CN107253709B - A kind of preparation method and application of the derivative carbon material of lignite - Google Patents
A kind of preparation method and application of the derivative carbon material of lignite Download PDFInfo
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- CN107253709B CN107253709B CN201710404868.1A CN201710404868A CN107253709B CN 107253709 B CN107253709 B CN 107253709B CN 201710404868 A CN201710404868 A CN 201710404868A CN 107253709 B CN107253709 B CN 107253709B
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- lignite
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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
The present invention relates to a kind of preparation method of the derivative carbon material of lignite and its in dye-sensitized solar cells to the application in electrode, belong to area of solar cell.A kind of preparation method of the derivative carbon material of lignite under inert atmosphere, by lignite particle in 700~800 DEG C of calcining at least 1.5h, obtains lignite derivative carbon material.It is of the present invention at low cost to the preparation method of electrode, it is environmental-friendly, it is easy to operate, stability is good, photoelectric conversion efficiency is high, and electric conductivity and catalytic activity are fine, and the incident photon-to-electron conversion efficiency for being assembled into dye-sensitized solar cells is higher, it is suitable with the incident photon-to-electron conversion efficiency of platinum electrode, it is a kind of alternative materials of very promising dye-sensitized solar cells to electrode.
Description
Technical field
The present invention relates to a kind of preparation method of the derivative carbon material of lignite and its in dye-sensitized solar cells to electrode
In application, belong to area of solar cell.
Background technique
Dye-sensitized solar cells, because it is with simple preparation process, lower cost of manufacture and to environment friend
Good feature, has broad application prospects.Electrode is still maintained most based on Pt nano material that tradition uses at present
The record of high incident photon-to-electron conversion efficiency.But its reserves is limited, involves great expense, in addition, Pt is easy to be corroded from an electrolyte.Therefore having must
Find the elctro-catalyst of substitution Pt.Not only there is good electric conductivity as electrode material, meanwhile, there is certain catalysis
Ability.
Summary of the invention
The present invention provides a kind of at low cost, environmental-friendly, easy to operate, photoelectric conversion efficiency height, and stability is good
Lignite derives the preparation method of carbon material and its in dye-sensitized solar cells to the application in electrode.
The present invention is prepared for the derivative carbon material of lignite using green route, during which without using other poisonous and harmful presomas,
Dopant and activator, but using lignite itself intrinsic metal abundant as catalytic active center, catalyzed graphitization carbon
It is formed, to enhance electric conductivity and catalytic activity.
Under inert atmosphere, lignite particle is fired in 700~800 DEG C for a kind of preparation method of the derivative carbon material of lignite
Few 1.5h obtains the derivative carbon material of lignite.
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 carry out in calciner disclosed in this field, such as tube furnace.
Further, the calcination time is 1.5~3h.
A preferred technical solution of the invention are as follows: under inert atmosphere, by the temperature programming of lignite particle to 700~800 DEG C
And in 700~800 DEG C of calcining at least 1.5h, it is down to room temperature naturally afterwards, obtains the derivative carbon material of lignite,
Wherein, described program heats up are as follows: is raised to 400 DEG C by room temperature, heating rate: 5 DEG C/min；800 are raised to by 400 DEG C again
DEG C, heating rate: 2 DEG C/m in.
Further, the lignite particle is made as follows:
1) bulk lignite is ground with coffee machine, is ground 2~3 times, each milling time 2min；Ball grinder is put it into again
Middle 1~3h of ball milling；200 meshes are crossed, 100~120 DEG C is placed in a vacuum drying oven and is dried；
2) the resulting lignite of step 1) is placed in spheroidal graphite tank, stainless shot is added, inert gas is full of in glove box,
Packaged tank body, ball milling 20~for 24 hours；The good lignite powder of ball milling is utilized soaked in absolute ethyl alcohol 2~3 times, supernatant liquid is discarded,
Lower sediment thing is dried in baking oven.
Preferably, in step 2), the following lignite of 200 mesh and stainless shot amount ratio are 1~2g:25~50g, stainless shot
Diameter is 1~1.2cm；Inert gas is high-purity argon gas；Drum's speed of rotation is set as 400~500 revs/min；The good lignite of ball milling
Powder and dehydrated alcohol amount ratio are 1~2g:35~50mL；Oven temperature is set as 40~80 DEG C.
The preparation method of the derivative carbon material of lignite of the present invention includes the steps that post-processing, and gained lignite after calcining is spread out
Raw carbon material is after 1.5~2.5mol/L HCl is ultrasonically treated, to filter using concentration, is washed, dry.
Further, the HCl amount ratio that the derivative carbon material of gained lignite and concentration are 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 derivative carbon material of lignite prepared by the above method and its dye sensitization too
Application in positive energy counter electrode of battery.
A kind of dye-sensitized solar cells is described that electrode is made as follows: will to utilize the above method to electrode
Mixed liquor obtained by ball milling is sprayed on electro-conductive glass, is done with after isopropanol mixing and ball milling 4h by the derivative carbon material of lignite obtained
Dry to get the derivative carbon material of, wherein lignite and isopropanol amount ratio is 60~80mg:5~8mL.
Further, the derivative carbon material particles object of the lignite to electrode in conductive glass surface with a thickness of 3~5 μm.
The invention has the benefit that the lignite age is young, there is high moisture, oxygen content height, hetero atom to enrich and be 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 pyrolysis and gasification, and graphitized carbon can be improved
Conversion ratio.The present invention is prepared for the derivative carbon material of lignite using green route, using lignite itself intrinsic metal abundant as
Catalytic active center, the formation of catalyzed graphitization carbon, to enhance electric conductivity and catalytic activity.System of the present invention to electrode
Preparation Method is at low cost, environmental-friendly, easy to operate, and stability is good, and photoelectric conversion efficiency is high, and electric conductivity and catalytic activity are very
Good, the incident photon-to-electron conversion efficiency for being assembled into dye-sensitized solar cells is higher, suitable with the incident photon-to-electron conversion efficiency of platinum electrode, is one
Alternative materials of the very promising dye-sensitized solar cells of kind to electrode.
Detailed description of the invention
((a), (b), (c) are the surface picture under different resolution to the SEM figure that Fig. 1 is Coal-800, (d) are shone for section
Piece)；
Fig. 2 (a) and (b) are respectively the powder x-ray diffraction and infrared spectrogram of Coal and Coal-800；
Fig. 3 (a) and (b) are respectively the TEM figure of Coal-800 and Coal-800-HCl；
Fig. 4 is that the I-V curve of dye-sensitized solar cells (is respectively Pt electrode, Coal after 800 DEG C of calcinings to electrode
Product, Coal through 800 DEG C calcining after using 2mol/L HCl handle product, light anode is TiO2)；
Fig. 5 (a) be dye-sensitized solar cells CV curve (working electrode be respectively Pt electrode, Coal-800,
Coal-800-HCl, reference electrode are Ag/AgCl electrode, are platinum electrode to electrode)；(b) cyclic voltammetric for being Coal-800
Stability curve (scanning circle number is 100 circles).
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
1) bulk lignite is ground in advance with coffee machine, grinds 2 times (2min/ times), then put it into ball milling in ball grinder
1h selects the sieve of 200 mesh, is placed in a vacuum drying oven 120 DEG C of dry water removals.
2) 2g lignite (below 200 mesh) are taken, are placed in spheroidal graphite tank, are added 50g stainless shot (diameter 1cm), in glove box
In be full of high-purity argon gas, packaged tank body, ball milling is for 24 hours (500 revs/min)；The good lignite powder of ball milling is placed in 100mL beaker
In, it is added 50mL soaked in absolute ethyl alcohol 3 times, removes soluble impurity, discard supernatant liquid, by lower sediment thing 60 in baking oven
DEG C drying.
3) will treated that lignite powder is put into tube furnace, calcined under nitrogen atmosphere, respectively 600 DEG C, 700 DEG C,
High temperature pyrolysis 2h under the conditions of 800 DEG C,
Specifically: by treated, lignite powder is put into tube furnace, so that temperature is raised to 400 by room temperature under nitrogen atmosphere
DEG C, heating rate: 5 DEG C/min；It is raised to 600 DEG C, 700 DEG C or 800 DEG C respectively by 400 DEG C again, heating rate: 2 DEG C/min；Finally
The Temperature fall after 600 DEG C, 700 DEG C or 800 DEG C holding 2h, products obtained therefrom are denoted as Coal-600, Coal-700, Coal- respectively
800。
After Coal-800 catalyst after 800 DEG C of pyrolysis is ultrasonically treated with 2mol/L HCl, filter, with deionized water and
Dehydrated alcohol is washed till neutrality, and 60 DEG C are dried in vacuum overnight, and products obtained therefrom is denoted as Coal-800-HCl.
4) four kinds of materials for obtaining step 3) are dispersed with isopropanol respectively, and ball milling 4h is sprayed on electro-conductive glass respectively,
3 μm of coating thickness, 200 DEG C of heating 2h in baking oven are then put into, obtain the derivative carbon material of lignite 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 dye-sensitized solar cells, tests the incident photon-to-electron conversion efficiency of battery, and with
Pt compares the incident photon-to-electron conversion efficiency of electrode.
Table 1 is photovoltaic parameter of the Coal-600 to electrode and the Coal-700 dye-sensitized solar cells formed to electrode
Table 2 is the dye sensitization of solar that Coal-800 forms electrode, Coal-800-HCl to electrode and Pt to electrode
The photovoltaic parameter of battery；
Table 3 is the EDS elemental analysis of Coal and Coal-800；
Table 3 is the EDS elemental analysis of Coal and Coal-800, and therefrom it can be concluded that, N is not present in the block surfaces such as lignite
Element；C content drastically reduces in Coal-800 sample, is because of Si migration of element after calcining to surface, and enriching section O member
Element causes C content accordingly to reduce；Sample contains micro Co and partial Sn and a large amount of Si；Calcining front and back Si content phase
Difference is very big, is to be present in bulk inner because of a large amount of Si, after burning, Si, which is migrated to block outer surface, to be exposed.
Performance evaluation
((a), (b), (c) are the surface picture under different resolution to the SEM figure that Fig. 1 is Coal-800, (d) are shone for section
Piece), from surface picture, it is seen that coal particle size is larger, and all in submicron order, and pore structure is bigger, this macroporous structure
Be conducive to the infiltration of electrolyte.It it can be seen that, is about 3 μm to thickness of electrode from cross-section photograph；
Fig. 2 is the powder x-ray diffraction and infrared spectrogram of Coal and Coal-800,700-900cm-1For aromatic hydrocarbon absorption
The absorption intensity variation of peak, raw coal and pyrolyzing coal at this less, illustrates that fragrant hydrocarbon structure is more stable；1000cm-1It is nearby
Mineral absorption peak, at relatively high temperatures, minerals are more stable, and variation at peak is smaller at this.Absorption peak is in 1100-
1500cm-1It is main to reflect C=O stretching vibration in range；1600cm-1It is nearby the carboxyl in raw coal, after pyrolytic gasification, with
CO2Form is run away disappearance；2900cm-1It is nearby respectively-CH3With-CH2Stretching vibration absworption peak, by pyrolysis after, the position
Absorption intensity substantially reduce, illustrate in gasification, the groups such as methyl and methylene are broken；3400cm-1It is nearby-OH
Absorption peak, peak type wideization, remitted its fury after pyrolysis illustrate the reduction of oxygen-containing group content；3696cm-1For the O-H vibration in lignite
Or free-OH, this peak disappears after pyrolysis, also illustrates the reduction of oxygen-containing group content；
The TEM that Fig. 3 is Coal-800 and Coal-800-HCl schemes, it can be seen from the figure that not washing off after pickling
Foreign metal and minerals in Coal-800 illustrate that Coal-800 forms onion clad structure, very stable, are not easy to remove.
Fig. 4 is the I-V curve of dye-sensitized solar cells, concludes that the dye sensitization prepared with the method by Fig. 4
Solar battery is to the battery efficiency and Pt electrode of electrode very close to (incident photon-to-electron conversion efficiency: Pt 8.24%, Coal-800-
HCl 8.23%), and the method preparation is simple, it is low in cost.
Fig. 5 left figure is the CV curve of dye-sensitized solar cells；The cyclic voltammetric stability that right figure is Coal-800 is bent
Line therefrom concludes that Coal-800 and Coal-800-HCl compared with Pt, have close iodine reduction potential poor, bigger
Current density after scanning 100 is enclosed, still has good cyclic voltammetric stability.
The assembling process of dye-sensitized solar cells:
1. by TiO2Slurry (granular size about 20nm) is printed on FTO electro-conductive glass that (effective area is 4mm × 4mm, thick
Degree is 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 in Muffle furnace are cooling
To room temperature, roasting light anode is then placed in 45 DEG C of immersions in dyestuff (main component N719, acetonitrile: tert-butyl=1:1)
120 minutes；
2. by TiO2Light anode is taken out from dye tank, is rinsed with ethyl alcohol, N2Rifle drying, then with obtained to electrode pair
It connects, with clamp, is assembled into battery, liquid electrolyte (is I-/I3 -Electrolyte) test when along conductive glass
Glass is added dropwise.
3. wherein, as a comparison: Pt electrode is prepared with the method for magnetron sputtering, Pt is splashed on FTO electro-conductive glass,
With a thickness of 200nm.
Using following apparatus test made of dye-sensitized solar cells I-V curve 1. digital sourcemeter
(Keithley2601, Keithley instrument company, the U.S.) 2. solar simulator (xenon lamp, lighting programmers AM1.5,100mW/
cm2) (PEC-L15, Japanese Peccell company) 3. standard silion cell (be used for calibration light source) (BS-520, Japanese Sharp company).
Claims (4)
1. a kind of dye-sensitized solar cells is to electrode, described that electrode is made as follows: by the derivative carbon material of lignite
After isopropanol mixing and ball milling 4h, mixed liquor obtained by ball milling is sprayed on electro-conductive glass, it is dry to get, wherein lignite is derivative
Carbon material and isopropanol amount ratio are the mL of 60 ~ 80 mg:5 ~ 8；
The derivative carbon material of the lignite is made as follows: under inert atmosphere, by the temperature programming of lignite particle to 700 ~ 800 DEG C
And in 700 ~ 800 DEG C of calcining at least 1.5h, it is down to room temperature naturally afterwards, obtains the derivative carbon material of lignite,
Wherein, described program heats up are as follows: is raised to 400 DEG C by room temperature, heating rate: 5 DEG C/min；700 ~ 800 are raised to by 400 DEG C again
DEG C, heating rate: 2 DEG C/min, the lignite particle is made as follows:
1) bulk lignite is ground with coffee machine, is ground 2 ~ 3 times, each 2 min of milling time；It puts it into ball grinder again
1 ~ 3h of ball milling；200 meshes are crossed, 100 ~ 120 DEG C is placed in a vacuum drying oven and is dried；
2) the resulting lignite of step 1) is placed in spheroidal graphite tank, stainless shot is added, inert gas, encapsulation are full of in glove box
Good tank body, 20 ~ 24 h of ball milling；By the good lignite powder of ball milling utilize soaked in absolute ethyl alcohol 2 ~ 3 times, discard supernatant liquid, will under
Layer sediment is dried in baking oven；
In step 2, the following lignite of 200 mesh and stainless shot amount ratio are the g of 1 ~ 2 g:25 ~ 50, stainless shot diameter is 1 ~
1.2cm；Inert gas is high-purity argon gas；Drum's speed of rotation is set as 400 ~ 500 revs/min；The good lignite powder of ball milling with it is anhydrous
Ethanol consumption ratio is the mL of 1 ~ 2 g:35 ~ 50；Oven temperature is set as 40 ~ 80 DEG C.
2. according to claim 1 to electrode, it is characterised in that: the derivative carbon material of the lignite includes the step of post-processing
It suddenly, is after 1.5 ~ 2.5mol/L HCl is ultrasonically treated, to filter by gained lignite derived carbon material use concentration after calcining, washing,
It is dry.
3. according to claim 2 to electrode, it is characterised in that: the derivative carbon material of gained lignite and concentration after the calcining
HCl amount ratio for 1.5 ~ 2.5mol/L is the mL of 100 ~ 120 mg:35 ~ 50.
4. according to claim 1 to electrode, it is characterised in that: the derivative carbon material particles object of the lignite is leading electrode
Electric glass surface with a thickness of 3 ~ 5 μm.
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| CN104752062A (en) * | 2015-04-09 | 2015-07-01 | 大连理工大学 | Dye-sensitized solar cell counter electrode and production method thereof |
| CN106318504A (en) * | 2016-09-07 | 2017-01-11 | 昆明理工大学 | Coal-quality machine-made charcoal preparation method |
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| JP2003297446A (en) * | 2002-01-29 | 2003-10-17 | Nippon Shokubai Co Ltd | Dye-sensitized solar cell |
| CN1247454C (en) * | 2004-03-19 | 2006-03-29 | 昆明理工大学 | Method for producing active carbon by using cinder of brown coal |
| CN102583322B (en) * | 2012-03-07 | 2013-10-02 | 中国华能集团清洁能源技术研究院有限公司 | Active brown coal and preparation method thereof |
| CN104681296A (en) * | 2015-03-18 | 2015-06-03 | 信阳师范学院 | Carbon black composite counter electrode for dye-sensitized solar cells and preparation method thereof |
| CN104817082A (en) * | 2015-05-22 | 2015-08-05 | 安徽工业大学 | Method for preparing nitrogen-enriched porous carbon material for supercapacitor by taking lignite as raw material |
| CN106298265A (en) * | 2015-06-10 | 2017-01-04 | 辽宁立德电力工程设计有限公司 | Ultracapacitor composite and preparation method thereof |
| CN106629719A (en) * | 2016-09-21 | 2017-05-10 | 广东美的制冷设备有限公司 | Preparation technology for activated carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104752062A (en) * | 2015-04-09 | 2015-07-01 | 大连理工大学 | Dye-sensitized solar cell counter electrode and production method thereof |
| CN106318504A (en) * | 2016-09-07 | 2017-01-11 | 昆明理工大学 | Coal-quality machine-made charcoal preparation method |
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