CN105727922B - A kind of Li adulterates SrTiO3The preparation method and product of ten octahedron nanometer particles - Google Patents
A kind of Li adulterates SrTiO3The preparation method and product of ten octahedron nanometer particles Download PDFInfo
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- CN105727922B CN105727922B CN201610178914.6A CN201610178914A CN105727922B CN 105727922 B CN105727922 B CN 105727922B CN 201610178914 A CN201610178914 A CN 201610178914A CN 105727922 B CN105727922 B CN 105727922B
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- 239000002245 particle Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 112
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 33
- 238000001556 precipitation Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000010936 titanium Substances 0.000 claims abstract description 24
- 239000002105 nanoparticle Substances 0.000 claims abstract description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 19
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 18
- 235000002639 sodium chloride Nutrition 0.000 claims abstract description 18
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 18
- 229910012675 LiTiO2 Inorganic materials 0.000 claims abstract description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 17
- 239000011780 sodium chloride Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 9
- 235000013339 cereals Nutrition 0.000 claims description 7
- 239000000052 vinegar Substances 0.000 claims description 7
- 235000021419 vinegar Nutrition 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 229910012672 LiTiO Inorganic materials 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 32
- 239000000047 product Substances 0.000 description 11
- 229910002367 SrTiO Inorganic materials 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000011858 nanopowder Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 4
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical class [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 229910052712 strontium Inorganic materials 0.000 description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000704 bioconcentration Toxicity 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000021332 multicellular organism growth Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/39—
-
- B01J35/50—
Abstract
The present invention relates to a kind of Li to adulterate SrTiO3The preparation method of ten octahedron nanometer particles, includes the following steps：1) using titanium sulfate and potassium hydroxide as raw material, the hydroxide precipitation of titanium is prepared；2) strontium nitrate solution and potassium hydroxide solution are prepared respectively；3) by the hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide solution and rock salt octahedron LiTiO2Nano particle is stirred to obtain presoma, carries out hydro-thermal reaction, filters, cleaning, is dried to obtain Li doping SrTiO3Ten octahedron nanometer particles.Present invention process process is simple, easily controllable, and non-environmental-pollution is at low cost, is easy to large-scale production；And products therefrom pattern is octahedra for ten, size is stablized between 50~250nm, product quality, and purity is high, powder granule good dispersion.
Description
Technical field
The present invention relates to inorganic material to synthesize field, and in particular to a kind of Li adulterates SrTiO3Ten octahedron nanometer particles
Preparation method and product.
Background technology
With the rapid development of social economy, the continuous improvement of people's living standard is increasingly paid attention to environmental problem, ring
The problem of guarantor gradually pays close attention to jointly as the whole society.And organic pollution is because it is with extended residual, bioconcentration, half
Volatility and high toxicity become the global environmental problem being concerned in the world at present.In recent years, with ABO3Perovskite structure
Photocatalysis technology for catalyst has become a kind of ideal environmental pollution treatment technology.Wherein, SrTiO3It is typical ABO3Calcium
Perovskite like structure has many advantages, such as that dielectric constant is high, dielectric loss is low, thermal stability is good, is widely used in electronics, machinery and ceramics
Industry.Meanwhile as a kind of functional material, strontium titanates has higher photocatalytic activity, unique electromagnetic property and oxidation also
Former catalytic activity, in photocatalysis fields such as photocatalytic hydrogen production by water decomposition, photocatalysis degradation organic contaminant and photochemical cells
It is widely used.
At present, SrTiO3Preparation method it is very much, such as sol-gel method, coprecipitation, oxidesintering method, microemulsion
Method, acetate method, hydro-thermal method etc..Research shows that synthesized using hydro-thermal method, it can prepare that grain size is tiny, knot at a lower temperature
Brilliant degree is high, reunites less, the nanometer split of sintering activity height, compound with regular structure, good dispersion.
Chinese invention patent (publication number CN102320651A) discloses a kind of preparation method of strontium titanate nano powder, weighs
Tetra-n-butyl titanate and strontium nitrate are simultaneously added in into reaction vessel, are added sodium hydroxide solution and are stirred with glass bar；It is packed into micro-
Heating rate heats in wave reaction instrument；It waits to be cooled to room temperature and solution is poured out into addition hydrochloric acid, then repeatedly washed with deionized water
Obtained precipitation is placed in baking oven in 70 DEG C of drying, obtains strontium titanate nano powder by filter precipitation.The preparation method is using micro-
Wave method prepares the strontium titanate nano powder of pure phase, and the strontium titanate nano powder grain size being prepared is about 100nm, without specific
Pattern, but pattern has a very big impact the performance of strontium titanates, therefore the strontium titanates nanometer obtained by the preparation method
Powder characteristic is poor.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of Li doping SrTiO3Ten octahedra nanometers
The preparation method and product of grain, preparation process is simple, and pattern is easy to regulate and control.
The present invention solves the technical solution of above-mentioned technical problem：
A kind of Li adulterates SrTiO3The preparation method of ten octahedron nanometer particles, includes the following steps：
1) using titanium sulfate and potassium hydroxide as raw material, the hydroxide precipitation of titanium is prepared；
2) strontium nitrate solution and potassium hydroxide solution are prepared respectively；The molar concentration 0.1 of the strontium nitrate solution~
0.36mol/L, the molar concentration of potassium hydroxide solution is 0.05~1mol/L；
3) by the hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide solution and rock salt octahedron LiTiO2Nanometer
Particle is stirred to obtain presoma, carries out hydro-thermal reaction, filters, cleaning, is dried to obtain Li doping SrTiO3Ten octahedrons are received
Rice grain；Hydroxide precipitation, strontium nitrate solution, potassium hydroxide solution and the rock salt octahedron LiTiO of the titanium2Nanometer
The mixed proportion of particle is：0.8~1.8g：15~20ml：10~15ml：0.5~2.5g.
Rock salt octahedron LiTiO2The preparation method of nano particle is in Chinese invention patent (publication number
CN103708543A disclosed in).
The hydroxide that the present invention promotes titanium using titanium sulfate and strontium nitrate as reaction mass, using precipitating reagent potassium hydroxide is given birth to
Into, while using the growth of mineralizer potassium hydroxide regulation and control crystal, finally realize Li doping SrTiO3Ten octahedra nanometers
The preparation of grain.Potassium hydroxide is highly basic, releases a large amount of OH in higher concentrations-Ion, nucleation point quantity increase, are conducive to
Forming core and obtain the smaller nano particle of size. LiTiO2Middle Li+Ion can be with selective absorption on the surface of growth crystal
On, and promote the dehydration on surface, the composition and structure of liquid on interface layer are destroyed, so as to increase adsorption layer to crystalline substance
Body growth resistance, so as to get nanocrystal product present ten octahedral structures.
Preferably, in the step 3) reaction temperature of hydro-thermal reaction for 150~250 DEG C, the reaction time for 6~
24h。
Further preferably, the reaction temperature is 190~200 DEG C, and the reaction time is 6~8h.In the reaction temperature and
Under reaction time, it is more favorable for Li doping SrTiO3The Morphological control of ten octahedron nanometer particles so that the pattern of product is more
Rule, size are more uniform.
Preferably, the method that the hydroxide precipitation of titanium is prepared in the step 1) is：Molar concentration is prepared respectively
For the titanium sulfate solution of 0.06~0.28mol/L and the potassium hydroxide solution of 4~9mol/L；Potassium hydroxide solution is added drop-wise to sulphur
In sour titanium solution, the hydroxide precipitation of titanium is obtained by filtration；The preparation process precipitated by the hydroxide for controlling titanium so that titanium
Hydroxide precipitation as raw material when be more conducive to Li doping SrTiO3The preparation of ten octahedron nanometer particles.
Further preferably, 2~4 drops/sec of the rate of addition.Potassium hydroxide solution is added drop-wise to titanium sulfate by controlling
Rate of addition in solution further regulates and controls Li doping SrTiO3Ten octahedral patterns.
Preferably, hydroxide precipitation, strontium nitrate solution and the potassium hydroxide solution of titanium in the step 3) and
Rock salt octahedron LiTiO2The mixed proportion of nano particle is：0.8~0.9g：15~16ml：10~11ml：0.5~
0.6g.The Li doping SrTiO of gained under the mixed proportion3Ten octahedral patterns are more regular, and size is more uniform.
Preferably, cleaning method is in the step 3)：By the product being obtained by filtration successively with spirit of vinegar, deionization
Water cleans.It is the SrCO in order to be mixed into carbon dioxide in presoma and be formed to the cleaning of hydrothermal synthesis product with spirit of vinegar3
The Li for being nitrate ion in order to which reaction mass is introduced and mineralizer potassium hydroxide and synthesizing clean in removal with deionized water
Adulterate SrTiO3Nano particle is sufficiently separated, and obtains the Li doping SrTiO of pure phase3Nano particle.
Preferably, the titanium sulfate solution and 4~4.5mol/ that molar concentration is 0.068~0.072mol/L are prepared respectively
The potassium hydroxide solution of L；Potassium hydroxide solution with rate of addition is added drop-wise in titanium sulfate solution for 2~4 drops/sec, is obtained by filtration
The hydroxide precipitation of titanium；Continue to prepare strontium nitrate solution and potassium hydroxide solution respectively, the molar concentration of strontium nitrate for 0.1~
0.12mol/L, the molar concentration of potassium hydroxide solution is 0.08~0.11mol/L.The hydrogen of 0.8~0.9g titaniums that will be cleaned
Oxide precipitation, 15~16ml strontium nitrates aqueous solution and 10~11ml potassium hydroxide solutions and 0.5~0.6g rock salts are octahedra
LiTiO2Nano particle is added separately in reaction kettle, and keeping the temperature 6~8 hours at 190~200 DEG C is heat-treated.Above-mentioned
Under the conditions of, gained Li doping SrTiO3Ten octahedron nanometer particles, pattern is good, stable quality, and purity is high, powder granule dispersibility
It is good.
The present invention also provides a kind of Li of above-mentioned preparation method synthesis to adulterate SrTiO3Ten octahedron nanometer particles.Li mixes
Miscellaneous SrTiO3The size of ten octahedron nanometer particles is between 50~250nm, and product pattern is good, and purity is high, good dispersion, equally
The advantageous effect brought with above-mentioned preparation method.
Compared with the existing technology, beneficial effects of the present invention are embodied in：
(1) present invention process process is simple, easily controllable, and non-environmental-pollution is at low cost, is easy to large-scale production.
(2) Li doping SrTiO produced by the present invention3Ten octahedron nanometer particle sizes are between 50~250nm, product quality
Stablize, purity is high, powder granule good dispersion.
Description of the drawings
Fig. 1 is rock salt octahedron LiTiO2The scanning electron microscope diagram of nano particle；
Fig. 2 is that the Li that embodiment 1 synthesizes adulterates SrTiO3The X-ray diffractogram of ten octahedron nanometer particles；
Fig. 3 is that the Li that embodiment 1 synthesizes adulterates SrTiO3The X-ray diffraction partial enlarged view of ten octahedron nanometer particles；
Fig. 4 is that the Li that embodiment 1 synthesizes adulterates SrTiO3The scanning electron microscope diagram of ten octahedron nanometer particles；
Fig. 5 adulterates SrTiO for Li3The octahedra atomic diagram of the ten of ten octahedron nanometer particles；
Fig. 6 is the SrTiO that comparative example 1 synthesizes3The scanning electron microscope diagram of nano particle；
Fig. 7 is that the Li that embodiment 1 synthesizes adulterates SrTiO3The ultraviolet degradation methylene blueprint of ten octahedron nanometer particles；
Fig. 8 is blank group ultraviolet degradation methylene blueprint.
Specific embodiment
It further illustrates the present invention with reference to embodiments.
Rock salt octahedron LiTiO2The preparation of nano particle：
1) by 0.8mmolK2Ti6O13Nanofiber is dissolved in deionized water, adjusts Ti4+A concentration of 0.16mol/L；
2) under stirring, KOH is added in into suspension made from step 1), a concentration of 8mol/L of KOH is adjusted, obtains
Suspension；
3) under stirring, add in lithium nitrate into the suspension prepared by step 2), it is to be mixed uniformly after continuously add
Plumbi nitras adjusts Li+A concentration of 5.34mol/L, Pb2+A concentration of 0.16mol/L, continue to stir 6h, obtain for hydro-thermal
The suspension of reaction；
4) the obtained suspension of step 3) is transferred in hydrothermal reaction kettle liner, makes its volume with deionized water adjusting
The 4/5 of reactor volume is accounted for, stirs 2h, wherein Ti4+Molar concentration be 0.12mol/L, Pb2+Molar ratio is 0.12mol/L,
Li+Molar concentration for 4mol/L, KOH molar concentrations are 6mol/L, and the volume radix of molar concentration is the total of precursor slurry
Volume；
5) the reaction kettle liner equipped with precursor pulp is placed in reaction kettle, sealed, be placed in 240 DEG C of heat preservations, 24 hours water
Heat treatment, then, cools down in air, is down to room temperature, takes out reaction product, and filtering is clear with deionized water, absolute ethyl alcohol successively
It washes, in 80 DEG C of drying, obtains rock salt octahedron LiTiO2Nano particle, scanning electron microscope (SEM) photograph is as shown in Figure 1, nano particle ruler
It is very little between 50~250nm.
Embodiment 1
1) 4mmol titanium sulfates and 2mmol potassium hydroxide are dissolved separately in deionized water, adjust rubbing for titanium sulfate solution
You are concentration 0.07mol/L, and the molar concentration of potassium hydroxide solution is 4mol/L.
2) 20ml potassium hydroxide solutions are slowly added dropwise in 50ml titanium sulfate solutions under stirring, rate of addition is
2 drops/sec, the hydroxide precipitation of white titanium is obtained, stands 20min, filtered and clean precipitation 3 times with deionized water.
3) strontium nitrate and potassium hydroxide being dissolved separately in deionized water, the molar concentration of strontium nitrate is 0.1mol/L,
The molar concentration of potassium hydroxide solution is 0.1mol/L.
4) by the hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrates aqueous solution, 10ml potassium hydroxide solutions and
Rock salt octahedron LiTiO2Nano particle is added separately in 50ml reaction kettles (rock salt octahedron LiTiO2Nano particle
Additive amount is respectively：0.5g, 0.8g, 1.0g, 1.5g, 2.0g, 2.5g), it is reaction kettle liner to adjust total volume with deionized water
40%, after stirring 2h, at 200 DEG C keeping the temperature 6 hours is heat-treated.Then, room temperature is down to, takes out reaction product, is filtered,
It is cleaned with spirit of vinegar, deionized water, is dried at a temperature of 60 DEG C successively, obtain Li doping SrTiO3Ten octahedron nanometer particles.
Synthesized 6 groups of Li doping SrTiO3X-ray diffractogram and partial enlarged view such as Fig. 2 of ten octahedron nanometer particles
It shown in~3, is compared with PDF cards, it is known that product is the SrTiO of perovskite3, with rock salt octahedron LiTiO2Nano particle
Additive amount increase, diffraction maximum first deviates to the left again to the right offset as shown in figure 3, explanation work as LiTiO2The addition of nano particle
(it is less than 1.5g) when measuring relatively low, Li is gap doping so that lattice dimensions increase, and diffraction maximum moves to left；When additive amount continues to increase,
Li is transformed into displacement doping, replaces Sr atoms, since Li atomic sizes are less than Sr atoms, lattice dimensions is caused to reduce, diffraction maximum
It moves to right.
Rock salt octahedron LiTiO2The additive amount of nano particle be 0.5g when, the scanning electron microscope of products therefrom
SEM photograph as shown in figure 4, and atomic diagram as shown in figure 5, Li obtained adulterate SrTiO3Ten octahedron nanometer particles
Size is between 50~250nm.
Embodiment 2
1) 6mmol titanium sulfates and 3mmol potassium hydroxide are dissolved separately in deionized water, adjust rubbing for titanium sulfate solution
You are concentration 0.15mol/L, and the molar concentration of potassium hydroxide solution is 7mol/L.
2) 20ml potassium hydroxide solutions are slowly added dropwise in 40ml titanium sulfate solutions under stirring, rate of addition is
4 drops/sec, the hydroxide precipitation of white titanium is obtained, stands 20min, filtered and clean precipitation 3 times with deionized water.
3) strontium nitrate and potassium hydroxide are dissolved separately in deionized water, the molar concentration of strontium nitrate is 0.15mol/
L, the molar concentration of potassium hydroxide solution is 0.5mol/L.
4) by the hydroxide of the 1.2g titaniums cleaned precipitation, 18ml strontium nitrates aqueous solution, 12ml potassium hydroxide solutions and
1g rock salt octahedrons LiTiO2Nano particle is added separately in 50ml reaction kettles, and it is reaction to adjust total volume with deionized water
The 40% of kettle liner, after stirring 2h, at 150 DEG C keeping the temperature 12 hours is heat-treated.Then, room temperature is down to, takes out reaction production
Object, filtering, is cleaned with spirit of vinegar, deionized water, is dried at a temperature of 60 DEG C successively, obtains Li doping SrTiO3Ten octahedra nanometers
Particle.
Embodiment 3
1) 8mmol titanium sulfates and 4mmol potassium hydroxide are dissolved separately in deionized water, adjust rubbing for titanium sulfate solution
You are concentration 0.28mol/L, and the molar concentration of potassium hydroxide solution is 1mol/L.
2) 20ml potassium hydroxide solutions are slowly added dropwise in 50ml titanium sulfate solutions under stirring, rate of addition is
3 drops/sec, the hydroxide precipitation of white titanium is obtained, stands 20min, filtered and clean precipitation 3 times with deionized water.
3) strontium nitrate and potassium hydroxide are dissolved separately in deionized water, the molar concentration of strontium nitrate is 0.36mol/
L, the molar concentration of potassium hydroxide solution is 1mol/L.
4) by the hydroxide of the 1.8g titaniums cleaned precipitation, 20ml strontium nitrates aqueous solution, 15ml potassium hydroxide solutions and
2.5g rock salt octahedrons LiTiO2Nano particle is added separately in 50ml reaction kettles, and it is anti-to adjust total volume with deionized water
Answer the 40% of kettle liner, after stirring 2h, at 240 DEG C keeping the temperature 24 hours is heat-treated.Then, room temperature is down to, takes out reaction
Product, filtering, is cleaned with spirit of vinegar, deionized water, is dried at a temperature of 60 DEG C successively, obtains Li doping SrTiO3Ten octahedrons are received
Rice grain.
Comparative example 1：
1) 4mmol titanium sulfates and 2mmol potassium hydroxide are dissolved separately in deionized water, adjust rubbing for titanium sulfate solution
You are concentration 0.07mol/L, and the molar concentration of potassium hydroxide solution is 0.1mol/L.
2) 20ml potassium hydroxide solutions are slowly added dropwise in 50ml titanium sulfate solutions under stirring, rate of addition is
2 drops/sec, the hydroxide precipitation of white titanium is obtained, stands 20min, filtered and clean precipitation 3 times with deionized water.
3) strontium nitrate and potassium hydroxide being dissolved separately in deionized water, the molar concentration of strontium nitrate is 0.1mol/L,
A concentration of 0.1mol/L of potassium hydroxide.
4) by the hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrates aqueous solution and 10ml potassium hydroxide solutions point
It is not added in 50ml reaction kettles, it is the 40% of reaction kettle liner to adjust total volume with deionized water, after stirring 2h, at 200 DEG C
Lower heat preservation is heat-treated for 6 hours.Then, room temperature is down to, takes out reaction product, filtering is clear with spirit of vinegar, deionized water successively
It washes, is dried at a temperature of 60 DEG C, obtained SrTiO3For the particle of elliposoidal, scanning electron microscope SEM photograph as shown in fig. 6,
It can not obtain ten octahedron nanometer particles.
Performance test：
10-5The Li doping SrTiO prepared by 0.1g embodiments 1 is added in the methylene blue solution of the 100mL of mol/L3
Ten octahedron nanometer particles after secretly stirring 40min irradiate, a sample, gained ultraviolet-visible are taken every 20min under ultraviolet light
Absorption spectrum is as shown in Figure 7.It is control separately to make one group of experiment for not adding any catalyst progress ultraviolet degradation methylene blue
Group, gained uv-visible absorption spectra are as shown in Figure 8.By comparison it is found that the perovskite SrTiO prepared by this method3Four directions
Nano particle has relatively good photocatalysis performance.
Claims (6)
1. a kind of Li adulterates SrTiO3The preparation method of ten octahedron nanometer particles, which is characterized in that include the following steps：
1) using titanium sulfate and potassium hydroxide as raw material, the hydroxide precipitation of titanium is prepared；
2) strontium nitrate solution and potassium hydroxide solution are prepared respectively；The molar concentration 0.1 of the strontium nitrate solution~
0.36mol/L, the molar concentration of potassium hydroxide solution is 0.05~1mol/L；
3) by the hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide solution and rock salt octahedron LiTiO2Nano particle stirs
It mixes and is mixed to get presoma, carry out hydro-thermal reaction, filter, cleaning is dried to obtain Li doping SrTiO3Ten octahedron nanometer particles；
Hydroxide precipitation, strontium nitrate solution, potassium hydroxide solution and the rock salt octahedron LiTiO of the titanium2Nano particle
Mixed proportion is：0.8~1.8g：15~20ml：10~15ml：0.5~2.5g；
The reaction temperature of the hydro-thermal reaction is 150~250 DEG C, the reaction time for 6~for 24 hours.
2. Li according to claim 1 adulterates SrTiO3The preparation method of ten octahedron nanometer particles, which is characterized in that institute
Prepared in the step 1) stated titanium hydroxide precipitation method be：It is 0.06~0.28mol/L's to prepare molar concentration respectively
The potassium hydroxide solution of titanium sulfate solution and 4~9mol/L；Potassium hydroxide solution is added drop-wise in titanium sulfate solution, is obtained by filtration
The hydroxide precipitation of titanium.
3. Li according to claim 2 adulterates SrTiO3The preparation method of ten octahedron nanometer particles, which is characterized in that institute
2~4 drops/sec of the rate of addition stated.
4. Li according to claim 1 adulterates SrTiO3The preparation method of ten octahedron nanometer particles, which is characterized in that institute
The reaction temperature stated is 190~200 DEG C, and the reaction time is 6~8h.
5. Li according to claim 1 adulterates SrTiO3The preparation method of ten octahedron nanometer particles, which is characterized in that institute
Hydroxide precipitation, strontium nitrate solution, potassium hydroxide solution and the rock salt octahedron LiTiO of titanium in the step 3) stated2It receives
The mixed proportion of rice grain is：0.8~0.9g：15~16ml：10~11ml：0.5~0.6g.
6. Li according to claim 1 adulterates SrTiO3The preparation method of ten octahedron nanometer particles, which is characterized in that institute
Cleaning method is in the step 3) stated：The product being obtained by filtration is cleaned successively with spirit of vinegar, deionized water.
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