CN107833754A - The method that the quick battery light anode material of diatom opal making dye is lost using high fever - Google Patents
The method that the quick battery light anode material of diatom opal making dye is lost using high fever Download PDFInfo
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- CN107833754A CN107833754A CN201711053114.2A CN201711053114A CN107833754A CN 107833754 A CN107833754 A CN 107833754A CN 201711053114 A CN201711053114 A CN 201711053114A CN 107833754 A CN107833754 A CN 107833754A
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- 239000011022 opal Substances 0.000 title claims abstract description 73
- 239000010405 anode material Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 21
- 208000021760 high fever Diseases 0.000 title claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002028 Biomass Substances 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 241000195493 Cryptophyta Species 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- FWFGVMYFCODZRD-UHFFFAOYSA-N oxidanium;hydrogen sulfate Chemical compound O.OS(O)(=O)=O FWFGVMYFCODZRD-UHFFFAOYSA-N 0.000 claims 1
- 238000003763 carbonization Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 12
- 239000000975 dye Substances 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 229920006395 saturated elastomer Polymers 0.000 abstract description 6
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 150000003608 titanium Chemical class 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000002131 composite material Substances 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 241000206761 Bacillariophyta Species 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008436 biogenesis Effects 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- -1 moon Ion Chemical class 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2045—Light-sensitive devices comprising a semiconductor electrode comprising elements of the fourth group of the Periodic Table with or without impurities, e.g. doping materials
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Hybrid Cells (AREA)
Abstract
The present invention relates to a kind of method that the quick battery light anode material of diatom opal making dye is lost using high fever.Porous of the present invention by diatom opal, TiO2Photoelectric activity and high fever lose the biomass three that adheres in diatom opal and combine, prepare low cost, the DSSC light anode materials of high activity.The biomass in-situ reducing of the invention for first being deposited high loss of ignition diatom opal surface by reducing calcining is porous carbonaceous presoma, is re-introduced into inorganic titanium salt and is reacted under hydrothermal conditions with carbonization diatom opal surface active ingredient, so as to improve TiO2Nanocrystalline crystallization degree, dispersiveness and adhesion-tight.This method simple production process, it is low for equipment requirements, easily realize industrialized production, cost of material is low, strong to environmental suitability, obtaining light anode material has higher cost performance and dyestuff saturated extent of adsorption, is obviously improved the short circuit current and efficiency of DSSC.
Description
Technical field
The invention belongs to mineral material to develop field, more particularly to a kind of to lose diatom opal mineral based on high fever
Prepared by high-performance photoelectricity converting function material, both a kind of preparation method of dye sensitized solar battery anode material.
Background technology
With getting worse the problems such as energy crisis and environmental pollution, greenhouse effects and depletion of the ozone layer, people couple can
The lasting increase of the demand of the regeneration green energy.Solar energy because its cleaning, it is pollution-free the features such as and turn into one kind preferably enjoy
The new energy of concern.Solar cell is one of utilization solar energy most effective way.Since Lausanne, SUI in 1991 joins
Since the Institute of Technology of nation professor GraetZel is successfully prepared DSSC (DSSC), its efficiency has moved closer to
The level of commercial solar cell, as a kind of inexpensive unconventional solar cell, show fabulous development prospect.
Manufacture high performance porous TiO2Photo-anode film, it is always the key of effective lifting DSSC battery efficiencies.People
Continuously attempt to lift TiO2The light utilization efficiency of light anode, optoelectronic transformation efficiency, charge transport properties, reduce and reunite, improve film
The modes such as pore passage structure, make high performance DSSC light anodes material.Such as【CN 102568854 A】Describe a kind of low band gaps
Conductor oxidate and manufacture method include DSSC simultaneously.By by carbon, nitrogen, fluorine and its combination the moon
Ion doping enters nano-TiO2In, the band-gap energy of conductor oxidate is reduced, so as to improve the energy of DSSC
Measure conversion ratio.【CN 102222575 A】Describe one kind and prepare dye-sensitized solar cell anode using magnetron sputtering method
Method, the thick fine and close semiconductor layer of one layer of about 50-300nm is sputtered on the surface of FTO electro-conductive glass as barrier layer, is then existed
Semiconductor grain is deposited on the FTO conductive bases with fine and close barrier layer by electrophoresis in alcoholic solution.The method can be done
Preferable semiconductor crystal film layer is orientated to a fairly large number of crystal orientation is obtained in conductive substrates in a short time.【CN
102496478 A】Disclose a kind of CNT and titanium tetrachloride improving performance of nanofiber membrane of dye-sensitized battery by synergistic action
Method.This method is first in TiO2Multi-walled carbon nanotube is mixed in spinning liquid as precursor, sintering obtains TiO after electrostatic spinning2Nanometer
Tunica fibrosa, finally post-processed with titanium tetrachloride aqueous solution.Carbon nano tube-doped with the synergy of titanium tetrachloride processing, making
The total photoelectric transformation efficiency of its dye-sensitized solar cells improves 15%-23%.Research shows, to TiO2Middle incorporation carbon, change
Kind TiO2Porous be all advantageous to lifted DSSC light anodes performance.
Diatom opal is also referred to as diatomite, the natural porous mineral being made up of amorphous silica, and it is ocean or lake
The Diatomeae remains grown in pool are in subaqueous deposit, the biogenesis siliceous sedimentary rock for acting on and gradually forming through natural environment.
There are a large amount of carboxyls to cover in the surface of diatom test and its micropore, and with the presence of hydrogen bond, thus aobvious faintly acid, therefore also referred to as solid
Acid.Diatom opal is because with unique shell structure, strong adsorptivity, bigger serface, high porosity and high temperature resistant etc. are excellent
Property and be widely used in the fields such as chemical industry, oil, building materials and food.【CN 102568854 A】Describe a kind of dye sensitization
The preparation method of solar cell, diatomite in powder and titanium dioxide powder are mixed according to a certain ratio, light anode titanium dioxide
Diatomite doping is 5%-50% in coating, 0.5-3 μm of coating layer thickness.It is quick that although dyestuff can be greatly lowered in this method
Change the cost and absorption, weatherability of solar battery light anode, contribute to DSSC popularization and application, but diatomite electric conductivity itself
Difference, it is unfavorable for the transmission of photogenerated charge, the effect for being difficult to lift battery efficiency is directly mixed with titanium oxide.
It is biogenic porous mineral in view of diatom opal, its surface deposition adheres to a large amount of biomass, especially
High fever loses the content of biomass in diatom opal mineral up to more than 10wt%, and containing for grey black can be obtained after reduction treatment
Carbon diatom opal, electric conductivity are obviously improved.TiO is carried using this diatom opal2It is expected to improving TiO2Porous,
While weatherability, TiO is realized2C doping and photogenerated charge effective transmission.But at present on high fever amount diatom opal
And its research that carbonized product is applied in terms of dye sensitized solar battery anode material has not been reported.
For problem above, the present invention is considered the porous of diatom opal, TiO2Photoelectric activity and high fever lose
The biomass three adhered in diatom opal combines, and prepares low cost, the DSSC light anode materials of high activity.
The principle of the present invention is to utilize to reduce calcination process, is high living by the biomass reduction of high loss of ignition diatom opal surface deposition
Property contains carbon matrix precursor, and be re-introduced into inorganic titanium salt interacts with diatom opal surface active ingredient, promotes TiO2It is excellent
First it is nucleated on the surface of carbon containing diatom opal, and constantly grows up under hydrothermal conditions to improve crystallinity, solves nano-TiO2
The problem of crystallinity is poor, caking, the bad dispersibility of easily reuniting.Simultaneously the biomass carbon in diatom opal in reduction process with
TiO2Fully combine, the electric conductivity of solar cell material can be improved, appropriate C doping can also extend light anode material
Spectrum utilization scope, improve DSSC light anode material reactivities.Moreover, because diatom opal improves light anode
Pore passage structure and adsorption capacity, fully can adsorb dyestuff after assembled battery, increase the work of DSSC
The Dye Adsorption amount of electrode, the consumption of circuit in battery is reduced, and then improve photoelectric transformation efficiency and service life.This method is given birth to
Production. art is simple, low for equipment requirements, easily realizes industrialized production, and cost of material is low, strong to environmental suitability, obtains light sun
Pole material has higher cost performance and the saturated extent of adsorption to dyestuff, is obviously improved the short circuit electricity of DSSC
Stream and efficiency.
The content of the invention：
It is an object of the invention to make full use of high fever to lose diatom opal to have abundant pore passage structure and attachment organic
The characteristics of matter, there is provided a kind of method of economical and effective synthesis diatom albumen ground mass DSSC light anode materials, and then realize silicon
The higher value application of algae opal mineral resources, while also provide a kind of feasible manufacturer to lift the cost performance of DSSC batteries
Method.
The purpose of the present invention is achieved through the following technical solutions：
The method that diatom opal making dye-sensitized solar battery light anode material is lost using high fever, is comprised the following steps：
A. the diatom opal raw ore that loss on ignition is more than 17wt% is chosen, is crushed through conventional method, water purification by floatation obtains
(purity accounts for its high temperature except the hundred of carbon calcination product gross mass to diatom opal of the purity more than 80wt% with the quality of diatom opal
Divide content meter).Below the crushing material to 100 mesh, 600~1000 DEG C of 4~6h of roasting under the conditions of carbon thermal reduction are placed in, are obtained
The diatom opal of biomass in-situ carburization.
B. according to WBe carbonized diatom opal：WTiO2=0.2~0.76 mass ratio, the carbonization diatom opal powder that step a is obtained
Body, it is added in 0.5~2mol/L titaniferous sulfate solution, wherein TiO2Quality by oxygen in titaniferous sulfate presoma
Change the content conversion of titanium.It is sufficiently stirred, regulation system pH to 2~6, is transferred in closed reactor, is warming up to 170~240 DEG C,
It is incubated 6~30h.Separation of solid and liquid after cooling, washing is to without free SO4 2-, dry and obtain be carbonized diatom opal and TiO2It is compound
Thing, as high fever lose diatom albumen ground mass DSSC light anode materials.
C. after taking the light anode composite obtained by step b finely ground in agate mortar, it is mixed to add appropriate cementing agent grinding
Conjunction obtains slurries, the FTO conductive glass surfaces coated on cleaning, and 400~450 DEG C of roastings in Muffle furnace are placed in after natural drying
0.5h, DSSC light anodes are obtained after taking out cooling.
Described titaniferous sulfate is defined to：One kind in titanium sulfate, titanyl sulfate.
Beneficial effect：The present invention loses the composition of diatom opal, design feature for high fever, utilizes the active hydroxyl on its surface
Base and biology in situ matter carbon, TiO is realized under thermal and hydric environment2Be carbonized diatom opal Interface composites and carbon doping,
So as to significantly improve TiO2Crystallinity, dispersiveness, photolytic activity and adsorptivity, while cost is reduced, improve DSSC
Short circuit current, battery efficiency and service life.
Brief description of the drawings：
1st, the DSSC cell I-V curves that Fig. 1 is assembled into for light anode prepared by embodiment 1.
Embodiment：
The present invention is described in further detail with reference to the accompanying drawings and examples：
Embodiment 1
A. the diatom opal raw ore that loss on ignition is 18.5wt% is chosen, is crushed through conventional method, water purification by floatation obtains
(purity accounts for percentage of its high temperature except carbon calcination product gross mass to the diatom opal that purity is 89wt% with the quality of diatom opal
Content meter).Below the crushing material to 100 mesh, 800 DEG C of roasting 4h under the conditions of carbon thermal reduction are placed in, obtain biomass original position
The diatom opal of carbonization.
B. according to WBe carbonized diatom opal：WTiO2=0.2 mass ratio, the carbonization diatom opal powder that step a is obtained, add
Into 0.5mol/L titaniferous sulfate solution, wherein TiO2Quality converted by Ti contents in titaniferous sulfate presoma.
It is sufficiently stirred, regulation system pH to 4.5, is transferred in closed reactor, be warming up to 180 DEG C, is incubated 10h.Solid-liquid point after cooling
From washing is to without free SO4 2-, dry and obtain be carbonized diatom opal and TiO2Compound, as high fever lose diatom opal
Base DSSC light anode materials.
C. after taking the light anode composite obtained by step b finely ground in agate mortar, it is mixed to add appropriate cementing agent grinding
Conjunction obtains slurries, the FTO conductive glass surfaces coated on cleaning, and 450 DEG C of roasting 0.5h in Muffle furnace are placed in after natural drying, are taken
DSSC light anodes are obtained after going out cooling.By light anode, immersion 40 is small in the ethanol solution for the N719 dyestuffs that concentration is 50mM
When take out, with to electrode assembling DSSC batteries and adding electrolyte after clean surface, DSSC batteries are obtained after encapsulation.With phase Tongfang
Pure TiO made from method2Light anode is compared, and carbonization diatom opal base light anode material is lifted to the saturated extent of adsorption of N719 dyestuffs
48%, DSSC short circuit current lift 81% (referring to accompanying drawing 1), photoelectric transformation efficiency lifting 19%.
Embodiment 2
A. the diatom opal raw ore that loss on ignition is 21.4wt% is chosen, is crushed through conventional method, water purification by floatation obtains
(purity accounts for percentage of its high temperature except carbon calcination product gross mass to the diatom opal that purity is 85wt% with the quality of diatom opal
Content meter).Below the crushing material to 100 mesh, 600 DEG C of roasting 6h under the conditions of carbon thermal reduction are placed in, obtain biomass original position
The diatom opal of carbonization.
B. according to WBe carbonized diatom opal：WTiO2=0.4 mass ratio, the carbonization diatom opal powder that step a is obtained, add
Into 1mol/L titaniferous sulfate solution, wherein TiO2Quality converted by Ti contents in titaniferous sulfate presoma.Fill
Divide stirring, regulation system pH to 6, be transferred in closed reactor, be warming up to 200 DEG C, be incubated 8h.Separation of solid and liquid after cooling, is washed
Wash to without free SO4 2-, dry and obtain be carbonized diatom opal and TiO2Compound, as high fever lose diatom albumen ground mass
DSSC light anode materials.
C. after taking the light anode composite obtained by step b finely ground in agate mortar, it is mixed to add appropriate cementing agent grinding
Conjunction obtains slurries, the FTO conductive glass surfaces coated on cleaning, and 450 DEG C of roasting 0.5h in Muffle furnace are placed in after natural drying, are taken
DSSC light anodes are obtained after going out cooling.By light anode, immersion 40 is small in the ethanol solution for the N719 dyestuffs that concentration is 50mM
When take out, with to electrode assembling DSSC batteries and adding electrolyte after clean surface, DSSC batteries are obtained after encapsulation.With phase Tongfang
Pure TiO made from method2Light anode is compared, and carbonization diatom opal base light anode material is lifted to the saturated extent of adsorption of N719 dyestuffs
76%, DSSC short circuit current lifting 35%.
Embodiment 3
A. the diatom opal raw ore that loss on ignition is 18.5wt% is chosen, is crushed through conventional method, water purification by floatation obtains
(purity accounts for percentage of its high temperature except carbon calcination product gross mass to the diatom opal that purity is 89wt% with the quality of diatom opal
Content meter).Below the crushing material to 100 mesh, 1000 DEG C of roasting 4h under the conditions of carbon thermal reduction are placed in, obtain biomass original position
The diatom opal of carbonization.
B. according to WBe carbonized diatom opal：WTiO2=0.76 mass ratio, the carbonization diatom opal powder that step a is obtained, adds
Enter into 0.5mol/L titaniferous sulfate solution, wherein TiO2Quality rolled over by Ti contents in titaniferous sulfate presoma
Calculate.It is sufficiently stirred, regulation system pH to 2, is transferred in closed reactor, be warming up to 170 DEG C, is incubated 24h.Solid-liquid point after cooling
From washing is to without free SO4 2-, dry and obtain be carbonized diatom opal and TiO2Compound, as high fever lose diatom opal
Base DSSC light anode materials.
C. after taking the light anode composite obtained by step b finely ground in agate mortar, it is mixed to add appropriate cementing agent grinding
Conjunction obtains slurries, the FTO conductive glass surfaces coated on cleaning, and 450 DEG C of roasting 0.5h in Muffle furnace are placed in after natural drying, are taken
DSSC light anodes are obtained after going out cooling.By light anode, immersion 40 is small in the ethanol solution for the N719 dyestuffs that concentration is 50mM
When take out, with to electrode assembling DSSC batteries and adding electrolyte after clean surface, DSSC batteries are obtained after encapsulation.With phase Tongfang
Pure TiO made from method2Light anode is compared, and carbonization diatom opal base light anode material is lifted to the saturated extent of adsorption of N719 dyestuffs
13%, DSSC short circuit current lifting 38%.
Embodiment 4
A. the diatom opal raw ore that loss on ignition is 23.6wt% is chosen, is crushed through conventional method, water purification by floatation obtains
(purity accounts for percentage of its high temperature except carbon calcination product gross mass to the diatom opal that purity is 91wt% with the quality of diatom opal
Content meter).Below the crushing material to 100 mesh, 700 DEG C of roasting 4h under the conditions of carbon thermal reduction are placed in, obtain biomass original position
The diatom opal of carbonization.
B. according to WBe carbonized diatom opal：WTiO2=0.3 mass ratio, the carbonization diatom opal powder that step a is obtained, add
Into 1mol/L titaniferous sulfate solution, wherein TiO2Quality converted by Ti contents in titaniferous sulfate presoma.Fill
Divide stirring, regulation system pH to 5, be transferred in closed reactor, be warming up to 240 DEG C, be incubated 18h.Separation of solid and liquid after cooling, is washed
Wash to without free SO4 2-, dry and obtain be carbonized diatom opal and TiO2Compound, as high fever lose diatom albumen ground mass
DSSC light anode materials.
C. after taking the light anode composite obtained by step b finely ground in agate mortar, it is mixed to add appropriate cementing agent grinding
Conjunction obtains slurries, the FTO conductive glass surfaces coated on cleaning, and 450 DEG C of roasting 0.5h in Muffle furnace are placed in after natural drying, are taken
DSSC light anodes are obtained after going out cooling.By light anode, immersion 40 is small in the ethanol solution for the N719 dyestuffs that concentration is 50mM
When take out, with to electrode assembling DSSC batteries and adding electrolyte after clean surface, DSSC batteries are obtained after encapsulation.With phase Tongfang
Pure TiO made from method2Light anode is compared, and carbonization diatom opal base light anode material is lifted to the saturated extent of adsorption of N719 dyestuffs
88%, DSSC short circuit current lifting 69%.
Claims (1)
- A kind of 1. method that the quick battery light anode material of diatom opal making dye is lost using high fever, it is characterised in that including such as Lower step：From loss on ignition, more than the diatom opal powder of 17wt% and purity more than 80wt%, (purity is with diatom opal Quality account for the percentage composition meter that its high temperature removes carbon calcination product gross mass), be placed under the conditions of 600~1000 DEG C of carbon thermal reduction and roast 4~6h is burnt, the diatom opal of biomass in-situ carburization is obtained, then according to WBe carbonized diatom opal：WTiO2=0.2~0.76 quality Than adding it in the solution of titanium sulfate or titanyl sulfate water, after being sufficiently stirred, regulation system pH to 2~6, being transferred to close Close in reactor, be warming up to 170~240 DEG C, held for some time, cooling, separation of solid and liquid, washing and drying, obtain high fever and lose silicon Algae albumen ground mass DSSC light anode materials；Slurries are made with appropriate cementing agent mixed grinding in described light anode material, are coated on The FTO conductive glass surfaces of cleaning, DSSC light anodes are can obtain after drying and roasting.
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