CN105800679B - A kind of TiO2The preparation method of spherical three-level hierarchy - Google Patents
A kind of TiO2The preparation method of spherical three-level hierarchy Download PDFInfo
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- CN105800679B CN105800679B CN201610130114.7A CN201610130114A CN105800679B CN 105800679 B CN105800679 B CN 105800679B CN 201610130114 A CN201610130114 A CN 201610130114A CN 105800679 B CN105800679 B CN 105800679B
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- tio
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- metal oxide
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of TiO2The preparation method of spherical three-level hierarchy.Concretely comprise the following steps：(1) by TiO2Nano particle, other metal oxide nanoparticles and polyethylene glycol are well mixed by the method for ball milling, obtain TiO2With other metal oxide nanoparticles and the mixed-powder of polyethylene glycol；(2) slurry is prepared using above-mentioned powder, stirred, film or bulk are obtained on substrate after drying；(3) calcining removes organic matter, obtains TiO2The spherical secondary hierarchy that nano particle and other metal oxide nanoparticles are formed；(4) other metal oxide nanoparticles are removed from spherical secondary hierarchy, that is, obtain TiO2Spherical three-level hierarchy.The preparation method cost of the present invention is low, easily operated, pollution-free, in high volume can quickly produce, and has extensive use in fields such as photocatalysis, sensing, pollution control, self-cleaning coatings.
Description
Technical field
The present invention relates to a kind of TiO2The preparation method of spherical three-level hierarchy, belongs to Nano/micron fine structure material
Extremely technology of preparing.
Background technology
The preparation of the spherical hierarchy of metal oxide and its regulation and control of series are a skills with important application background
Art.Such as its photocatalytic activity can be improved by adding a certain proportion of iron oxide in titanium dioxide, contained by adding difference
The iron oxide of amount can be controlled to the color of film coating because the Superhydrophilic of material in itself, therefore can be used as decoration and
Self-cleaning coating；The spherical compound of titanium dioxide and zinc oxide or tin oxide can be used as the material of semiconductor transducer.
The compound of multi-component can integrate the performance advantage of each constituent element, realize that performance enhancement and application are wider, lead in addition
Regulation and control to its series are crossed without changing spherical structure, completely maintain the advantage of spherical structure, make it in photoelectric field,
Waste gas wastewater treatment, self-cleaning coating etc. are widely used.
The content of the invention
It is an object of the invention to provide easily operated, the cheap TiO of cost of one kind2The preparation side of spherical three-level hierarchy
Method.
The spherical three-level hierarchy of the present invention is made up of following structure：By TiO2The micron-size spherical knot that particle is formed
The nano-TiO formed after other metal oxides is removed in structure, micron-size spherical structure2Structure, nano-TiO2Particle is in itself
Nanostructured.The TiO2The preparation method of spherical three-level hierarchy comprises the following steps：
(1) by TiO2Nano particle, other metal oxide nanoparticles and polyethylene glycol are mixed by the method for ball milling
Close uniform, acquisition TiO2With other metal oxide nanoparticles and the mixed-powder of polyethylene glycol；
(2) slurry is prepared using above-mentioned powder, stirred, film or bulk are obtained on substrate after drying；
(3) calcining removes organic matter, obtains TiO2Nano particle and other metal oxide nanoparticles form spherical
Two level hierarchy；
(4) other metal oxides are removed using the method for dissolving or reaction from spherical secondary hierarchy to receive
Rice grain, that is, obtain TiO2Spherical three-level hierarchy.
Described TiO2Nano particle diameter is 2~100 nanometers, and other metal oxide nanoparticles particle diameters are 2-100
Nanometer.
Described other metal oxides are iron oxide, nickel oxide, cupric oxide, silver oxide, magnesia, zinc oxide or oxygen
Change one or several kinds of combinations in tin.
The present invention compared with prior art, has advantages below：(1) provide that a kind of new to prepare nano-metal-oxide more
The preparation method of level structure；(2) material requested can easily be prepared by regulating and controlling the content ratio of each metal oxide；(3)
The inventive method realizes the regulation and control to compound series while spherical structure is kept；(4) technique is easily operated, is not required to
Equipments and devices that will be complicated, cost are low；(5) it is pollution-free, high production, in high volume can quickly it produce, it is dirty in photocatalysis, sensing
Dye is administered, and the field such as self-cleaning coating has extensive use.
Brief description of the drawings
Fig. 1 is titanium dioxide and its prepared spherical secondary hierarchy is mixed with 10% Zinc oxide nanoparticle；
Fig. 2 is the TiO obtained after Zinc oxide nanoparticle is removed2Spherical three-level hierarchy.
Embodiment
Embodiment 1：
By mass ratio 1:0.02 grain diameter is 2 nanometers of TiO2Nano particle and the oxidation that particle diameter is 2 nanometers
Iron nano-particle mix, then again the polyethylene glycol with molecular weight 20000 according to 3:1 mass ratio is mixed by the method for ball milling
Uniformly, TiO is obtained2With ferric oxide nanometer particle and the mixed-powder of polyethylene glycol；Slurry is prepared using above-mentioned powder, stirring is equal
It is even, film or bulk are obtained on substrate after drying；Calcining removes organic matter at 450 DEG C, obtains TiO2Nano particle and oxygen
Change the spherical secondary hierarchy of iron nano-particle.By dissolving with hydrochloric acid, reaction removes ferric oxide nanometer particle, obtains TiO2's
Spherical three-level hierarchy.
Embodiment 2：
By mass ratio 1:0.04 grain diameter is 100 nanometers of TiO2Nano particle and particle diameter are 100 nanometers
Nickel oxide nanoparticle mix, then again the polyethylene glycol with molecular weight 20000 according to 3:The method that 1 mass ratio passes through ball milling
It is well mixed, obtain TiO2With nickel oxide nanoparticle and the mixed-powder of polyethylene glycol；Slurry is prepared using above-mentioned powder, is stirred
Mix uniformly, film or bulk are obtained on substrate after drying；Calcining removes organic matter at 450 DEG C, obtains TiO2Nano particle
With the spherical secondary hierarchy of nickel oxide nanoparticle.Dissolved by dilute sulfuric acid and remove nickel oxide nanoparticle, obtain TiO2
Spherical three-level hierarchy.
Embodiment 3：
By mass ratio 1：0.1 grain diameter is 30 nanometers of TiO2Nano particle and the zinc oxide that particle diameter is 20 nanometers
Nano particle mix, then again the polyethylene glycol with molecular weight 20000 according to 3:1 mass ratio is mixed equal by the method for ball milling
It is even, obtain TiO2With Zinc oxide nanoparticle and the mixed-powder of polyethylene glycol；Slurry is prepared using above-mentioned powder, stirring is equal
It is even, film or bulk are obtained on substrate after drying；Calcining removes organic matter at 450 DEG C, obtains TiO2Nano particle and oxygen
Change the spherical secondary hierarchy of zinc nanoparticles.Above-mentioned Zinc oxide nanoparticle is removed by hydrochloric acid reaction, obtains TiO2's
Spherical three-level hierarchy.
Embodiment 4：
It is 1 by mass ratio：0.06 grain diameter is 50 nanometers of TiO2Nano particle and the oxygen that particle diameter is 60 nanometers
Change copper nano particles mixing, then again the polyethylene glycol with molecular weight 20000 according to 3:1 mass ratio is mixed by the method for ball milling
Close uniform, acquisition TiO2With copper oxide nanometer particle and the mixed-powder of polyethylene glycol；Slurry, stirring are prepared using above-mentioned powder
Uniformly, film or bulk are obtained on substrate after drying；Calcining removes organic matter at 450 DEG C, obtains TiO2Nano particle and
The spherical secondary hierarchy of copper oxide nanometer particle.Above-mentioned copper oxide nanometer particle is removed by sulfuric acid dissolution, reaction etc., obtained
Obtain TiO2Spherical three-level hierarchy.
Embodiment 5：
It is 1 by mass ratio:0.08 grain diameter is 40nm TiO2Nano particle and the oxidation that grain diameter is 80 nanometers
Magnesium nano particle mix, then again the polyethylene glycol with molecular weight 20000 according to 3:1 mass ratio is mixed by the method for ball milling
Uniformly, TiO is obtained2With magnesium oxide nanoparticle and the mixed-powder of polyethylene glycol；Slurry is prepared using above-mentioned powder, stirring is equal
It is even, film or bulk are obtained on substrate after drying；Organic matter is calcined away at 450 DEG C, obtains TiO2 nano particles and oxygen
Change the spherical secondary hierarchy of magnesium nano particle.Above-mentioned magnesium oxide nanoparticle is removed by dissolving with hydrochloric acid, reaction, obtained
TiO2Spherical three-level hierarchy.
Embodiment 6：
It is 1 by mass ratio:0.15 grain diameter is 100nm TiO2Nano particle and the oxidation that grain diameter is 70 nanometers
Silver nano-grain mix, then again the polyethylene glycol with molecular weight 20000 according to 3:1 mass ratio is mixed by the method for ball milling
Uniformly, TiO is obtained2With oxidation silver nano-grain and the mixed-powder of polyethylene glycol；Slurry is prepared using above-mentioned powder, stirring is equal
It is even, film or bulk are obtained on substrate after drying；Organic matter is calcined away at 450 DEG C, obtains TiO2Nano particle and oxygen
Change the spherical secondary hierarchy of silver nano-grain.Above-mentioned oxidation silver nano-grain is removed by dissolving with hydrochloric acid, reaction, obtained
TiO2Spherical three-level hierarchy.
Embodiment 7：
It is 1 by mass ratio:The TiO2 nano particles that 0.2 grain diameter is 100nm and the oxidation that grain diameter is 100 nanometers
Silver nano-grain mix, then again the polyethylene glycol with molecular weight 20000 according to 3:1 mass ratio is mixed by the method for ball milling
Uniformly, TiO2 is obtained with aoxidizing the mixed-powder of silver nano-grain and polyethylene glycol；Slurry is prepared using above-mentioned powder, stirring is equal
It is even, film or bulk are obtained on substrate after drying；Organic matter is calcined away at 450 DEG C, obtains TiO2 nano particles and oxygen
Change the spherical secondary hierarchy of silver nano-grain.Above-mentioned oxidation silver nano-grain is removed by dissolving with hydrochloric acid, reaction, obtained
TiO2 spherical three-level hierarchy.
Embodiment 8：
Zinc oxide and ferric oxide nanometer particle that grain diameter is 30nm are mixed, are 1 according to mass ratio:0.1 by particle
Particle diameter is 30 nanometers of TiO2Nano particle and said mixture mixing, then again with the polyethylene glycol of molecular weight 20000 according to
3:1 mass ratio is well mixed by the method for ball milling, obtains TiO2With zinc oxide, ferric oxide nanometer particle and polyethylene glycol
Mixed-powder；Slurry is prepared using above-mentioned powder, is stirred, film or bulk are obtained on substrate after drying；At 450 DEG C
Calcining removes organic matter, obtains TiO2The spherical secondary hierarchy of nano particle and zinc oxide and ferric oxide nanometer particle.It is logical
Persalt dissolving removes above-mentioned zinc oxide and ferric oxide nanometer particle, obtains TiO2Spherical three-level hierarchy.
Embodiment 9：
Magnesia and tin oxide nanoparticles that particle diameter is 50 nanometers are mixed, are 1 according to mass ratio:0.05 general
The TiO that grain particle diameter is 40 nanometers2Nano particle and said mixture mixing, then the polyethylene glycol again with molecular weight 20000 is pressed
According to 3:1 mass ratio is well mixed by the method for ball milling, obtains TiO2With magnesia, tin oxide nanoparticles and polyethylene glycol
Mixed-powder；Slurry is prepared using above-mentioned powder, is stirred, film or bulk are obtained on substrate after drying；At 450 DEG C
Lower calcining removes organic matter, obtains TiO2The spherical secondary hierarchy of nano particle and magnesia and tin oxide nanoparticles.
Above-mentioned magnesia and tin oxide nanoparticles are removed by dissolving with hydrochloric acid, reaction etc., obtain TiO2Spherical three-level hierarchy.
Embodiment 10：
Zinc oxide, iron oxide and magnesium oxide nanoparticle that grain diameter is 30nm are mixed, are 1 according to mass ratio:0.2
By the TiO that grain diameter is 50 nanometers2Nano particle and said mixture mixing, the then poly- second two with molecular weight 20000 again
Alcohol is according to 3:1 mass ratio is well mixed by the method for ball milling, obtains TiO2With zinc oxide, iron oxide, bitter earth nano
The mixed-powder of grain and polyethylene glycol；Using above-mentioned powder prepare slurry, stir, dry after obtained on substrate film or
Bulk；Calcining removes organic matter at 450 DEG C, obtains TiO2The spherical secondary of nano particle and magnesium oxide nanoparticle is classified
Structure.Above-mentioned zinc oxide, iron oxide and magnesium oxide nanoparticle are removed by dissolving with hydrochloric acid, reaction, obtain TiO2Spherical three
Level hierarchy.
Claims (2)
- A kind of 1. TiO2The preparation method of spherical three-level hierarchy, it is characterised in that comprise the following steps：(1) by TiO2Nano particle, other metal oxide nanoparticles and polyethylene glycol are mixed equal by the method for ball milling It is even, obtain TiO2With other metal oxide nanoparticles and the mixed-powder of polyethylene glycol；Described other metal oxides For the one or several kinds combination in iron oxide, nickel oxide, cupric oxide, silver oxide, magnesia, zinc oxide or tin oxide；(2) slurry is prepared using above-mentioned powder, stirred, film or bulk are obtained on substrate after drying；(3) calcining removes organic matter, obtains TiO2The spherical secondary point that nano particle and other metal oxide nanoparticles are formed Level structure；(4) other metal oxide nanoparticles are removed from spherical secondary hierarchy, that is, obtain TiO2Spherical three fraction Level structure.
- A kind of 2. TiO according to claim 12The preparation method of spherical three-level hierarchy, it is characterised in that described TiO2Nano particle diameter is 2~100 nanometers, and other metal oxide nanoparticles particle diameters are 2-100 nanometers.
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| CN107603425A (en) * | 2017-09-25 | 2018-01-19 | 常州市协旺纺织品有限公司 | A kind of preparation method of Superhydrophilic coating |
| CN108097181B (en) * | 2017-12-19 | 2020-05-19 | 东北大学 | Method for preparing indium oxide shell structure and product |
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