CN106186060B - A kind of diameter is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm - Google Patents
A kind of diameter is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm Download PDFInfo
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Abstract
The present invention provides the preparation method that a kind of diameter is less than the ultra-fine hollow titanium dioxide nano-spheres of 100nm, provides nano carbon microsphere particle as template；Nano carbon microsphere particle (CSs) template of different-grain diameter is evenly dispersed in organic solvent respectively, form carbon ball sol system, the tetra-n-butyl titanate solution through organic solvent diluting is then added dropwise respectively, reaction obtains the nanometer CSs@TiO of wall thickness and size tunable2Colloidal sol；The above-mentioned CSs@TiO of centrifugal treating2Gained solid content is dried and is calcined by colloidal sol, and the residue of final calcining gained is target product；The method of the present invention realize sphere is complete, monodispersity is good, storage-stable, grain size 100nm or less, the wall thickness uniform controllable titanium dioxide hollow nanosphere within 10nm preparation；Whole preparation process is easy to operate, and controllability is strong, reproducible, and mould material derives from a wealth of sources and cheap, and production cost is relatively low and safety and environmental protection, is suitble to large-scale production.
Description
Technical field
The application belongs to a kind of nanoparticle preparation field, is less than 100nm ultra-fine hollow two more particularly to a kind of diameter
The preparation method of TiOx nano ball.
Background technology
As a kind of specific surface area, high, low density nano semiconductor material, hollow titanium dioxide nano-sphere not only have
The features such as good permeability, characterization of adsorption, high stability, nontoxicity, the transparency, photocatalytic, especially less than 100nm's
In nanometer confinement, ultra-fine hollow titanium dioxide nano-sphere has apparent quantum effect and skin effect.It is directed not only to physics,
A variety of subjects such as chemistry, material, biology, and be owned by widely in terms of photoelectric device, molecular detection, biomedicine and catalysis
Application value and foreground, such as biological controlled drug transport, medical diagnosis on disease, micro-nano container, biological capsule, fuel cell.Currently,
Preparation method about hollow titanium dioxide nano-sphere has many document reports, these methods include mainly hard template method, soft mode
Plate method and non-template method.Wherein, template is applied relatively broad, ripe, and the monodispersity of grain size is preferable, and template is easy
Removal.
In template, soft template method mainly uses microemulsion particles, surfactant, supermolecule micella, polyphosphazene polymer
Object vesica even bubble is closed as template and prepares titanium dioxide hollow microballoon.Due to template form be difficult to control and it is unstable,
Not only pattern differs titanium dioxide hollow microballoon prepared by this method, and monodispersity and regularity are all poor, meanwhile, this preparation
A large amount of reverse micelle and reverse microemulsion, solution pollute the environment involved in process, therefore this method is limited primarily at present
Laboratory research, be not appropriate for large-scale production application (Chem.Rev., 2012,2373；Chem.Soc.Rev., 2011,
5472；J.Phys.Chem.B, 2004,3492.).
Hard template method is to prepare the most direct effective method of hollow titanium dioxide microballoon, because of the hollow Nano particle of its preparation
With good regularity, and entire experiment controllability is good.But traditional hard template method mainly uses the materials conduct such as polymer
Mould material not only uses a large amount of organic solvent and catalyst in the preparation process of template, but also the template of gained is often
There are agglomerations, and addition exhibiting high surface activating agent is needed to be alleviated, meanwhile, in order to enable Shell Materials are well wrapped
Cover, these templates need to additionally carry out surface active toward contact, and this method be difficult to obtain 100nm hereinafter, and monodispersity it is good
Good, grain size and the controllable titanium dioxide hollow nanosphere of wall thickness (J.Am.Chem.Soc., 2005,3928；Chem., 2006,
749；J.Colloid.Interface Sci., 2006,370；Langmuir., 2001,3579.).
Invention content
For the prior art from deficiency, that the purpose of the present invention is to provide a kind of monodispersities is good, storage-stable,
Grain size and the controllable diameter of wall thickness are less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm.
The present invention uses following scheme in order to achieve the above objectives：
A kind of diameter is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, includes the following steps：
S1, provide grain size 20-90nm nano carbon microsphere template；
S2, the nano carbon microsphere template of step s1 is dispersed in absolute ethyl alcohol, and deionized water is added and forms nanometer
Carbon ball sol system, while being placed in 60 DEG C of water-bath and accompanying by lasting high-speed stirred, be then added dropwise under this condition through
The diluted tetra-n-butyl titanate weak solution of absolute ethyl alcohol, reaction response 2-10h obtain the CSs@TiO of wall thickness and size tunable2It is molten
Glue；
The CSs@TiO that s3, centrifugal treating step s2 are obtained2Colloidal sol, and the solid content that sub-argument is gone out carries out drying and processing,
Gained block carries out high-temperature calcination after then drying, and is warming up to 400-800 DEG C with 20 DEG C/min or less, soaking time 1-
6h, gained powder is target product after calcining, and the grain size of target product is 20-90nm.
Further, the nano carbon microsphere template is that glucose carries out hydro-thermal reaction acquisition as carbon source.
Further, in the step s2, in tetra-n-butyl titanate weak solution, absolute ethyl alcohol and tetra-n-butyl titanate original solution
Volume ratio be 100 times or more.
Further, in the step s3 when centrifugal treating, speed is in 20000r/min or more, and the time is in 10min or more.
Further, drying and processing, drying temperature are 60 DEG C hereinafter, drying time period is in vacuum drying oven in the step s3
6h or more.
Further, the step s3 high temperature calcination atmospheres are air.
Further, the wall thickness of target product titanium dioxide nano-sphere is 2-5nm.
Diameter of the present invention is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, with realize sphere circle it is complete,
Monodispersity is good, storage-stable, grain size and the controllable hollow titanium dioxide nano-sphere of wall thickness preparation method.Simultaneously to having
The condition of method optimizes, and while ensureing final product quality, preferentially the selection reaction time is short as possible, the prices of raw materials are low
Experiment condition honest and clean, reaction step is few improves production efficiency, reduces production cost, and overcomes previous preparation small size carbon ball
In the problems such as easily reuniting, be conducive to prepare with scale and practical application.
Compared with the prior art, the advantages of the present invention are as follows：The present invention is in lower temperature and ball is realized in the short period
Body is complete, monodispersity is good, storage-stable, grain size in 100nm hereinafter, ultra-fine hollow titanium dioxide of the wall thickness in 2-5nm is received
Rice ball.And the diameter of nanosphere can be regulated and controled in 20-90nm.And the prices of raw materials are cheap, preparation time is short, improve life
Efficiency is produced, production cost is reduced.
Although the method for the present invention, using hard template method, the carbon ball using grain size less than 100nm is template, is passed through
Stringent control experiment parameter is successfully realized grain size and is less than in the case where being added without any surfactant and catalyst
The preparation of the ultra-fine hollow titanium dioxide nano particle of 100nm.An important feature of nano-particle of the diameter less than 100nm be
Its size oneself close to or smaller than electronics mean free path and superconduction be concerned with wavelength, their larger specific surfaces make be in surface
Oneself is suitable with the atom inside the particle, number of electrons for the atom and number of electrons of state.Skin effect caused by this and
Quantum confined effect so that nano-particle is in optical property, electric property, mechanical property, catalytic performance, biological etc.
Reveal the characteristic that conventional material does not have.Therefore, ultra-fine hollow titanium dioxide nano-sphere of the diameter less than 100nm is in photoelectricity skill
The every field such as art, biotechnology, energy technology all have wide practical use.
Description of the drawings
Transmission electron microscope photos of the Fig. 1 by obtaining ultra-fine hollow titanium dioxide nano-sphere in the embodiment of the present invention 1；
Transmission electron microscope photos of the Fig. 2 by obtaining ultra-fine hollow titanium dioxide nano-sphere in the embodiment of the present invention 2；
Transmission electron microscope photos of the Fig. 3 by obtaining ultra-fine hollow titanium dioxide nano-sphere in the embodiment of the present invention 3；
Specific implementation mode
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The preparation method of the ultra-fine hollow titanium dioxide nano-sphere of the present invention, includes the following steps：
S1, provide grain size 20-90nm nano carbon microsphere template；
S2, nano carbon microsphere template described in step s1 is dispersed in absolute ethyl alcohol, and a certain amount of deionization is added
Water forms nano carbon microsphere sol system, while being placed in 60 DEG C of water-bath and accompanying by lasting high-speed stirred, then under this condition
The CSs@through the diluted tetra-n-butyl titanate weak solution of absolute ethyl alcohol, reaction 2h wall thickness achieved above and size tunable are added dropwise
TiO2Colloidal sol；
The CSs@TiO that s3, centrifugal treating step s2 are obtained2Colloidal sol, and the solid content that sub-argument is gone out carries out drying and processing,
Gained block carries out high-temperature calcination after then drying, and it is 400-800 DEG C that heating rate, which is 20 DEG C/min or less calcination temperatures,
1-6h is kept the temperature in Muffle furnace, calcination atmosphere is air；Gained powder is target product, the grain of said target product after calcining
Diameter is 20-90nm.
Preferably, in the step s1, the preparation process of the nano carbon microsphere template includes：Use glucose as carbon source
Hydro-thermal reaction is carried out, nano carbon microsphere is obtained.
Preferably, in the step s2, in tetra-n-butyl titanate weak solution, absolute ethyl alcohol and tetra-n-butyl titanate original solution
Volume ratio be 100 times or more.
Preferably, in the step s3, the condition of the centrifugal treating includes：Speed is in 20000r/min or more, time
In 10min or more.
Preferably, in the step s3, the drying and processing condition includes：Drying unit is vacuum drying oven, drying temperature
For 60 DEG C hereinafter, drying time period is 6h or more.
As one of preferable concrete application scheme, the diameter is less than the ultra-fine hollow titanium dioxide nano-spheres of 100nm
Preparation method specifically comprises the following steps：
S1, grain size is taken to be dispersed in formation nano carbon microsphere colloidal sol in absolute ethyl alcohol for the nano carbon microsphere template of 20-80nm；
S2, above-mentioned nano carbon microsphere colloidal sol is added to deionized water, and continues to stir energetically under conditions of 60 DEG C of water-bath, then
The tetra-n-butyl titanate weak solution after absolute ethyl alcohol dilutes is added dropwise, after tetra-n-butyl titanate weak solution is all added,
2-10h is reacted, grain size and the controllable nanometer CSs@TiO of wall thickness are obtained2Colloidal sol；
S3, by above-mentioned nanometer CSs@TiO2Colloidal sol centrifuges 10min or more with the centrifugal speed not less than 20000r/min, obtains
Obtain solid content；
S4, above-mentioned solid content is placed in vacuum drying oven, with the Temperature Treatment 6h or more not higher than 60 DEG C, is obtained dry solid
Body；
S5, above-mentioned drying solid is placed in Muffle furnace, under air atmosphere, is heated up with 20 DEG C/min heating rates below
To 400-800 DEG C and 1-6h is kept the temperature, obtains hollow titanium dioxide nano-sphere.
The wall thickness of the hollow titanium dioxide nano-sphere is in 2-5nm.
Embodiment 1
S1, to take grain size be that the nano carbon microsphere template 20mg of 20-40nm is dispersed in 60mL absolute ethyl alcohols and forms nano carbon microsphere
Colloidal sol；
S2, above-mentioned nano carbon microsphere colloidal sol is added to 120 μ L deionized waters, and continues to stir energetically under conditions of 60 DEG C of water-bath
It mixes, then the tetra-n-butyl titanate weak solution after absolute ethyl alcohol dilutes is added dropwise (150 μ L of tetra-n-butyl titanate original solution are dissolved in
In 20mL absolute ethyl alcohols), after tetra-n-butyl titanate weak solution is all added, 2-10h is reacted, obtains grain size and wall thickness is controllable
Nanometer CSs@TiO2Colloidal sol；
S3, by above-mentioned nanometer CSs@TiO2Colloidal sol centrifuges 15min with the centrifugal speed of 30000r/min, obtains solid content；
S4, above-mentioned solid content is placed in vacuum drying oven, 40 DEG C of Temperature Treatment 12h, obtains drying solid；
S5, above-mentioned drying solid is placed in Muffle furnace, under air atmosphere, 550 is warming up to the heating rate of 2 DEG C/min
DEG C and keep the temperature 3h, obtain hollow titanium dioxide nano-sphere.
Fig. 1 show the transmission electron microscope photo for the carbon ball that embodiment 1 is obtained, as can be seen from Figure, hollow titanium dioxide
A diameter of 30-40nm of titanium nanosphere, wall thickness are about 2nm.
Embodiment 2
S1, to take grain size be that the nano carbon microsphere template 20mg of 30-60nm is dispersed in 60mL absolute ethyl alcohols and forms nano carbon microsphere
Colloidal sol；
S2, above-mentioned nano carbon microsphere colloidal sol is added to 120 μ L deionized waters, and continues to stir energetically under conditions of 60 DEG C of water-bath
It mixes, then the tetra-n-butyl titanate weak solution after absolute ethyl alcohol dilutes is added dropwise (150 μ L of tetra-n-butyl titanate original solution are dissolved in
In 20mL absolute ethyl alcohols), after tetra-n-butyl titanate weak solution is all added, 2-10h is reacted, obtains grain size and wall thickness is controllable
Nanometer CSs@TiO2Colloidal sol；
S3, by above-mentioned nanometer CSs@TiO2Colloidal sol centrifuges 15min with the centrifugal speed of 30000r/min, obtains solid content；
S4, above-mentioned solid content is placed in vacuum drying oven, 40 DEG C of Temperature Treatment 12h, obtains drying solid；
S5, above-mentioned drying solid is placed in Muffle furnace, under air atmosphere, 550 is warming up to the heating rate of 2 DEG C/min
DEG C and keep the temperature 3h, obtain hollow titanium dioxide nano-sphere.
Fig. 2 show the transmission electron microscope photo that embodiment 2 is obtained, and as can be seen from Figure, hollow titanium dioxide is received
The a diameter of 60nm, wall thickness 4nm of rice ball.
Embodiment 3
S1, to take grain size be that the nano carbon microsphere template 20mg of 60-90nm is dispersed in 60mL absolute ethyl alcohols and forms nano carbon microsphere
Colloidal sol；
S2, above-mentioned nano carbon microsphere colloidal sol is added to 120 μ L deionized waters, and continues to stir energetically under conditions of 60 DEG C of water-bath
It mixes, then the tetra-n-butyl titanate weak solution after absolute ethyl alcohol dilutes is added dropwise (150 μ L of tetra-n-butyl titanate original solution are dissolved in
In 20mL absolute ethyl alcohols), after tetra-n-butyl titanate weak solution is all added, 2-10h is reacted, obtains grain size and wall thickness is controllable
Nanometer CSs@TiO2Colloidal sol；
S3, by above-mentioned nanometer CSs@TiO2Colloidal sol centrifuges 15min with the centrifugal speed of 30000r/min, obtains solid content；
S4, above-mentioned solid content is placed in vacuum drying oven, 40 DEG C of Temperature Treatment 12h, obtains drying solid；
S5, above-mentioned drying solid is placed in Muffle furnace, under air atmosphere, 550 is warming up to the heating rate of 2 DEG C/min
DEG C and keep the temperature 3h, obtain hollow titanium dioxide nano-sphere.
Fig. 3 show the transmission electron microscope photo for the carbon ball that embodiment 3 is obtained, as can be seen from Figure, hollow titanium dioxide
The grain size of titanium nanosphere is 88nm, and wall thickness is 3-5nm or so.
Embodiment 4
S1, to take grain size be that the nano carbon microsphere template 20mg of 60-90nm is dispersed in 60mL absolute ethyl alcohols and forms nano carbon microsphere
Colloidal sol；
S2, above-mentioned nano carbon microsphere colloidal sol is added to 120 μ L deionized waters, and continues to stir energetically under conditions of 60 DEG C of water-bath
It mixes, then the tetra-n-butyl titanate weak solution after absolute ethyl alcohol dilutes is added dropwise (150 μ L of tetra-n-butyl titanate original solution are dissolved in
In 20mL absolute ethyl alcohols), after tetra-n-butyl titanate weak solution is all added, 2-10h is reacted, obtains grain size and wall thickness is controllable
Nanometer CSs@TiO2Colloidal sol；
S3, by above-mentioned nanometer CSs@TiO2Colloidal sol centrifuges 10min with the centrifugal speed of 40000r/min, obtains solid content；
S4, above-mentioned solid content is placed in vacuum drying oven, 60 DEG C of Temperature Treatment 6h, obtains drying solid；
S5, above-mentioned drying solid is placed in Muffle furnace, under air atmosphere, 400 is warming up to the heating rate of 2 DEG C/min
DEG C and keep the temperature 6h, obtain hollow titanium dioxide nano-sphere.
Embodiment 5
S1, to take grain size be that the nano carbon microsphere template 20mg of 60-90nm is dispersed in 60mL absolute ethyl alcohols and forms nano carbon microsphere
Colloidal sol；
S2, above-mentioned nano carbon microsphere colloidal sol is added to 120 μ L deionized waters, and continues to stir energetically under conditions of 60 DEG C of water-bath
It mixes, then the tetra-n-butyl titanate weak solution after absolute ethyl alcohol dilutes is added dropwise (150 μ L of tetra-n-butyl titanate original solution are dissolved in
In 20mL absolute ethyl alcohols), after tetra-n-butyl titanate weak solution is all added, 2-10h is reacted, obtains grain size and wall thickness is controllable
Nanometer CSs@TiO2Colloidal sol；
S3, by above-mentioned nanometer CSs@TiO2Colloidal sol centrifuges 20min with the centrifugal speed of 30000r/min, obtains solid content；
S4, above-mentioned solid content is placed in vacuum drying oven, 45 DEG C of Temperature Treatment 10h, obtains drying solid；
S5, above-mentioned drying solid is placed in Muffle furnace, under air atmosphere, 800 is warming up to the heating rate of 1 DEG C/min
DEG C and keep the temperature 1h, obtain hollow titanium dioxide nano-sphere.
The preparation of hollow titanium dioxide nano-sphere the method for the invention realizes grain size less than 100nm and size control,
Participation of the reaction process without toxic chemical can not only effectively avoid fault of construction and environmental pollution as caused by introducing impurity
Problem, simultaneously because the characteristic that the hollow titanium dioxide nano-sphere is nontoxic, can be widely used for biochemistry and biological diagnosis.Entirely
Preparation process is grasped, and is made simply, and controllability is strong, reproducible, is suitble to industrial production.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above is only the specific implementation mode of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection domain of the application.
Claims (5)
1. a kind of diameter is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, it is characterised in that including following step
Suddenly：
S1, provide grain size 20-40nm nano carbon microsphere template；
S2, the nano carbon microsphere template of step s1 is dispersed in absolute ethyl alcohol, and deionized water is added and forms nano carbon microsphere
Sol system, while being placed in 60 DEG C of water-bath and accompanying by lasting high-speed stirred, then it is added dropwise under this condition through anhydrous
The diluted tetra-n-butyl titanate weak solution of ethyl alcohol, reaction 2-10h obtain the CSs@TiO of wall thickness and size tunable2Colloidal sol；
The CSs@TiO that s3, centrifugal treating step s2 are obtained2Colloidal sol, and the solid content isolated is subjected to drying and processing, then
Gained block after drying is subjected to high-temperature calcination under air atmosphere, 400-800 DEG C is warming up to 20 DEG C/min or less, when heat preservation
Between 1-6h, gained powder is target product after calcining, and the grain size of target product is 20-40nm, and target product titanium dioxide is received
The wall thickness of rice ball is 2-5nm.
2. diameter as described in claim 1 is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, feature exists
In：The nano carbon microsphere template is that glucose carries out hydro-thermal reaction acquisition as carbon source.
3. diameter as described in claim 1 is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, feature exists
In：In the step s2, in tetra-n-butyl titanate weak solution, the volume ratio of organic solvent and tetra-n-butyl titanate original solution is
100 times or more.
4. diameter as described in claim 1 is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, feature exists
In：In the step s3 when centrifugal treating, speed is in 20000r/min or more, and the time is in 10min or more.
5. diameter as described in claim 1 is less than the preparation method of the ultra-fine hollow titanium dioxide nano-spheres of 100nm, feature exists
In：Drying and processing, drying temperature are 60 DEG C hereinafter, drying time period is 6h or more in vacuum drying oven in the step s3.
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