CN105800681A - Preparation method of TiO2 nanoparticles with photonic crystal characteristics - Google Patents
Preparation method of TiO2 nanoparticles with photonic crystal characteristics Download PDFInfo
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- CN105800681A CN105800681A CN201610092480.8A CN201610092480A CN105800681A CN 105800681 A CN105800681 A CN 105800681A CN 201610092480 A CN201610092480 A CN 201610092480A CN 105800681 A CN105800681 A CN 105800681A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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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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Abstract
The invention discloses a preparation method of TiO2 nanoparticles with photonic crystal characteristics. The preparation method comprises the following steps: preparing a precursor solution by mixing TiCl4 solution, absolute ethyl alcohol and deionized water; and with butterfly wings as a bio-template, treating the template by a solution impregnation method and removing the template at a high temperature to obtain the TiO2 nanoparticles. The preparation method disclosed by the invention has the advantages of simple technology, easily available raw materials, good product structure and performance and the like; and the prepared TiO2 nanoparticles with photonic crystal characteristics have a good application prospect in the field of thin-film solar cell study.
Description
One, technical field
The preparation method that the present invention relates to a kind of photonic crystal, specifically a kind of TiO with photonic crystal properties2The preparation method of nano-particle, belongs to semiconductor materials and devices technical field.
Two, background technology
In nature, some materials are owing to himself having the structure of periodic arrangement, it is possible to be counted as natural photonic crystal.Such as butterfly's wing, opal, beetle shell etc..Why these natural photonic crystals have multicoloured color under the irradiation of natural light, are because what the reflection of the light generation different-waveband of different angles incidence can be caused by their distinctive periodic structure.Wherein butterfly's wing is because having the periodic structure of in-plane and belonging to two-dimensional photon crystal structure.Current Technology aspect, colloidal crystal self-assembly method and counter opal structure method are two kinds of methods the most frequently used in photonic crystal preparation method.But it is not fully up to expectations using its photonic crystal prepared as light scattering layer performance in DSSC.Still need better method badly to prepare photonic crystal.
Find according to the study, the color of Argynnis wing comes from the interaction of its internal two-dimentional porous photon crystal structure and ambient, and the photonic crystal that this bioprotein is constituted changes into conductor oxidate just can obtain the conductor oxidate with two-dimensional photon crystal structure.TiO2Being a kind of wide bandgap semiconductor materials, not only have high transmission rate rare in other quasiconductors, and its refractive index ratio bioprotein is high, this is conducive to photon transmission therein and transport.
Present stage utilizes metal-oxide to replicate biological template structure and still has more incomplete place.Etc. IwaseE. using photoetching technique to scribe the diffraction lattice of similar butterfly's wing scale structure at silicon chip surface, but its technological level is limited, the microstructural fine degree obtained of institute cannot be mentioned in the same breath with nature butterfly；CookG. wait with a peafowl a kind of butterfly harmful to crop plants (Peacockbutterfly) scale for template, adopt chemical vapour deposition technique (CVD), prepare SiO2Butterfly wing morph-genetic materials, owing to silane hydrolyzate speed is difficult to control to, causes just having been formed SiO after not yet penetrating into the internal structure of scale2Layer, it is impossible to accurately replicate its structure；SilverJ. the big scale structure dodging butterfly MorphoPleides with the South America with class photon crystal structure is waited for template, to adopt sol-gel process to prepare TiO2Photon crystal material, but due to TiO2The hydrolysis rate of presoma cannot well control, and the final butterfly wing hierarchy details replicated obscures, and is only capable of the architectural feature retaining wing ridge with the micron-scale of wing rib；HuangJ.Y. wait and adopt atomic layer deposition method (ALD), carried out successively covering comparatively accurately to the microstructure of MorphoPeleides, obtained the butterfly fin structure material of different-thickness.But due to Al2O3The refractive index of refractive index and chitin basically identical, final reflection spectral line there is no too big change.
Three, summary of the invention
It is desirable to provide a kind of TiO with photonic crystal properties2The preparation method of nano-particle, to be solved technical problem is that the photonic absorbance improving photonic crystal, to improve thin-film solar cells to the rate that makes full use of of light and its photoelectric properties.
Described photonic crystal properties and a series of have a ridge that quasi-parallel structure has comb teeth-shaped to inlay, the rib vertical with ridge and their apertures of forming are the distribution of netted regular micro-nano hierarchy.
The present invention has the TiO of photonic crystal properties2The preparation method of nano-particle, comprises the steps:
(1) by the TiCl of 20mL2mol/L4Solution adds in 200mL volumetric flask, is subsequently added dehydrated alcohol and is settled to 200mL, obtains precursor solution；
(2) the butterfly wing after process is immersed in described precursor solution, closed processes 1.5 hours at 70 DEG C, 100mL deionized water is added subsequently in precursor solution, closed processes is continued 3.5 hours at 70 DEG C, butterfly wing is taken out and washes away with dehydrated alcohol the precursor solution of remained on surface by process after terminating, dry under room temperature；
Butterfly wing after processing described in step (2) processes by the following method and obtains:
Take butterfly some, remove its thorax abdomen with shears, retain butterfly wing；Butterfly wing immerses ultrasonic cleaning 1-15 minute in dehydrated alcohol, and ultrasonic cleaning takes out butterfly wing with tweezers after terminating, and rinses with dehydrated alcohol, the butterfly wing after being processed.
(3) the butterfly wing after step (2) processes is warming up to 400-600 DEG C of reaction 100-140min, is naturally down to room temperature subsequently, obtains the TiO with photonic crystal properties2Nano-particle.
Heating rate when being warming up to 400-600 DEG C in step (3) is 1-5 DEG C/min.
The course of reaction of step (3) is that butterfly wing is laid on clean slide surface, puts into and is connected with in the Muffle furnace of oxygen to carry out.
The present invention has the TiO of photonic crystal properties2Nano-particle can use as the scattering layer of DSSC He other thin-film solar cells.
The present invention utilizes biological template preparation to have the TiO of photonic crystal properties2Nano-particle, existing method is 1 micromachined method such as: by mechanical-physical size limitation, it is impossible to processing microwave band photonic crystal once；The 2 successively additions method: though below microwave band can be processed, the photonic crystal of near infrared band, but cost is that time cost is higher, also by the restriction of its size；3 microelectronics photoetching processes: cost is high, and it is only intended to the manufacture of mask, it is not that the photonic crystal finally given is had an effect, by the impact of optics systemic resolution；, so can there is, when preparing extremely small structure, the problem that deformation etc. is difficult to overcome in 4 soft lithographies: the preparation method still falling within physical layer；5 laser writing technology: owing to focus area is little, preparation time is longer, and efficiency is low and technical costs is high；6 laser-holographic interferometry: owing to the dielectric constant of photosensitive resin is little, therefore can not form three-dimensional complete photonic band gap, need to carry out secondary filling with other material；7 colloidal self-assembly methods: to the concentration of solution, pH value, ambient temperature, granule particle diameter etc. have harsher requirement, process conditions be difficult to grasp.
In the inventive method, in the process processing butterfly's wing with precursor solution, precursor solution is removed form TiO along the filling of butterfly's wing Hole and the high temperature of template2Network structure.Specifically first by TiCl4Solution is attached to the surface of butterfly wing template, through high-temperature process postadhesion in the TiCl of template surface4Solution reaction generates one layer the cancellated TiO of butterfly wing2Oxide.And through high temperature sintering, eliminate biological template originally.The template of the present invention is biological template, comes from the Nature, environment friendly and pollution-free, cost is low, quantity is many.Precursor power is simple, it is not necessary to long agitation, reduces the requirement to equipment.Template is at high temperature easily removed, and stove is also pollution-free, can reuse for a long time.Preparation method of the present invention is simple, and cost is low, reproducible.The present invention adopts transparent glass as substrate, and synthesis has the TiO of photonic crystal properties2Nano-particle inherits the schemochrome of the original template of original template, can be widely used for thin-film solar cells, has great market prospect.
The present invention has the TiO of photonic crystal properties2Nano-particle (abbreviation photonic crystal) is mainly used in field of thin film solar cells, for third generation novel thin film solaode DSSC.Photonic crystal prepared by the present invention can be effectively improved the absorbed probability of photon, the thickness being because depositing the resonator cavity of the length of penetration decision of incident illumination in the photonic crystal and the mesoporous layer between photonic crystal and substrate changes the location of photon in light anode caused, and improves light and catches.In the design of early stage photonic crystal, by structural modification in the process of integrated photon crystal and raising average cell size, its working electrode can improve photoelectric current and the photovoltage of battery such as theory prophesy simultaneously.Using the electrode being only 2 microns thick, these cooperative effects make photoelectric transformation efficiency reach 8.1%, compare to reference battery efficiency and improve 100%-150%.It can be seen that the introducing of photonic crystal can be obviously improved the photoelectric current of DSSC and corresponding photoelectric properties, the further investigation to it is also the problem that field of thin film solar cells can not be ignored.
Four, accompanying drawing explanation
Fig. 1 is electronic scanner microscope (SEM) overall diagram of former Argynnis wing template.
Fig. 2 is high power electronic scanner microscope (SEM) figure of former Argynnis wing template.
Fig. 3 is super-high power electronic scanner microscope (SEM) figure of former Argynnis wing template.
Fig. 4 is the TiO having photonic crystal properties2Electronic scanner microscope (SEM) overall diagram of nano-particle.
Fig. 5 is the TiO having photonic crystal properties2High power electronic scanner microscope (SEM) figure of nano-particle.
Fig. 6 is the TiO having photonic crystal properties2Super-high power electronic scanner microscope (SEM) figure of nano-particle.
Five, detailed description of the invention
In conjunction with specific examples below and accompanying drawing, the present invention is described in further detail, and the protected content of the present invention is not limited to following example.Under the spirit and scope without departing substantially from inventive concept, those skilled in the art it is conceivable that change and advantage be all included in the present invention, and with appending claims for protection domain.
Embodiment 1:
The present embodiment utilize Argynnis wing for templated synthesis TiO2The method of two dimension porous photon crystal material, specifically comprises the following steps that
1, take butterfly some, remove its thorax abdomen with shears, retain butterfly wing；Butterfly wing is immersed ultrasonic cleaning in dehydrated alcohol, and ultrasonic cleaning takes out butterfly wing with tweezers after terminating, and dries, the butterfly wing after being processed after rinsing with dehydrated alcohol under room temperature.
2, by the TiCl of 20mL2mol/L4Solution adds in 200mL volumetric flask, is subsequently added dehydrated alcohol and is settled to 200mL, obtains precursor solution；
3, the butterfly wing after process is immersed in described precursor solution, closed processes 1.5 hours at 70 DEG C, its ionized water of 100mL is added subsequently in precursor solution, closed processes is continued 3.5 hours at 70 DEG C, butterfly wing is taken out and washes away with dehydrated alcohol the solution of remained on surface by process after terminating, it is laid on clean microscope slide, naturally dries under room temperature；
4, the butterfly wing just dried is put in Muffle furnace together with the microscope slide under it, it is warming up to 500 DEG C with the heating rate of 1 DEG C/min and is incubated 120min, Temperature fall subsequently, microscope slide is taken out when muffle furnace is down to below 100 DEG C, with spoon, the butterfly wing powder baked is scraped, put into disposable test tube seals and preserve, obtain the TiO with photonic crystal properties2Nano-particle.
Embodiment 2:
The present embodiment utilize Sasakia charonda wing for templated synthesis TiO2The method of two dimension porous photon crystal material, specifically comprises the following steps that
1, take butterfly some, remove its thorax abdomen with shears, retain butterfly wing；Butterfly wing is immersed ultrasonic cleaning in dehydrated alcohol, and ultrasonic cleaning takes out butterfly wing with tweezers after terminating, and dries, the butterfly wing after being processed after rinsing with dehydrated alcohol under room temperature.
2, by the TiCl of 20mL2mol/L4Solution adds in 200mL volumetric flask, is subsequently added dehydrated alcohol and is settled to 200mL, obtains precursor solution；
3, the butterfly wing after process is immersed in described precursor solution, closed processes 1.5 hours at 70 DEG C, its ionized water of 100mL is added subsequently in precursor solution, closed processes is continued 3.5 hours at 70 DEG C, butterfly wing is taken out and washes away with dehydrated alcohol the solution of remained on surface by process after terminating, it is laid on clean microscope slide, naturally dries under room temperature；
4, the butterfly wing just dried is put in Muffle furnace together with the microscope slide under it, it is warming up to 500 DEG C with the heating rate of 1 DEG C/min and is incubated 100min, Temperature fall subsequently, microscope slide is taken out when muffle furnace is down to below 100 DEG C, with spoon, the butterfly wing powder baked is scraped, put into disposable test tube seals and preserve, obtain the TiO with photonic crystal properties2Nano-particle.
Embodiment 3:
Utilizing military triumphant butterfly wing in the present embodiment is templated synthesis TiO2The method of two dimension porous photon crystal material, specifically comprises the following steps that
1, take butterfly some, remove its thorax abdomen with shears, retain butterfly wing；Butterfly wing is immersed ultrasonic cleaning in dehydrated alcohol, and ultrasonic cleaning takes out butterfly wing with tweezers after terminating, and dries, the butterfly wing after being processed after rinsing with dehydrated alcohol under room temperature.
2, by the TiCl of 20mL2mol/L4Solution adds in 200mL volumetric flask, is subsequently added dehydrated alcohol and is settled to 200mL, obtains precursor solution；
3, the butterfly wing after process is immersed in described precursor solution, closed processes 1.5 hours at 70 DEG C, its ionized water of 100mL is added subsequently in precursor solution, closed processes is continued 3.5 hours at 70 DEG C, butterfly wing is taken out and washes away with dehydrated alcohol the solution of remained on surface by process after terminating, it is laid on clean microscope slide, naturally dries under room temperature；
4, the butterfly wing just dried is put in Muffle furnace together with the microscope slide under it, it is warming up to 500 DEG C with the heating rate of 1 DEG C/min and is incubated 140min, Temperature fall subsequently, microscope slide is taken out when muffle furnace is down to below 100 DEG C, with spoon, the butterfly wing powder baked is scraped, put into disposable test tube seals and preserve, obtain the TiO with photonic crystal properties2Nano-particle.
Scanned ultramicroscope (SEM) is observed, and Fig. 1 is electronic scanner microscope (SEM) overall diagram of former Argynnis wing template；Fig. 2 is high power electronic scanner microscope (SEM) figure of former Argynnis wing template；Fig. 3 is super-high power electronic scanner microscope (SEM) figure of former Argynnis wing template；Being taken respectively by obtained photonic crystal nanometer material and be dissolved in dehydrated alcohol in right amount, scanned ultramicroscope (SEM) is observed, and Fig. 4 is the TiO having photonic crystal properties2Electronic scanner microscope (SEM) overall diagram of nano-particle；Fig. 5 is the TiO having photonic crystal properties2High power electronic scanner microscope (SEM) figure of nano-particle；Fig. 6 is the TiO having photonic crystal properties2Super-high power electronic scanner microscope (SEM) figure of nano-particle.As can be seen from the figure whether from overall scale yardstick, or to more trickle micro-meter scale, butterfly's wing all can be forced by the method for the present invention and really be replicated.
Claims (4)
1. a TiO with photonic crystal properties2The preparation method of nano-particle, it is characterised in that comprise the steps:
(1) by the TiCl of 20mL2mol/L4Solution adds in 200mL volumetric flask, is subsequently added dehydrated alcohol and is settled to 200mL, obtains precursor solution；
(2) the butterfly wing after process is immersed in described precursor solution, closed processes 1.5 hours at 70 DEG C, 100mL deionized water is added subsequently in precursor solution, closed processes is continued 3.5 hours at 70 DEG C, butterfly wing is taken out and washes away with dehydrated alcohol the precursor solution of remained on surface by process after terminating, dry under room temperature；
(3) the butterfly wing after step (2) processes is warming up to 400-600 DEG C of reaction 100-140min, is naturally down to room temperature subsequently, obtains the TiO with photonic crystal properties2Nano-particle.
2. preparation method according to claim 1, it is characterised in that:
Butterfly wing after processing described in step (2) processes by the following method and obtains:
Remove butterfly thorax abdomen with shears, retain butterfly wing；Butterfly wing immerses ultrasonic cleaning 1-15 minute in dehydrated alcohol, and ultrasonic cleaning takes out butterfly wing with tweezers after terminating, and rinses with dehydrated alcohol, the butterfly wing after being processed.
3. preparation method according to claim 1, it is characterised in that:
Heating rate when being warming up to 400-600 DEG C in step (3) is 1-5 DEG C/min.
4. preparation method according to claim 1, it is characterised in that:
The course of reaction of step (3) is that butterfly wing is laid on clean slide surface, puts into and is connected with in the Muffle furnace of oxygen to carry out.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112239872A (en) * | 2020-10-15 | 2021-01-19 | 常州大学 | Modified branched TiO2Preparation method of photo-anode |
| CN112537757A (en) * | 2020-11-20 | 2021-03-23 | 浙江瑞成新材料股份有限公司 | Inorganic sheet material and method for producing same |
| CN114323362A (en) * | 2022-01-05 | 2022-04-12 | 吉林大学 | Flexible conformal electrode on surface of living insect prepared based on laser, preparation method and application thereof |
| CN114323362B (en) * | 2022-01-05 | 2024-05-14 | 吉林大学 | Flexible conformal electrode based on living insect surface prepared by laser, preparation method and application thereof |
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| JP2001180933A (en) * | 1999-12-22 | 2001-07-03 | Nippon Shokubai Co Ltd | Titanium black dispersion solution and manufacturing method |
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| JP2001180933A (en) * | 1999-12-22 | 2001-07-03 | Nippon Shokubai Co Ltd | Titanium black dispersion solution and manufacturing method |
| CN103103601A (en) * | 2011-11-10 | 2013-05-15 | 中国科学院化学研究所 | Method for preparing crack-free photonic crystal on surface of super-hydrophobic organism or super-hydrophobic imitation organism |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112239872A (en) * | 2020-10-15 | 2021-01-19 | 常州大学 | Modified branched TiO2Preparation method of photo-anode |
| CN112537757A (en) * | 2020-11-20 | 2021-03-23 | 浙江瑞成新材料股份有限公司 | Inorganic sheet material and method for producing same |
| CN114323362A (en) * | 2022-01-05 | 2022-04-12 | 吉林大学 | Flexible conformal electrode on surface of living insect prepared based on laser, preparation method and application thereof |
| CN114323362B (en) * | 2022-01-05 | 2024-05-14 | 吉林大学 | Flexible conformal electrode based on living insect surface prepared by laser, preparation method and application thereof |
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Inventor after: Xu Jinzhang Inventor after: Huang Bin Inventor after: Niu Haihong Inventor after: Cheng Cong Inventor after: Zhou Ru Inventor after: Hu Yu Inventor after: Zhang Gonghai Inventor before: Niu Haihong Inventor before: Xu Jinzhang Inventor before: Cheng Cong Inventor before: Hu Yu Inventor before: Zhang Gonghai Inventor before: Huang Bin Inventor before: Zhou Ru |