present invention relates to a kind of lignite, belong to area of solar cell.A kind of lignite derives under the preparation method of carbon material, inert atmosphere, and lignite particle is calcined at least 1.5h in 700~800 DEG C, obtains lignite and derives carbon material.Preparation method cost of the present invention to electrode is low, it is environment-friendly, it is simple to operate, stability is good, photoelectric transformation efficiency is high, and electric conductivity and catalytic activity are very well, and the electricity conversion for being assembled into DSSC is higher, it is suitable with the electricity conversion of platinum electrode, it is a kind of alternative materials of very promising DSSC to electrode.
Description
Technical field
Derive the preparation method of carbon material and its in DSSC to electrode the present invention relates to a kind of lignite
In application, belong to area of solar cell.
Background technology
DSSC, because it has simple preparation technology, relatively low cost of manufacture and to environment friend
Good the characteristics of, have broad application prospects.Being remained in that most to electrode based on Pt nano materials that current tradition is used
The record of high electricity conversion.But its reserves is limited, involves great expense, in addition, Pt is easily corroded from an electrolyte.Therefore having must
Find the elctro-catalyst for substituting Pt.Not only there is good electric conductivity as electrode material, meanwhile, there is certain catalysis
Ability.
The content of the invention
A kind of cost of present invention offer is low, environment-friendly, simple to operate, and photoelectric transformation efficiency is high, and stability is good
Lignite derives the preparation method of carbon material and its in DSSC to the application in electrode.
The present invention is prepared for lignite using green route and derives carbon material, during which without using other poisonous and harmful presomas,
Dopant and activator, but by the use of the abundant intrinsic metal of lignite itself as catalytic active center, catalyzed graphitization carbon
Formed, so as to strengthen electric conductivity and catalytic activity.
A kind of lignite derives under the preparation method of carbon material, inert atmosphere, and lignite particle is fired in 700~800 DEG C
Few 1.5h, obtains lignite and derives carbon material.
Inert atmosphere of the present invention can be provided by inert gas, such as high-purity argon gas or nitrogen.
Calcine technology of the present invention can be carried out in calciner disclosed in this area, such as tube furnace.
Further, the calcination time is 1.5~3h.
A preferred technical scheme of the invention is:Under inert atmosphere, by the temperature programming of lignite particle to 700~800 DEG C
And at least 1.5h is calcined in 700~800 DEG C, room temperature is down to naturally afterwards, is obtained lignite and is derived carbon material,
Wherein, described program, which heats up, is:400 DEG C, heating rate are raised to by room temperature:5℃/min;Again 800 are raised to by 400 DEG C
DEG C, heating rate:2℃/m in.
Further, the lignite particle is made as follows:
1) bulk lignite is ground with coffee machine, ground 2~3 times, each milling time 2min;Ball grinder is put it into again
Middle 1~3h of ball milling;200 mesh sieves are crossed, 100~120 DEG C is placed in vacuum drying chamber and is dried;
2) by step 1) obtained by lignite be placed in spheroidal graphite tank, add stainless shot, in glove box be full of inert gas,
Packaged tank body, 20~24h of ball milling;The good lignite powder of ball milling is utilized into soaked in absolute ethyl alcohol 2~3 times, supernatant liquid is discarded,
Lower sediment thing is dried in baking oven.
Preferably, step 2) in, the following lignite of 200 mesh is 1~2g with stainless shot amount ratio:25~50g, stainless shot
A diameter of 1~1.2cm;Inert gas is high-purity argon gas;Drum's speed of rotation is set to 400~500 revs/min;The good lignite of ball milling
Powder is 1~2g with absolute ethyl alcohol amount ratio:35~50mL;Oven temperature is set to 40~80 DEG C.
The step of preparation method that lignite of the present invention derives carbon material includes post processing, gained lignite after calcining is spread out
After raw carbon material is 1.5~2.5mol/L HCl ultrasonically treated using concentration, suction filtration is washed, and is dried.
Further, the HCl amount ratios that gained lignite derives carbon material with concentration is 1.5~2.5mol/L after the calcining
For 100~120mg:35~50mL.
It is a further object of the present invention to provide the lignite derivative carbon material as made from the above method and its in dye sensitization too
Application in positive energy counter electrode of battery.
A kind of DSSC is described that electrode is made as follows to electrode:The above method will be utilized
Obtained lignite derives carbon material with after isopropanol mixing and ball milling 4h, mixed liquor obtained by ball milling is sprayed on electro-conductive glass, does
It is dry, produce, wherein, it is 60~80mg that lignite, which derives carbon material with isopropanol amount ratio,:5~8mL.
Further, it is 3~5 μm in the thickness of conductive glass surface to electrode that the lignite, which derives carbon material particles thing,.
Beneficial effects of the present invention are:The lignite age is young, with moisture is high, oxygen content is high, hetero atom is abundant and is rich in
The characteristics of aliphatic structure.But young lignite poorly conductive, it is necessary to the conductive capability of its own is improved through Overheating Treatment, and
The hetero atoms such as Si, Ca, Co, the Sn having inside lignite have catalytic action to being pyrolyzed and gasifying, and can improve graphitized carbon
Conversion ratio.The present invention is prepared for lignite using green route and derives carbon material, the intrinsic metal enriched by the use of lignite itself as
Catalytic active center, the formation of catalyzed graphitization carbon, so as to strengthen electric conductivity and catalytic activity.System of the present invention to electrode
Preparation Method cost is low, environment-friendly, simple to operate, and stability is good, and photoelectric transformation efficiency is high, and electric conductivity and catalytic activity are very
Good, the electricity conversion for being assembled into DSSC is higher, suitable with the electricity conversion of platinum electrode, is one
Plant alternative materials of the very promising DSSC to electrode.
Brief description of the drawings
((a), (b), (c) are the surface picture under different resolution to the SEM figures that Fig. 1 is Coal-800, and (d) shines for section
Piece);
Fig. 2 (a) and (b) are respectively Coal and Coal-800 powder x-ray diffraction and infrared spectrogram;
Fig. 3 (a) and (b) are respectively Coal-800 and Coal-800-HCl TEM figures;
Fig. 4 for DSSC I-V curve (be respectively to electrode Pt electrodes, Coal through 800 DEG C calcine after
Product, Coal calcined through 800 DEG C after product again by 2mol/L HCl processing, light anode is TiO2);
Fig. 5 (a) for DSSC CV curves (working electrode be respectively Pt electrodes, Coal-800,
Coal-800-HCl, reference electrode is Ag/AgCl electrodes, is platinum electrode to electrode);(b) cyclic voltammetric for being Coal-800
Stability curve (the scanning number of turns is 100 circles).
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments, is conventional method unless otherwise specified;The reagent and material, such as
Without specified otherwise, commercially obtain.
1) bulk lignite is ground with coffee machine in advance, grinds 2 times (2min/ times), then put it into ball milling in ball grinder
1h, from the sieve of 200 mesh, is placed in 120 DEG C of dry water removals in vacuum drying chamber.
2) 2g lignite (below 200 mesh) is taken, is placed in spheroidal graphite tank, 50g stainless shots (diameter 1cm) are added, in glove box
In be full of high-purity argon gas, packaged tank body, ball milling 24h (500 revs/min);The good lignite powder of ball milling is placed in 100mL beakers
In, add 50mL soaked in absolute ethyl alcohol 3 times, remove soluble impurity, discard supernatant liquid, by lower sediment thing 60 in baking oven
DEG C drying.
3) lignite powder after processing is put into tube furnace, under nitrogen atmosphere calcine, respectively 600 DEG C, 700 DEG C,
High temperature pyrolysis 2h under the conditions of 800 DEG C,
Specially:Lignite powder after processing is put into tube furnace, in making temperature be raised to 400 by room temperature under nitrogen atmosphere
DEG C, heating rate:5℃/min;It is raised to 600 DEG C, 700 DEG C or 800 DEG C, heating rate respectively by 400 DEG C again:2℃/min;Finally
The Temperature fall after 600 DEG C, 700 DEG C or 800 DEG C holding 2h, products obtained therefrom is designated as Coal-600, Coal-700, Coal- respectively
800。
Coal-800 catalyst after being pyrolyzed through 800 DEG C with 2mol/L HCl it is ultrasonically treated after, suction filtration, with deionized water and
Absolute ethyl alcohol is washed till neutrality, and 60 DEG C are dried in vacuum overnight, and products obtained therefrom is designated as Coal-800-HCl.
4) by step 3) obtained four kinds of materials are scattered with isopropanol respectively, and ball milling 4h is sprayed on electro-conductive glass respectively,
3 μm of coating thickness, is then put into 200 DEG C of heating 2h in baking oven, obtains lignite and derives carbon material as dye sensitization of solar electricity
Pond is to electrode:Coal-600 to electrode, Coal-700 to electrode, Coal-800 to electrode, Coal-800-HCl to electrode.Finally
Will to electrode respectively with TiO2Light anode is assembled into DSSC, tests the electricity conversion of battery, and with
Pt is contrasted to the electricity conversion of electrode.
Table 1 is photovoltaic parameters of the Coal-600 to electrode and the Coal-700 DSSC constituted to electrode
Table 2 is the dye sensitization of solar that Coal-800 is constituted to electrode, Coal-800-HCl to electrode and Pt to electrode
The photovoltaic parameter of battery;
Table 3 is Coal and Coal-800 EDS elementary analyses;
Table 3 is Coal and Coal-800 EDS elementary analyses, can therefrom be drawn, N is not present in the block surface such as lignite
Element;C content is drastically reduced in Coal-800 samples, is because of Si migration of element after calcining to surface, and enriching section O members
Element, causes C content accordingly to reduce;Sample contains micro Co and partial Sn and substantial amounts of Si;Si content phases before and after calcining
Difference is very big, is that Si, which is migrated to block outer surface, to be exposed because substantial amounts of Si is present in after bulk inner, burning.
Performance evaluation
((a), (b), (c) are the surface picture under different resolution to the SEM figures that Fig. 1 is Coal-800, and (d) shines for section
Piece), from surface picture, it is seen that coal particle size is larger, all in submicron order, and pore structure is than larger, this macroporous structure
Be conducive to the infiltration of electrolyte.From cross-section photograph it can be seen that, be about 3 μm to thickness of electrode;
Fig. 2 is Coal and Coal-800 powder x-ray diffraction and infrared spectrogram, 700-900cm-1Absorbed for aromatic hydrocarbon
The absorption intensity change of peak, raw coal and pyrolyzing coal in this place is little, illustrates that fragrant hydrocarbon structure is more stable;1000cm-1It is nearby
Mineral absorption peak, at relatively high temperatures, mineral matter is more stable, and change at peak is smaller at this.Absworption peak is in 1100-
1500cm-1In the range of, main reflection C=O stretching vibrations;1600cm-1It is nearby the carboxyl in raw coal, after pyrolytic gasification, with
CO2Form is run away disappearance;2900cm-1It is respectively nearby-CH3With-CH2- stretching vibration absworption peak, after pyrolysis, the position
Absorption intensity significantly reduce, illustrate in gasification, the group such as methyl and methylene is broken;3400cm-1It is nearby-OH
Absworption peak, is pyrolyzed postpeak molded breadth, and remitted its fury illustrates the reduction of oxy radical content;3696cm-1For the O-H vibrations in lignite
Or free-OH, this peak disappears after pyrolysis, also illustrate that the reduction of oxy radical content;
Fig. 3 schemes for Coal-800 and Coal-800-HCl TEM, it can be seen that after pickling, not washing off
Foreign metal and mineral matter in Coal-800, illustrate that Coal-800 forms onion clad structure, very stable, are difficult to remove.
Fig. 4 is the I-V curve of DSSC, is drawn a conclusion by Fig. 4:The dye sensitization prepared with the method
Solar cell is to the battery efficiency of electrode and Pt electrodes closely (electricity conversion:Pt 8.24%, Coal-800-
HCl 8.23%), and the method preparation is simple, it is with low cost.
Fig. 5 left figures are the CV curves of DSSC;Right figure is bent for Coal-800 cyclic voltammetric stability
Line, therefrom draws a conclusion:Coal-800 and Coal-800-HCl are poor with close iodine reduction potential compared with Pt, bigger
After current density, the circle of scanning 100, still with good cyclic voltammetric stability.
The assembling process of DSSC:
1. by TiO2Slurry (granular size about 20nm) is printed onto on FTO electro-conductive glass that (effective area is 4mm × 4mm, thick
Spend for 14 μm), 325 DEG C of burnings 15min, 375 DEG C of burnings 15min, 450 DEG C of burnings 25min, 500 DEG C of burning 30min, cooling in Muffle furnace
To room temperature, roasting light anode is then placed in dyestuff (main component N719, acetonitrile:The tert-butyl group=1:1) 45 DEG C of immersions in
120 minutes;
2. by TiO2Light anode is taken out from dye tank, with alcohol flushing, N2Rifle is dried up, then with obtained to electrode pair
Connect, with clamp, be assembled into battery, liquid electrolyte (is I-/I3 -Electrolyte) test when along conductive glass
Glass is added dropwise.
3. wherein, as a comparison:Pt electrodes are prepared with the method for magnetron sputtering, Pt is splashed on FTO electro-conductive glass, its
Thickness is 200nm.
The I-V curve of DSSC being made 1. digital sourcemeter is tested using following apparatus
(Keithley2601, Keithley instrument company of the U.S.) 2. solar simulator (xenon lamp, lighting programmers are AM1.5,100mW/
cm2) (PEC-L15, Japanese Peccell companies) 3. standard silion cell (be used for calibration light source) (BS-520, Japanese Sharp company).
Claims (9)
1. a kind of lignite derives the preparation method of carbon material, it is characterised in that:Under inert atmosphere, by lignite particle in 700~800
DEG C calcining at least 1.5h, obtain lignite derive carbon material.
2. according to the method described in claim 1, it is characterised in that:The calcination time is 1.5~3h.
3. method according to claim 1 or 2, it is characterised in that:Under inert atmosphere, by the temperature programming of lignite particle extremely
700~800 DEG C and in 700~800 DEG C calcine at least 1.5h, be down to room temperature naturally afterwards, obtain lignite derivative carbon material,
Wherein, described program, which heats up, is:400 DEG C, heating rate are raised to by room temperature:5℃/min;800 DEG C are raised to by 400 DEG C again,
Heating rate:2℃/min.
4. according to the method described in claim 1, it is characterised in that:The lignite particle is made as follows:
1) bulk lignite is ground with coffee machine, ground 2~3 times, each milling time 2min;Ball in ball grinder is put it into again
Grind 1~3h;200 mesh sieves are crossed, 100~120 DEG C is placed in vacuum drying chamber and is dried;
2) by step 1) obtained by lignite be placed in spheroidal graphite tank, add stainless shot, in glove box be full of inert gas, encapsulation
Good tank body, 20~24h of ball milling;The good lignite powder of ball milling is utilized into soaked in absolute ethyl alcohol 2~3 times, supernatant liquid is discarded, by under
Layer sediment is dried in baking oven.
5. method according to claim 4, it is characterised in that:Step 2) in, the following lignite of 200 mesh and stainless shot consumption
Than for 1~2g:25~50g, a diameter of 1~1.2cm of stainless shot;Inert gas is high-purity argon gas;Drum's speed of rotation is set to
400~500 revs/min;The good lignite powder of ball milling is 1~2g with absolute ethyl alcohol amount ratio:35~50mL;Oven temperature is set to
40~80 DEG C.
6. according to the method described in claim 1, it is characterised in that:The step of material includes post processing, by institute after calcining
Lignite derived carbon material use concentration be 1.5~2.5mol/L HCl it is ultrasonically treated after, suction filtration, wash, dry.
7. method according to claim 6, it is characterised in that:Gained lignite derivative carbon material is with concentration after the calcining
1.5~2.5mol/L HCl amount ratios are 100~120mg:35~50mL.
8. a kind of DSSC is to electrode, it is characterised in that:It is described that electrode is made as follows:It will utilize
Lignite derives after carbon material and isopropanol mixing and ball milling 4h made from any one of claim 1~7 methods described, by obtained by ball milling
Mixed liquor is sprayed on electro-conductive glass, is dried, is produced,
Wherein, it is 60~80mg that lignite, which derives carbon material with isopropanol amount ratio,:5~8mL.
9. it is according to claim 8 to electrode, it is characterised in that:The lignite derives carbon material particles thing is leading to electrode
The thickness of electric glass surface is 3~5 μm.
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