CN109706505A - A kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array - Google Patents
A kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array Download PDFInfo
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- CN109706505A CN109706505A CN201910076646.0A CN201910076646A CN109706505A CN 109706505 A CN109706505 A CN 109706505A CN 201910076646 A CN201910076646 A CN 201910076646A CN 109706505 A CN109706505 A CN 109706505A
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Abstract
The present invention provides a kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array belongs to nanocomposite technical field.The step of specific preparation method are as follows: nano-tube array structure is prepared by the electrochemistry anodic oxidation of Titanium or titanium alloy first；Then Crystallizing treatment is carried out in Muffle furnace, obtains TiO2Nano-tube array；Again by CsPbI3G-C is added in nanoparticle3N4In suspension, obtain containing CsPbI3And g-C3N4Mixed solution；Finally by TiO2Nano-tube array is reacted with mixed solution, and g-C is prepared3N4/CsPbI3/TiO2Nano-tube array.For the modification processing method while advantage for giving full play to Nanotube Array, the multiple elements design for realizing two kinds of semiconductor materials is modified.The g-C being prepared3N4/CsPbI3/TiO2Nano-tube array, large specific surface area is wide to the response absorption region of sunlight, can be used as high performance combination electrode, the design for high-performance optical catalyst provides support.
Description
Technical field
The invention belongs to nanocomposite technical field, in particular to a kind of g-C3N4/ CsPbI3/TiO2Nanotube battle array
The preparation method of column.
Background technique
Currently, many researchers are dedicated to developing high performance optoelectronic pole material, and titanium dioxide (TiO2) rely on it
The good characteristics such as high chemical stability, cheap, nontoxic cause extensive concern.In TiO2Various nanostructure materials
In material, TiO2Nano-tube array is due to large specific surface area, adsorption capacity is strong, structure feature is conducive to the features such as electron-transport, quilt
It is considered one of most promising optoelectronic pole material.
However, TiO2Forbidden bandwidth it is wider (about 3.2 eV), can only be at ultraviolet light (3 ~ 5 % for accounting for solar energy resources)
Irradiation under be excited, and its photo-generated carrier is easy compound, and these problems greatly limit TiO2Nano-tube array is in light
The application of electricity conversion aspect.It therefore must be to TiO2Nano-tube array is modified processing.TiO2The modification side of nano-tube array
There are many kinds of methods, nonmetallic ion-doped such as metal ion mixing, noble metal loading and semiconductors coupling etc..In general, no
Same method of modifying improves TiO in terms of different2The photoelectric properties of nano-tube array, therefore multiple elements design is modified often
It can be TiO2The raising of nano-tube array photoelectric properties brings synergistic effect, becomes a kind of new modification trend.
Summary of the invention
The present invention is directed to the defect of traditional method of modifying, first by the electrochemistry anodic oxidation of Titanium or titanium alloy
Nano-tube array structure is prepared, Crystallizing treatment is then carried out in Muffle furnace, obtains TiO2Nano-tube array, then by CsPbI3It receives
G-C is added in rice corpuscles3N4In suspension, obtain containing CsPbI3And g-C3N4Mixed solution, finally by TiO2Nano-tube array with
Mixed solution reaction, has been prepared g-C3N4/ CsPbI3/TiO2Nano-tube array.
Specifically, a kind of g-C provided by the invention3N4/ CsPbI3/TiO2The preparation method of nano-tube array, is specifically pressed
Implement according to following steps:
S1: on titaniferous metallic matrix, Nanotube Array is prepared by anodizing；
S2: Crystallizing treatment is carried out to prepared Nanotube Array, obtains TiO2Nano-tube array；
S3: preparation g-C3N4Suspension and CsPbI3Nanoparticle, by CsPbI3G-C is added in nanoparticle3N4In suspension, obtain
Mixed solution.
S4: to prepared TiO2Nano-tube array is reacted with mixed solution, and g-C is prepared3N4/CsPbI3/TiO2It receives
Mitron array.
Preferably, the titaniferous metallic matrix is Titanium or titanium alloy.
Preferably, the specific steps of S1 are as follows:
S11: selecting electrolyte is fluorine-containing acidic aqueous solution or aqueous fluorine-containing organic system；
S12: by titaniferous metallic matrix in fluorine-containing acidic aqueous solution or aqueous fluorine-containing organic system electrolyte system in 15~
60V anodic oxygenization 0.5~for 24 hours, the Nanotube Array of high-sequential is grown in titaniferous metal base surface.
It is highly preferred that the specific steps of S2 are as follows:
By prepared Nanotube Array through 400~550 DEG C of heat treatment 2h, TiO is obtained2Nano-tube array.
It is highly preferred that the specific steps of S3 are as follows:
A certain amount of urea (or thiocarbamide or melamine) is weighed, by urea (or thiocarbamide or melamine) in Muffle furnace
400~600 DEG C of 2~3h of heat treatment, obtain flaxen g-C3N4Powder；
According to solid-to-liquid ratio: 0.1 ~ 2:50(g:ml) ratio, measure g-C respectively3N4Powder and dehydrated alcohol, sufficiently ultrasound removing
2h obtains a nanometer g-C3N4Suspension；
According to 0.05 ~ 0.2:0.05 ~ 0.2:5(mmol:mmol:ml) ratio, respectively measure CsI, PbI2With dimethyl formyl
Amine, while 0.5ml oleic acid and 0.25ml oleyl amine is added as surface ligand, mixed solution is added in 10ml toluene at room temperature,
Abundant centrifugal treating takes lower sediment to be scattered in ethane and refilters, and CsPbI is made3Nanoparticle；
By CsPbI3Nanometer g-C is added in nanoparticle3N4In suspension, the two molar ratio: 0.01 ~ 1:1；Abundant ultrasonic mixing, obtains
To containing CsPbI3And g-C3N4Mixed liquor.
It is highly preferred that the specific steps of S4 are as follows:
Obtained it will contain CsPbI3And g-C3N4Mixed solution with spin-coating method be coated in the TiO2On nano-tube array, coating
Number is 3 ~ 9 times, then handles 1 ~ 3h at 150 ~ 250 DEG C in drying box, obtains the g-C3N4/CsPbI3/TiO2Nanotube battle array
Column.
It is highly preferred that the specific steps of S4 are as follows:
By the TiO2Nano-tube array is impregnated in described containing CsPbI3And g-C3N4Mixed solution in, at room temperature impregnate 1 ~
10min, then 1 ~ 3h is handled at 150 ~ 250 DEG C in drying box, obtain g-C3N4/CsPbI3/TiO2Nano-tube array.
The present invention also provides a kind of g-C3N4/CsPbI3/TiO2Nano-tube array is prepared by any of the above-described method.
Technical solution of the present invention has the following beneficial effects:
(1) nano-tube array knot is prepared in Titanium or titanium alloy surface by electrochemistry anodic oxidation first in the present invention
Then structure carries out Crystallizing treatment in Muffle furnace, obtains TiO2Nano-tube array, then by CsPbI3G-C is added in nanoparticle3N4
In suspension, obtain containing CsPbI3And g-C3N4Mixed solution, finally by TiO2Nano-tube array is reacted with mixed solution, system
For g-C3N4/ CsPbI3/TiO2Nano-tube array.While by the advantage that gives full play to Nanotube Array, realize
The multiple elements design of two kinds of semiconductor materials is modified, and design for high-performance optical catalyst provides thinking.
(2) g-C provided by the invention3N4/CsPbI3/TiO2Nano-tube array, large specific surface area, the response to sunlight
Absorption region is wide, can be used as high performance combination electrode, carrys out photocatalysis removal pollutant.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
When embodiment provides numberical range, it should be appreciated that except non-present invention is otherwise noted, two ends of each numberical range
Any one numerical value can be selected between point and two endpoints.Unless otherwise defined, the present invention used in all technologies and
Scientific term is identical as the normally understood meaning of those skilled in the art of the present technique.Except specific method, equipment used in embodiment,
Outside material, grasp and record of the invention according to those skilled in the art to the prior art can also be used and this
Any method, equipment and the material of the similar or equivalent prior art of method described in inventive embodiments, equipment, material come real
The existing present invention.
A kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array, is specifically implemented according to the following steps:
S1: on titaniferous metallic matrix, Nanotube Array is prepared by anodizing；
S2: Crystallizing treatment is carried out to prepared Nanotube Array, obtains TiO2Nano-tube array；
S3: preparation g-C3N4Suspension and CsPbI3Nanoparticle, by CsPbI3G-C is added in nanoparticle3N4In suspension, obtain
Mixed solution.
S4: to prepared TiO2Nano-tube array is reacted with mixed solution, and g-C is prepared3N4/CsPbI3/TiO2It receives
Mitron array.
Technical solution of the present invention is specifically illustrated below.
Embodiment 1
A kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array, specific steps are as follows:
The titanium sheet for selecting 0.2mm thickness, is successively respectively cleaned by ultrasonic 5min in deionized water, acetone, isopropanol, dehydrated alcohol, does
It is dry spare.Using titanium sheet as anode, graphite flake is as cathode, 0.5wt%NH4F+0.3MH3PO4 Aqueous solution as electrolyte,
Electrochemical anodic oxidation 1h is carried out under 20V constant pressure, grows the Nanotube Array of high-sequential in titanium plate surface.It will receive
Mitron oldered array is heat-treated 2h at 550 DEG C, is obtained TiO with the heating rate of 3 DEG C/min2Nano-tube array.
A certain amount of urea is weighed, urea is heat-treated at 550 DEG C, obtains flaxen g-C3N4Powder；According to solid-liquid
Ratio than 1g:50ml, measures g-C respectively3N4Powder and dehydrated alcohol, ultrasound removing, obtains a nanometer g-C after being sufficiently mixed3N4
Suspension；PbI2Be dissolved in dimethyl sulfoxide with CsI, then plus oleic acid and oleyl amine are as outer ligand on a small quantity, after completely dissolution,
In toluene with liquid-transfering gun transfer 1ml to 10ml, after particulate matter to be generated, it is centrifugally separating to obtain a nanometer CsPbI3.By nanometer
CsPbI3Nanometer g-C is added3N4In suspension, the two molar ratio is 0.1:1, after abundant ultrasonic disperse, is obtained containing CsPbI3And g-
C3N4Mixed solution.
By above-mentioned TiO2Nano-tube array impregnates 5min at room temperature in the mixed solution, takes out and does at 200 DEG C
Dry 2h to get arrive g-C3N4/CsPbI3/TiO2Nano-tube array.
Embodiment 2
A kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array, specific steps are as follows:
TiO is prepared using the method for embodiment 12Nano-tube array and contain CsPbI3And g-C3N4Mixed solution.It will be made
Mixed solution with spin-coating method be coated in the TiO2On nano-tube array, coating number is 9 times, is taken out dry at 200 DEG C
2h obtains g-C3N4/CsPbI3/TiO2Nano-tube array.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, and protection scope is unlimited
In this.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in protection of the invention
Within the scope of, protection scope of the present invention is subject to claims.
Claims (8)
1. a kind of g-C3N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that specifically real according to the following steps
It applies:
S1: on titaniferous metallic matrix, Nanotube Array is prepared by anodizing；
S2: Crystallizing treatment is carried out to prepared Nanotube Array, obtains TiO2Nano-tube array；
S3: preparation g-C3N4Suspension and CsPbI3Nanoparticle, by CsPbI3G-C is added in nanoparticle3N4In suspension, obtain
Mixed solution；
S4: to prepared TiO2Nano-tube array is reacted with mixed solution, and g-C is prepared3N4/CsPbI3/TiO2Nanotube
Array.
2. a kind of g-C according to claim 13N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that
The titaniferous metallic matrix is Titanium or titanium alloy.
3. a kind of g-C according to claim 13N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that
The specific steps of S1 are as follows:
S11: selecting electrolyte is fluorine-containing acidic aqueous solution or aqueous fluorine-containing organic system；
S12: by titaniferous metallic matrix in fluorine-containing acidic aqueous solution or aqueous fluorine-containing organic system electrolyte system in 15~
60V anodic oxygenization 0.5~for 24 hours, the Nanotube Array of high-sequential is grown in titaniferous metal base surface.
4. a kind of g-C according to claim 33N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that
The specific steps of S2 are as follows:
By prepared Nanotube Array through 400~550 DEG C of heat treatment 2h, TiO is obtained2Nano-tube array.
5. a kind of g-C according to claim 43N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that
The specific steps of S3 are as follows:
A certain amount of urea (or thiocarbamide or melamine) is weighed, by urea (or thiocarbamide or melamine) in Muffle furnace
400~600 DEG C of 2~3h of heat treatment, obtain flaxen g-C3N4Powder；
According to solid-to-liquid ratio: 0.1 ~ 2:50(g:ml) ratio, measure g-C respectively3N4Powder and dehydrated alcohol, sufficiently ultrasound removing
2h obtains a nanometer g-C3N4Suspension；
According to 0.05 ~ 0.2:0.05 ~ 0.2:5(mmol:mmol:ml) ratio, respectively measure CsI, PbI2With dimethyl formyl
Amine, while 0.5ml oleic acid and 0.25ml oleyl amine is added as surface ligand, mixed solution is added in 10ml toluene at room temperature,
Abundant centrifugal treating takes lower sediment to be scattered in ethane and refilters, and CsPbI is made3Nanoparticle；
By CsPbI3Nanometer g-C is added in nanoparticle3N4In suspension, the two molar ratio: 0.01 ~ 1:1；Abundant ultrasonic mixing, obtains
To containing CsPbI3And g-C3N4Mixed liquor.
6. a kind of g-C according to claim 53N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that
The specific steps of S4 are as follows:
Obtained it will contain CsPbI3And g-C3N4Mixed solution with spin-coating method be coated in the TiO2On nano-tube array, coating time
Number is 3 ~ 9 times, then handles 1 ~ 3h at 150 ~ 250 DEG C in drying box, obtains the g-C3N4/CsPbI3/TiO2Nanotube battle array
Column.
7. a kind of g-C according to claim 53N4/CsPbI3/TiO2The preparation method of nano-tube array, which is characterized in that
The specific steps of S4 are as follows:
By the TiO2Nano-tube array is impregnated in described containing CsPbI3And g-C3N4Mixed solution in, at room temperature impregnate 1 ~
10min, then 1 ~ 3h is handled at 150 ~ 250 DEG C in drying box, obtain g-C3N4/CsPbI3/TiO2Nano-tube array.
8. a kind of g-C3N4/CsPbI3/TiO2Nano-tube array, which is characterized in that by any the method system of claim 1~7
It is standby to obtain.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743592A (en) * | 2019-10-25 | 2020-02-04 | 天津理工大学 | Perovskite photocatalyst and preparation method and application thereof |
| CN111518558A (en) * | 2019-12-11 | 2020-08-11 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN112981484A (en) * | 2021-02-22 | 2021-06-18 | 上海电力大学 | Method for preparing perovskite material based on electrochemical method |
| CN114682242A (en) * | 2022-03-31 | 2022-07-01 | 武汉理工大学 | Porous structure large-area photocatalytic device with built-in electric field and preparation method thereof |
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2019
- 2019-01-26 CN CN201910076646.0A patent/CN109706505A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743592A (en) * | 2019-10-25 | 2020-02-04 | 天津理工大学 | Perovskite photocatalyst and preparation method and application thereof |
| CN110743592B (en) * | 2019-10-25 | 2022-09-13 | 天津理工大学 | Perovskite photocatalyst and preparation method and application thereof |
| CN111518558A (en) * | 2019-12-11 | 2020-08-11 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN111518558B (en) * | 2019-12-11 | 2021-10-26 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN112981484A (en) * | 2021-02-22 | 2021-06-18 | 上海电力大学 | Method for preparing perovskite material based on electrochemical method |
| CN114682242A (en) * | 2022-03-31 | 2022-07-01 | 武汉理工大学 | Porous structure large-area photocatalytic device with built-in electric field and preparation method thereof |
| CN114682242B (en) * | 2022-03-31 | 2024-02-27 | 武汉理工大学 | Large-area photocatalytic device with built-in electric field and porous structure and preparation method thereof |
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Application publication date: 20190503 |