CN105883910A - Preparation method and product for perovskite SrTiO3 porous nano particles - Google Patents
Preparation method and product for perovskite SrTiO3 porous nano particles Download PDFInfo
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- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention relates to a preparation method for perovskite SrTiO3 porous nano particles. The preparation method comprises the following steps: 1) by taking titanium sulfate and potassium hydroxide as raw materials, preparing hydroxide precipitates of titanium; 2) separately preparing a strontium nitrate solution, a potassium hydroxide solution and a lithium nitrate solution; 3) mixing the hydroxide precipitates of titanium, the trontium nitrate solution, the potassium hydroxide solution and the lithium nitrate solution, carrying out hydrothermal reaction for 3-32 hours at a reaction temperature of 150-220 DEG C, centrifuging, and washing to obtain the perovskite SrTiO3 porous nano particles. The preparation process is simple, the shape of the porous structure is easy to control, the dimension is uniform, and the porous structure exists on the surface.
Description
Technical field
The present invention relates to inorganic material synthesis field, be specifically related to a kind of perovskite SrTiO3Porous nano
The preparation method of grain and product.
Background technology
In recent years research finds, the performance of nano material is the most influenced by their size, also by the shadow of its pattern
Ringing, therefore various patterns have been done substantial amounts of research by research worker.The preparation of nanostructured causes people
Pay close attention to greatly, the most only zero-dimension nano granule, monodimension nano stick, nanofiber and three-dimensional branch crystal,
Also there are many nano-particles self assemble Mesoporous Spheres, nanotube or nanometer sheet self-assembled nano structures etc..
Strontium titanates SrTiO3As one typical Ca-Ti ore type ternary oxide, not only there is dielectric constant
The advantages such as height, low, the Heat stability is good of dielectric loss, are widely used in electronics, machinery and ceramic industry,
And its energy gap is 3.2Ev, also by as a kind of excellent photocatalyst, it is applied to organic pollution
Photocatalytic degradation and the photocatalytic cleavage of water to prepare clean energy resource hydrogen.
In recent years, about the SrTiO with different-shape feature3Preparation and performance study cause people's
Great interest.Solid reaction process, the sedimentation method, sol-gel process and hydrothermal synthesis method are SrTiO3Conventional system
Preparation Method.Wherein first three methods is both needed to the calcining through higher temperature, and synthesized powder reuniting is serious,
And granule does not have well-regulated pattern.The open one of Chinese invention patent (publication number CN102320651A)
The preparation method of strontium titanate nano powder, weighs tetra-n-butyl titanate and strontium nitrate and adds to reaction vessel
In, add sodium hydroxide solution Glass rod and stir；Load heating rate heating in microwave reaction instrument；
After being down to room temperature, solution is poured out addition hydrochloric acid, then filters precipitation with deionized water cyclic washing, by institute
The precipitation obtained is placed in baking oven in 70 DEG C of drying, obtains strontium titanate nano powder.This preparation method uses
Microwave method prepares the strontium titanate nano powder of pure phase, but does not control SrTiO3Granule-morphology.
Chinese invention patent (publication number CN104098125A) discloses the system of a kind of strontium titanates nano cubic block
Preparation Method, the method is using titanium dioxide as titanium source, and solubility strontium salt, as strontium source, is made of sodium hydroxide
Acid-base modifier.First by titanium dioxide ultrasonic disperse in the middle of aqueous solution, then it is added to containing strontium
Soluble-salt, constantly stirring is allowed to dissolve, and adds alkali the most again, regulation suspension pH value to 8～14,
Finally suspension is put in reactor, carry out hydro-thermal reaction.Product is through washing, separate, doing
The dry strontium titanates nano cubic block obtaining regular appearance and size uniformity.The application patent system is for strontium titanates table
Face porous, is more beneficial for being adsorbed with organic pollutants, and photocatalysis effect is more excellent.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of perovskite SrTiO3Porous is received
The preparation method of rice grain and product, preparation process is simple, and the pattern of porous structural is prone to regulation and control, chi
Very little homogeneous and surface has pore passage structure.
The present invention solves the technical scheme of above-mentioned technical problem:
A kind of perovskite SrTiO3The preparation method of porous nano granule, comprises the following steps:
1) with titanium sulfate and potassium hydroxide as raw material, the hydroxide precipitation of titanium is prepared；
2) strontium nitrate solution, potassium hydroxide solution and lithium nitrate solution are prepared respectively；Described strontium nitrate is molten
The molar concentration 0.2～0.6mol/L of liquid, the molar concentration of potassium hydroxide solution is 1～3mol/L, lithium nitrate
Solution molar concentration 0.6～1mol/L；
3) the hydroxide precipitation of titanium, strontium nitrate solution, potassium hydroxide solution and lithium nitrate solution are mixed,
At reaction temperature is 150～220 DEG C, carry out hydro-thermal reaction 3～32h, centrifugal, then clean, obtain calcium
Titanium ore SrTiO3Porous nano granule；The hydroxide precipitation of described titanium, strontium nitrate solution, hydroxide
The mixed proportion of potassium solution and lithium nitrate solution is: 0.6～2g:5～10ml:10～15ml:5～10ml.
Technique scheme, with titanium sulfate and strontium nitrate as reaction mass, utilizes precipitant potassium hydroxide to promote
The generation of the hydroxide of titanium, doping lithium nitrate regulates and controls the growth of crystal simultaneously, finally achieves calcium titanium
Ore deposit SrTiO3The preparation of porous nano granule.Potassium hydroxide is highly basic, OH-Ion concentration is higher, and crystal is raw
The long symmetry easily deviateing its structure cell intrinsic, the surface, edges and corners of crystal grain can be higher simultaneously, in order to reduce
Surface energy, corner angle can form new granule, so gained granule corner is rounding off by dissolution precipitation.
Lithium ion can promote plane of crystal OH-Dehydration, upset the constituent of liquid level, reduce absorption resistance,
OH-Readily diffuse into crystals, OH during natural cooling-Ion escapes, and defines the structure of porous surface.
There is the perovskite SrTiO of the structure of porous surface3There is more excellent photocatalysis performance.
As preferably, described step 1) in prepare titanium the method for hydroxide precipitation be: prepare respectively
Molar concentration is titanium sulfate solution and the potassium hydroxide solution of 6～10mol/L of 0.15～0.5mol/L；By hydrogen
Potassium oxide solution is added drop-wise in titanium sulfate solution, is filtrated to get the hydroxide precipitation of titanium.
As further preferably, described step 1) in potassium hydroxide solution is added drop-wise in titanium sulfate solution,
Obtain the hydroxide precipitation of titanium, stand 15～20min, clean the hydroxide precipitation of titanium with deionized water
And centrifugal 4～5 times.
As further preferably, described rate of addition 2～4 drops/sec.By controlling rate of addition, enter one
Step controls SrTiO3The pattern of loose structure.
As preferably, described step 3) in reaction temperature be 160～180 DEG C, the response time is 3～6h.
As preferably, described step 3) in the hydroxide precipitation of titanium, strontium nitrate solution, hydroxide
The mixed proportion of potassium solution and lithium nitrate solution is: 0.6～0.8g:5～8ml:10～13ml:5～8ml.
As preferably, described step 3) in cleaning method be: by the product that is filtrated to get successively with dilute
Acetic acid, deionized water clean.Add spirit of vinegar to stir to presoma will be mixed into what carbon dioxide was formed
SrCO3Remove, clean with deionized water be nitrate ion in order to reaction mass is introduced, potassium ion and
The perovskite SrTiO of synthesis3Porous nano granule is sufficiently separated, and obtains the perovskite SrTiO of pure phase3Porous
Nano-particle.
As preferably, described step 1) in prepare titanium the method for hydroxide precipitation be: prepare respectively
Molar concentration is titanium sulfate solution and the potassium hydroxide solution of 5.5～6.5mol/L of 0.13～0.17mol/L；
By potassium hydroxide solution under stirring 2～3 drops/sec be added drop-wise in titanium sulfate solution, be filtrated to get titanium
Hydroxide precipitates；Described step 2) in the molar concentration 0.18～0.22mol/L of strontium nitrate solution, hydrogen
The molar concentration of potassium oxide solution is 0.9～1.1mol/L, lithium nitrate solution molar concentration 0.5～0.7mol/L；
Described step 3) in the hydroxide of 0.6～0.7g titanium is precipitated, 5～6ml strontium nitrate aqueous solution, 10～11ml
Potassium hydroxide solution and 5～6ml lithium nitrate solutions are mixed to join in reactor, protect at 160～170 DEG C
Temperature carries out heat treatment in 3～5 hours.Under the conditions described above, gained perovskite SrTiO3Porous nano knot
The pattern of structure is best, steady quality, and purity is high, powder granule good dispersion.
The present invention also provides for the perovskite SrTiO of a kind of above-mentioned preparation method synthesis3Porous nano granule.Institute
The perovskite SrTiO stated3The size of porous nano granule is 300～600nm.Described size is that porous is received
The circumscribed diameter of rice grain or the length of side of porous nano granule.The perovskite SrTiO prepared3Many
Hole nano-particle has above-mentioned beneficial effect equally.
Compared with the existing technology, beneficial effects of the present invention is embodied in:
(1) present invention process process is simple, it is easy to control, non-environmental-pollution, low cost, it is easy to scale
Metaplasia is produced.
(2) the perovskite SrTiO prepared3The nano-powder size of porous nano granule is between 300～600nm
And surface has loose structure.Product quality is stable, and purity is high, powder granule good dispersion.
Accompanying drawing explanation
Fig. 1 is the perovskite SrTiO of embodiment 1 synthesis3The X-ray diffractogram of porous nano granule；
Fig. 2 is the perovskite SrTiO of embodiment 1 synthesis3The scanning electron microscope diagram of porous nano granule；
Fig. 3 is the perovskite SrTiO of comparative example 1 synthesis3The scanning electron microscope diagram of porous nano granule；
Fig. 4 is the perovskite SrTiO of embodiment 1 synthesis3The degraded of porous nano pellet degradation methylene blue
Figure；
Fig. 5 be methylene blue from degraded figure.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing.
Embodiment 1
1) 4mmol titanium sulfate and 0.15mol potassium hydroxide are dissolved separately in deionized water, regulate sulfur
Molar concentration 0.15mol/L of acid titanium solution, the molar concentration of potassium hydroxide solution is 6mol/L.
2) being slowly added dropwise in titanium sulfate solution by potassium hydroxide solution under stirring, rate of addition is
2 drops/sec, it is thus achieved that the hydroxide precipitation of white titanium, stand 20min, be centrifuged 4～5 times.
3) strontium nitrate, potassium hydroxide and lithium nitrate are dissolved separately in deionized water, strontium nitrate mole
Concentration is 0.2mol/L, and the molar concentration of potassium hydroxide solution is 1mol/L, lithium nitrate solution mole dense
Degree is 0.6mol/L.
4) by the hydroxide precipitation of cleaned 0.6g titanium, 5ml strontium nitrate aqueous solution, 10ml hydroxide
Potassium solution and 5ml lithium nitrate solution are added separately in 50ml reactor, regulate cumulative volume with deionized water
For the 40% of reactor inner bag, after stirring 2h, at 160 DEG C, insulation carries out heat treatment in 4 hours.Then,
It is down to room temperature, takes out product, filter, clean with spirit of vinegar, deionized water successively, 60 DEG C of temperature
Lower drying, obtains perovskite SrTiO3Porous nano granule.
Synthesized perovskite SrTiO3The X-ray diffractogram of porous nano granule, as it is shown in figure 1, produce
Thing is the SrTiO of perovskite3Porous particle, does not has other impurity peaks, and the SrTiO that product is pure phase is described3。
Scanning electron microscope SEM photograph is as in figure 2 it is shown, prepared perovskite SrTiO3Porous nano
Particle size is between 300～600nm, and pattern is the porous cube of rounding off, and surface has loose structure.
Embodiment 2
1) 6mmol titanium sulfate and 0.2mol potassium hydroxide are dissolved separately in deionized water, regulate sulfur
Molar concentration 0.3mol/L of acid titanium solution, the molar concentration of potassium hydroxide solution is 8mol/L.
2) being slowly added dropwise in titanium sulfate solution by potassium hydroxide solution under stirring, rate of addition is
4 drops/sec, it is thus achieved that the hydroxide precipitation of white titanium, stand 20min, be centrifuged 4～5 times.
3) strontium nitrate, potassium hydroxide and lithium nitrate are dissolved separately in deionized water, strontium nitrate mole
Concentration is 0.4mol/L, and the molar concentration of potassium hydroxide solution is 2mol/L, lithium nitrate solution mole dense
Degree is 0.8mol/L.
4) by the hydroxide precipitation of cleaned 0.8g titanium, 8ml strontium nitrate aqueous solution, 13ml hydroxide
Potassium solution and 8ml lithium nitrate solution are added separately in 50ml reactor, regulate cumulative volume with deionized water
For the 40% of reactor inner bag, after stirring 2h, at 200 DEG C, insulation carries out heat treatment in 12 hours.So
After, it is down to room temperature, takes out product, be sequentially added into spirit of vinegar and deionized water is centrifuged 4～5 times, 60 DEG C
At a temperature of dry, obtain perovskite SrTiO3Porous nano granule.
Comparative example 1:
1) 6mmol titanium sulfate and 0.2mol potassium hydroxide are dissolved separately in deionized water, regulate sulfur
Molar concentration 0.3mol/L of acid titanium solution, the molar concentration of potassium hydroxide solution is 8mol/L.
2) being slowly added dropwise in titanium sulfate solution by potassium hydroxide solution under stirring, rate of addition is
4 drops/sec, it is thus achieved that the hydroxide precipitation of white titanium, stand 20min, be centrifuged 4～5 times.
3) strontium nitrate, potassium hydroxide being dissolved separately in deionized water, the molar concentration of strontium nitrate is
0.4mol/L, the molar concentration of potassium hydroxide solution is 2mol/L.
4) by the hydroxide precipitation of cleaned 0.8g titanium, 8ml strontium nitrate aqueous solution, 13ml hydroxide
Potassium solution is added separately in 50ml reactor, is reactor inner bag with deionized water regulation cumulative volume
40%, after stirring 2h, at 200 DEG C, insulation carries out heat treatment in 12 hours.Then, it is down to room temperature, takes
Go out product, be sequentially added into spirit of vinegar and deionized water is centrifuged 4～5 times, dry at a temperature of 60 DEG C.
Scanning electron microscope SEM photograph is as it is shown on figure 3, be ganoid elliposoidal SrTiO3Granule,
Perovskite SrTiO cannot be obtained3Porous nano granule.
Comparative example 2:
1) 4mmol titanium sulfate and 0.15mol potassium hydroxide are dissolved separately in deionized water, regulate sulfur
Molar concentration 0.15mol/L of acid titanium solution, the molar concentration of potassium hydroxide solution is 6mol/L.
2) being slowly added dropwise in titanium sulfate solution by potassium hydroxide solution under stirring, rate of addition is
2 drops/sec, it is thus achieved that the hydroxide precipitation of white titanium, stand 20min, be centrifuged 4～5 times.
3) strontium nitrate, tetramethyl aqua ammonia and lithium nitrate are dissolved separately in deionized water, strontium nitrate
Molar concentration be 0.2mol/L, the molar concentration of tetramethyl Dilute Ammonia Solution is 1mol/L, lithium nitrate
The molar concentration of solution is 0.6mol/L.
4) by the hydroxide precipitation of cleaned 0.6g titanium, 5ml strontium nitrate aqueous solution, 10ml tetramethyl
Aqua ammonia and 5ml lithium nitrate solution are added separately in 50ml reactor, overall with deionized water regulation
Amassing 40% for reactor inner bag, after stirring 2h, at 160 DEG C, insulation carries out heat treatment in 4 hours.So
After, it is down to room temperature, takes out product, filter, clean with spirit of vinegar, deionized water successively, 60 DEG C
At a temperature of dry.It is demonstrated experimentally that perovskite SrTiO cannot be obtained3Porous nano granule.
Degradation of methylene blue performance test:
10-5The methylene blue solution of the 100mL of mol/L adds the calcium prepared by 0.1g embodiment 1
Titanium ore SrTiO3Porous particle, irradiates under ultraviolet light after dark stirring 40min, takes once every 20min
Sample, gained uv-visible absorption spectra is as shown in Figure 4.
Separately making one group of experiment carrying out ultraviolet degradation methylene blue without any catalyst is matched group,
Gained uv-visible absorption spectra is as shown in Figure 5.By contrast, the perovskite prepared by this method
SrTiO3Porous nano granule has preferable photocatalysis performance.
Claims (8)
1. a perovskite SrTiO3The preparation method of porous nano granule, it is characterised in that include following
Step:
1) with titanium sulfate and potassium hydroxide as raw material, the hydroxide precipitation of titanium is prepared；
2) strontium nitrate solution, potassium hydroxide solution and lithium nitrate solution are prepared respectively；Described strontium nitrate is molten
The molar concentration 0.2～0.6mol/L of liquid, the molar concentration of potassium hydroxide solution is 1～3mol/L, lithium nitrate
Solution molar concentration 0.6～1mol/L；
3) the hydroxide precipitation of titanium, strontium nitrate solution, potassium hydroxide solution and lithium nitrate solution are mixed,
At reaction temperature is 150～220 DEG C, carry out hydro-thermal reaction 3～32h, centrifugal, then clean, obtain calcium
Titanium ore SrTiO3Porous nano granule；The hydroxide precipitation of described titanium, strontium nitrate solution, hydroxide
The mixed proportion of potassium solution and lithium nitrate solution is: 0.6～2g:5～10ml:10～15ml:5～10ml.
Perovskite SrTiO the most according to claim 13The preparation method of porous nano granule, it is special
Levy and be, described step 1) in prepare titanium the method for hydroxide precipitation be: preparation mole is dense respectively
Degree is titanium sulfate solution and the potassium hydroxide solution of 6～10mol/L of 0.15～0.5mol/L；By potassium hydroxide
Solution is added drop-wise in titanium sulfate solution, is filtrated to get the hydroxide precipitation of titanium.
Perovskite SrTiO the most according to claim 23The preparation method of porous nano granule, it is special
Levy and be, described rate of addition 2～4 drops/sec.
Perovskite SrTiO the most according to claim 13The preparation method of porous nano granule, it is special
Levy and be, described step 3) in reaction temperature be 160～180 DEG C, the response time is 3～6h.
Perovskite SrTiO the most according to claim 13The preparation method of porous nano granule, it is special
Levy and be, described step 3) in the hydroxide precipitation of titanium, strontium nitrate solution, potassium hydroxide solution
With the mixed proportion of lithium nitrate solution it is: 0.6～0.8g:5～8ml:10～13ml:5～8ml.
Perovskite SrTiO the most according to claim 13The preparation method of porous nano granule, it is special
Levy and be, described step 3) in cleaning method be: by the product that is filtrated to get successively with spirit of vinegar,
Deionized water cleans.
Perovskite SrTiO the most according to claim 23The preparation method of porous nano granule, it is special
Levy and be, described step 1) in prepare titanium the method for hydroxide precipitation be: preparation mole is dense respectively
Degree is titanium sulfate solution and the potassium hydroxide solution of 5.5～6.5mol/L of 0.13～0.17mol/L；By hydrogen-oxygen
Change potassium solution under stirring 2～3 drops/sec be added drop-wise in titanium sulfate solution, be filtrated to get the hydroxide of titanium
Thing precipitates；
Described step 2) in the molar concentration 0.18～0.22mol/L of strontium nitrate solution, potassium hydroxide solution
Molar concentration be 0.9～1.1mol/L, lithium nitrate solution molar concentration 0.5～0.7mol/L；
Described step 3) in the hydroxide of 0.6～0.7g titanium is precipitated, 5～6ml strontium nitrate aqueous solution,
10～11ml potassium hydroxide solutions and 5～6ml lithium nitrate solutions are mixed to join in reactor,
At 160～170 DEG C, insulation carries out heat treatment in 3～5 hours.
8. the perovskite SrTiO according to the arbitrary described preparation method synthesis of claim 1～73Porous
Nano-particle.
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| CN106673057A (en) * | 2016-11-16 | 2017-05-17 | 浙江大学 | Perovskite Li-doped SrTiO3 nano particles preparation method and product thereof |
| CN106745210A (en) * | 2017-01-06 | 2017-05-31 | 浙江大学 | A kind of Li doping SrTiO3The preparation method and product of porous surface nano particle |
| CN106745211A (en) * | 2017-01-06 | 2017-05-31 | 浙江大学 | A kind of Li doping SrTiO3The preparation method and product of square nano particle |
| CN110952143A (en) * | 2019-12-03 | 2020-04-03 | 华东理工大学 | Synthesis method of mesoporous single-crystal strontium titanate |
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| CN106745211A (en) * | 2017-01-06 | 2017-05-31 | 浙江大学 | A kind of Li doping SrTiO3The preparation method and product of square nano particle |
| CN106745210B (en) * | 2017-01-06 | 2018-06-29 | 浙江大学 | A kind of Li adulterates SrTiO3The preparation method and product of porous surface nano particle |
| CN106745211B (en) * | 2017-01-06 | 2018-06-29 | 浙江大学 | A kind of Li adulterates SrTiO3The preparation method and product of square nano particle |
| CN110952143A (en) * | 2019-12-03 | 2020-04-03 | 华东理工大学 | Synthesis method of mesoporous single-crystal strontium titanate |
| CN110952143B (en) * | 2019-12-03 | 2021-09-03 | 华东理工大学 | Synthesis method of mesoporous single-crystal strontium titanate |
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| CN105883910B (en) | 2017-10-13 |
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