CN104773757A - Method for preparing hollow nanostructure constructed by TiO2 nanorods - Google Patents
Method for preparing hollow nanostructure constructed by TiO2 nanorods Download PDFInfo
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- CN104773757A CN104773757A CN201510220121.1A CN201510220121A CN104773757A CN 104773757 A CN104773757 A CN 104773757A CN 201510220121 A CN201510220121 A CN 201510220121A CN 104773757 A CN104773757 A CN 104773757A
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- tio
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- hollow nanostructure
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Abstract
The invention relates to a method for preparing a hollow nanostructure constructed by TiO2 nanorods and belongs to the field of photoelectric semiconductor materials. According to the method, TiF4 serves as a titanium source, a mixed solution of ethylene glycol and glacial acetic acid serves as a solvent, and ellipsoidal Fe2O3 nanoparticles serve as templates. The hollow nanostructure constructed by the TiO2 nanorods is prepared according to the hydrothermal method, the length of the hollow nanostructure is about 450 nm-500 nm, and the diameter of the hollow nanostructure is about 180 nm-220 nm; the length of the nanorods on the surface is about 70 nm-100 nm, and the diameter of the nanorods on the surface is about 10 nm. By means of the pre-growing templates, the form and inner surface structure of nanomaterials can be controlled, and better control over the performance of the hollow nanostructure is facilitated. The prepared TiO2 hollow nanostructure has the advantages that the size is controllable, operation is simple, raw materials are easy to obtain, and cost is low, and the prepared TiO2 hollow nanostructure has potential application prospects in the fields of environment, energy sources and the like.
Description
Technical field
The invention belongs to photoelectric semiconductor material field, relate to a kind of TiO
2the preparation method of hollow nano-material, is specifically related to one and utilizes hydrothermal template process to prepare nanometer core-shell structure copolymer composite structure and etched away by core and obtain by TiO
2the hollow nanostructured method that nanometer rod is constructed.
Background technology
Energy and environment are two principal themes of 21 century scientific research.Solve current day by day serious energy shortage and environmental problem be improve people's living standard, realize human social in the urgent need to.TiO
2as a kind of important semiconductor material with wide forbidden band, there is the character of excellent optics, electricity and chemical stability, and to human non-toxic, and there is good photochemical catalysis and opto-electronic conversion performance and be widely used the fields such as sensor, photocatalyst, electronic material, coating, solar cell, and be expected to utilize sun power to demonstrate wide application prospect in organic synthesis, photocatalytic water and environmental improvement.But the performance of material is by various factors such as size, specific surface area, pattern, porousness, crystalline phase and degree of crystallinity.Therefore, people wish can by exploring new synthetic method and controlling that building-up process reaches morphology controllable, particle diameter is adjustable, the TiO of excellent performance
2nano material.
At present, increasing research focuses on the TiO with special appearance and character
2in nanostructure, as nanometer ball, nanometer rod, nanotube etc.Although preparation TiO
2the method of nano material has a lot, but template is still considered to the very important technology of one of nano materials, utilizes its structure-directing effect effectively can control the size of synthetic materials, pattern, structure etc.Nano hollow structure has bigger serface, low relative density, the advantage such as mesoporosity, therefore, widely apply the promotion of demand in such as optoelectronic device, power storage, drug delivery etc. under, people have dropped into a large amount of energy in the nano hollow structure preparation with specific composition and structure.
Summary of the invention
The object of this invention is to provide a kind of by TiO
2nanometer rod is constructed and is formed hollow nanostructured preparation method, adopts the method for the shell of template growth material requested to prepare TiO
2nano hollow structure, uses pregrown template can handle the form of nano material and interior list structure, is conducive to the performance better controlling nano hollow structure.
The object of the invention is to be achieved through the following technical solutions:
A kind of by TiO
2the preparation method of the hollow nanostructured material that nanometer rod is constructed, with TiF
4do titanium source, ethylene glycol, glacial acetic acid mixing solutions as solvent, spheroid shape Fe
2o
3nanoparticle, as template, utilizes hydrothermal method to prepare by TiO
2the hollow nanostructured material that nanometer rod is constructed, concrete preparation technology is:
(1) Fe
2o
3the preparation of template:
By a certain amount of FeCl
3with deionized water dissolving, then add a certain amount of NaH
2pO
4the aqueous solution, moves in reactor, at 100 ~ 110 DEG C of heating 48h, obtained spheroid shape Fe
2o
3nanoparticle template.For guaranteeing Fe
2o
3template size is homogeneous and in ellipsoid shape, FeCl
3with NaH
2pO
4concentration ratio should remain on 100:1.5 ~ 2.
(2) Fe
2o
3/ TiO
2prepared by nanometer nucleocapsid structure:
By a certain amount of TiF
4powder is dissolved in 40 mL ethylene glycol, control TiF
4in ethylene glycol solution, concentration is 5 ~ 40mM, then adds 2 ~ 8mL glacial acetic acid and 0.02gFe successively
2o
3template, moves into after stirring in reactor, then puts into heating container reacting by heating, and last eccentric cleaning also collects product, obtains Fe
2o
3/ TiO
2nanometer nucleocapsid structure.
(3) TiO
2hollow nanostructured preparation:
By obtained Fe
2o
3/ TiO
2nano composite structure obtains TiO with aqueous hydrochloric acid etching at 60 ~ 70 DEG C
2hollow nanostructured.
In the present invention, Heating temperature is 180 ~ 220 DEG C, and the reaction times is 8 ~ 15h.
In the present invention, Fe
2o
3/ TiO
2nanometer nucleocapsid structure is about 450 ~ 500nm, diameter about 180 ~ 220nm.
In the present invention, for making Fe
2o
3template etching completely, does not destroy the TiO being coated on its surface simultaneously
2shell, obtains pure and complete hollow nanostructured material, need by 0.01 ~ 0.02g Fe
2o
3/ TiO
2it is in 5 ~ 7M aqueous hydrochloric acid that nano composite structure joins 20mL concentration, and etches 7 ~ 9h at 60 ~ 70 DEG C.
The present invention is with TiF
4for titanium source, ethylene glycol and Glacial acetic acid are solvent, spheroid shape Fe
2o
3nanoparticle is template, adopts the template that accurately can control nanotopography, by changing TiF
4the processing condition such as concentration, Glacial acetic acid content, temperature, heat-up time, prepare by one dimension TiO
2it is hollow nanostructured that nanometer rod is constructed, and it is about 450 ~ 500nm, and diameter is 180 ~ 220nm about; Nano surface rod is about 70 ~ 100nm, and diameter is about 10nm.TiO prepared by the present invention
2hollow nanostructured have the features such as size is controlled, simple to operate, raw material is easy to get, with low cost, has potential application prospect in the field such as environment, the energy.
Accompanying drawing explanation
Fig. 1 is gained TiO in the embodiment of the present invention 1
2hollow nanostructured SEM picture;
Fig. 2 is gained TiO in the embodiment of the present invention 1
2hollow nanostructured TEM picture;
Fig. 3 is gained TiO in the embodiment of the present invention 1
2hollow nanostructured XRD figure sheet.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited thereto; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment 1
(1) α-Fe
2o
3nanoneedle Template preparation: take 0.2703g FeCl with beaker
3, add 45ml deionized water ultrasonic vibration, after short its fully dissolves, add the NaH of 5ml 3.5mM concentration
2pO
4the aqueous solution.Reaction soln is placed in reagent bottle to take out with room temperature to be down to after 105 DEG C of thermostatically heating 48h, collection bottom settlings deionized water and ethanol are with 7000r/min rotating speed eccentric cleaning repeatedly.Product after centrifugal is collected at 60 DEG C of oven drying at low temperatures, is Fe
2o
3nanoneedle template.
(2) Fe
2o
3/ TiO
2prepared by nanometer nucleocapsid structure: by 0.099g TiF
4powder is dissolved in the ethylene glycol of 40ml, i.e. 20mM TiF
4solution, adds 5ml glacial acetic acid again and stirs, by the Fe that step (1) obtains after dissolution of solid is complete
2o
3nanoneedle 0.02g adds in above-mentioned solution, after stirring 3h, solution is put into reactor with 200 DEG C of thermostatically heating 15h; After taking out reactor, bottom settlings deionized water and ethanol are collected so that 5000r/min rotating speed eccentric cleaning is repeatedly dry afterwards, is Fe
2o
3/ TiO
2nano composite structure.
(3) TiO
2hollow nanostructured preparation: take the Fe that 0.02g step (2) obtains
2o
3/ TiO
2in reagent bottle, then be that 6M aqueous hydrochloric acid adds in reagent bottle by 20mL concentration, with putting it at 60 DEG C of heating 8h in baking oven after ultrasonic oscillation dispersion, after taking out, same step (2) eccentric cleaning is also dry collects product, is the TiO finally obtained
2hollow nanostructured.
Fig. 1 is the TiO that the present embodiment obtains
2hollow nanostructured scanning electron microscope (SEM) picture, as can be seen from the figure TiO
2hollow nanostructured size uniformity, regular shape.Each particle is constructed by upright nanometer rod and is formed.
Fig. 2 is the TiO that the present embodiment obtains
2hollow nanostructured transmission electron microscope (TEM) picture, as can be seen from the figure Fe after over etching
2o
3/ TiO
2the core of nanometer nucleocapsid structure is dissolved completely, obtains hollow TiO
2, and TiO
2there is not obvious change in hollow nanostructured surface topography, nanorod structure is complete, is about 60nm, and diameter is about 10nm, is consistent with SEM figure.
Fig. 3 is hollow TiO
2the XRD figure of nanometer powder.Can see from XRD figure and occur the characteristic diffraction peak such as (110), (101), (111), (211), with Rutile Type TiO
2the standard diagram of (PDF 87-0920) coincide, and inclusion-free peak.Fe is described
2o
3etching completely, conforms to expection.
Embodiment 2
The present embodiment is as different from Example 1: TiF in step (2)
4concentration changes 5 into, 10,15,25,30,40mM, other is identical with embodiment 1.Along with TiF
4the increase of concentration, nanometer rod becomes large gradually.This is mainly due to the Ti of solution
4+solubility increases and accelerates its speed of growth.
Embodiment 3
The present embodiment is as different from Example 1: in step (2), Glacial acetic acid content changes 1,2,3,4,6,7,9 mL into, and other is identical with embodiment 1.The result obtained is along with Glacial acetic acid content increases, TiO
2nanometer rod by short elongated and after acquiring a certain degree change little, but nanorod diameter continues to increase.Illustrate that Glacial acetic acid is to TiO
2nanorod growth has regulating and controlling effect.
Embodiment 4
The present embodiment is as different from Example 1: in step (2), Heating temperature changes 180,220 DEG C into, and other is identical with embodiment 1.The result obtained is the Fe when temperature is 180 DEG C
2o
3surface is without obvious bar-shaped TiO
2growth; When temperature is 220 DEG C, TiO
2nanorod diameter becomes large, Fe
2o
3/ TiO
2nano composite structure diameter obviously increases.
Embodiment 5
The present embodiment is as different from Example 1: in step (2) heat-up time change 1 into, 3,5,8,10,20h, other is identical with embodiment 1.The result obtained be when heated between for 5h time TiO
2nanometer rod just starts forming core growth, and thereafter along with the time increases, nanometer rod is slowly thicker, and length is increased to and to a certain degree remains unchanged afterwards.
Claims (4)
1. one kind by TiO
2the hollow nanostructured preparation method that nanometer rod is constructed, is characterized in that described method steps is as follows:
(1) Fe
2o
3the preparation of template:
By a certain amount of FeCl
3with deionized water dissolving, then add a certain amount of NaH
2pO
4the aqueous solution, FeCl
3with NaH
2pO
4concentration ratio be 100:1.5 ~ 2, move in reactor, at 100 ~ 110 DEG C of heating 48h, obtained spheroid shape Fe
2o
3nanoparticle template;
(2) Fe
2o
3/ TiO
2prepared by nanometer nucleocapsid structure:
By a certain amount of TiF
4powder is dissolved in 40 mL ethylene glycol, control TiF
4in ethylene glycol solution, concentration is 5 ~ 40mM, then adds 2 ~ 8mL glacial acetic acid and 0.02gFe successively
2o
3template, moves into after stirring in reactor, then puts into heating container reacting by heating, and last eccentric cleaning also collects product, obtains Fe
2o
3/ TiO
2nanometer nucleocapsid structure;
(3) TiO
2hollow nanostructured preparation:
By obtained Fe
2o
3/ TiO
2nano composite structure obtains TiO with aqueous hydrochloric acid etching at 60 ~ 70 DEG C
2hollow nanostructured.
2. according to claim 1 by TiO
2the hollow nanostructured preparation method that nanometer rod is constructed, it is characterized in that described Heating temperature is 180 ~ 220 DEG C, the reaction times is 8 ~ 15h.
3. according to claim 1 by TiO
2the hollow nanostructured preparation method that nanometer rod is constructed, is characterized in that described Fe
2o
3/ TiO
2nanometer nucleocapsid structure long 450 ~ 500nm, diameter 180 ~ 220nm.
4. according to claim 1 by TiO
2the hollow nanostructured preparation method that nanometer rod is constructed, is characterized in that the concrete grammar of described step 4 is as follows: by 0.01 ~ 0.02g Fe
2o
3/ TiO
2it is in 5 ~ 7M aqueous hydrochloric acid that nano composite structure joins 20mL concentration, and etches 7 ~ 9h at 60 ~ 70 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517353A (en) * | 2016-11-02 | 2017-03-22 | 绥化学院 | Preparation method of alpha-Fe2O3/TiO2 nano-composite gas sensing material |
| CN109052466A (en) * | 2018-11-07 | 2018-12-21 | 浙江大学台州研究院 | The method for preparing Nano grade titanium dioxide stud |
| CN110615470A (en) * | 2019-10-16 | 2019-12-27 | 浙江大学台州研究院 | One-dimensional metal-doped rutile titanium dioxide nanowire and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994558A (en) * | 2006-12-19 | 2007-07-11 | 武汉理工大学 | Method for preparing unidimensional TiO2 hollow structured photocatalyst using vanadium oxide nanobelt as template |
| CN104576074A (en) * | 2015-01-09 | 2015-04-29 | 哈尔滨工业大学 | Preparation method for ultra-long TiO2 nanowire array thin-film photo-anode |
-
2015
- 2015-05-04 CN CN201510220121.1A patent/CN104773757A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994558A (en) * | 2006-12-19 | 2007-07-11 | 武汉理工大学 | Method for preparing unidimensional TiO2 hollow structured photocatalyst using vanadium oxide nanobelt as template |
| CN104576074A (en) * | 2015-01-09 | 2015-04-29 | 哈尔滨工业大学 | Preparation method for ultra-long TiO2 nanowire array thin-film photo-anode |
Non-Patent Citations (1)
| Title |
|---|
| 尹贻超: "电磁流变双功能纳米复合材料的制备及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517353A (en) * | 2016-11-02 | 2017-03-22 | 绥化学院 | Preparation method of alpha-Fe2O3/TiO2 nano-composite gas sensing material |
| CN109052466A (en) * | 2018-11-07 | 2018-12-21 | 浙江大学台州研究院 | The method for preparing Nano grade titanium dioxide stud |
| CN110615470A (en) * | 2019-10-16 | 2019-12-27 | 浙江大学台州研究院 | One-dimensional metal-doped rutile titanium dioxide nanowire and preparation method thereof |
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Application publication date: 20150715 |