CN106745211B - A kind of Li adulterates SrTiO3The preparation method and product of square nano particle - Google Patents
A kind of Li adulterates SrTiO3The preparation method and product of square nano particle Download PDFInfo
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- CN106745211B CN106745211B CN201710009407.4A CN201710009407A CN106745211B CN 106745211 B CN106745211 B CN 106745211B CN 201710009407 A CN201710009407 A CN 201710009407A CN 106745211 B CN106745211 B CN 106745211B
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 124
- 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 64
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 38
- 238000001556 precipitation Methods 0.000 claims abstract description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 30
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims abstract description 30
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 26
- 239000010936 titanium Substances 0.000 claims abstract description 26
- 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 21
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 11
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000052 vinegar Substances 0.000 claims description 3
- 235000021419 vinegar Nutrition 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 4
- 238000005424 photoluminescence Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 229910002367 SrTiO Inorganic materials 0.000 description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 229910052712 strontium Inorganic materials 0.000 description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 5
- 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 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910006715 Li—O Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- LFIWDPYJFLBDMX-UHFFFAOYSA-N lithium;sulfuric acid Chemical compound [Li].OS(O)(=O)=O LFIWDPYJFLBDMX-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/002—Compounds containing, besides titanium, two or more other elements, with the exception of oxygen or hydrogen
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/671—Chalcogenides
- C09K11/673—Chalcogenides with alkaline earth metals
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- 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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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The present invention relates to a kind of Li to adulterate SrTiO3The preparation method of square nano particle, 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, lithium sulfate solution, potassium hydroxide solution are prepared respectively；0.1~0.3mol/L of molar concentration of the strontium nitrate solution, the molar concentration of lithium sulfate solution is 0.3~0.5mol/L, and the molar concentration of potassium hydroxide solution is 0.5~1.5mol/L；3) hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide solution and lithium sulfate solution are stirred to obtain presoma, carry out hydro-thermal reaction, filter, cleaning is dried to obtain Li doping SrTiO3Square nano particle.The preparation method process is simple, and pattern is easy to regulate and control, and product has excellent photoluminescence performance, and is widely used.
Description
Technical field
The present invention relates to inorganic material to synthesize field, and in particular to a kind of Li adulterates SrTiO3The system of square nano particle
Preparation Method and product.
Background technology
Perovskite composite oxide strontium titanates (SrTiO3) it is a kind of excellent electron ceramic material, belong to titanate system
The Major Members of row electronic ceramics powder.SrTiO3Powder body material has excellent physics and chemical property, as dielectric constant is high,
Refractive index is high, dielectric loss is low, energy gap is high, photocatalytic activity is good, high dieletric strength etc..Therefore strontium titanates
(SrTiO3) electronics, photocatalysis and ceramic industry are widely used in, for manufacturing oxygen sensitive element, grain-boundary layer capacitor and photocatalysis electricity
Pole material etc..
There are four types of the main methods for preparing Sr titanate powder at present：High-temperature solid-phase sintering method, hydro-thermal method, chemical coprecipitation
Method, sol-gel method.Wherein, the Sr titanate powder that solid phase method is prepared often there are diameter of particle it is big, reunite it is serious,
The problems such as impurity content is high, reaction temperature is high, the development of modern science and technology, the requirement to the pattern and grain size of Sr titanate powder material
It is higher and higher, the synthesis to strontium titanates is needed to carry out diversified regulation and control, grain size fine uniform, good dispersion are prepared with this
Sr titanate powder material.
Chinese invention patent (105883910 A of CN) discloses a kind of perovskite SrTiO3The preparation side of porous nano particle
Method includes the following steps：1) using titanium sulfate and potassium hydroxide as raw material, the hydroxide precipitation of titanium is prepared；2) nitre is prepared respectively
Sour strontium solution, potassium hydroxide solution and lithium nitrate solution；3) it is the hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide is molten
Liquid and lithium nitrate solution mixing, carry out hydro-thermal reaction, obtain perovskite SrTiO3Porous nano particle.Nitric acid is used in step 2)
Lithium solution, the NO introduced in water-heat process3 -, with the K in potassium hydroxide solution+Obtain KNO3, and KNO3Ionization equilibrium constant
It is larger, therefore enter SrTiO in hydrothermal reaction process3The K of particle+More, the SrTiO that doping lithium nitrate is formed3Duct meeting
Through entire nano particle.
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 SrTiO3Square nano particle
Preparation method and product, preparation process is simple, and pattern is easy to regulate and control, and has excellent photoluminescence performance, and is widely used.
Technical solution provided by the present invention is：
A kind of Li adulterates SrTiO3The preparation method of square nano particle, 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, lithium sulfate solution, potassium hydroxide solution are prepared respectively；The molar concentration of the strontium nitrate solution
0.1~0.3mol/L, the molar concentration of lithium sulfate solution is 0.3~0.5mol/L, and the molar concentration of potassium hydroxide solution is 0.5
~1.5mol/L；
3) hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide solution and lithium sulfate solution are stirred to obtain
Presoma carries out hydro-thermal reaction, filters, cleaning, is dried to obtain Li doping SrTiO3Square nano particle.
In above-mentioned technical proposal, the hydroxide that titanium is prepared by titanium sulfate and potassium hydroxide precipitates, then by raw material nitre
Hydro-thermal reaction is passed through in the hydroxide precipitation mixing of sour strontium, lithium sulfate, potassium hydroxide and titanium, obtains Li doping SrTiO3Square
Nano particle.The selection Li in lithium source selection2SO4Substitute LiNO3It allows for and SO is introduced in water-heat process4 2-, identical item
Under part with KNO3It compares, K2SO4Ionization equilibrium constant smaller, in hydrothermal reaction process enter SrTiO3The K of particle+Less,
Simultaneously with Li2SO4The increase of concentration, Li+The quantity that ion is entered in crystal increases, and Li-O keys have more covalent bonds
Ingredient has good directionality and saturability, can promote SrTiO3The forming core growth of intrinsic cube structure, meanwhile, Li+From
Son, which introduces, can inhibit K+Into crystal, hole is caused to reduce until disappearing, the Li doping SrTiO of gained3Square nano particle
With excellent photoluminescence performance.
Preferably, in the step 3) titanium hydroxide precipitation, strontium nitrate solution, potassium hydroxide solution and lithium sulfate
The mixed proportion of solution is：0.4~1.2g：10~20ml：5~15ml：10~20ml.
Preferably, in the step 3) reaction temperature of hydro-thermal reaction for 150~250 DEG C, the reaction time for 6~for 24 hours.
Preferably, in the step 3) reaction temperature of hydro-thermal reaction for 190~210 DEG C, the reaction time for 20~
24h.By the sufficient hydro-thermal reactions of more than 20h, the Li finally obtained can be allowed to adulterate SrTiO3Square nano particle crystallizes
Property is more preferable.
Preferably, the method that the hydroxide precipitation of titanium is prepared in the step 1) is：Preparing molar concentration respectively is
The titanium sulfate solution of 0.06~0.18mol/L and the potassium hydroxide solution of 5~10mol/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 square nano particle.
Preferably, 2~4 drops/sec of the rate of addition.Potassium hydroxide solution is added drop-wise to titanium sulfate solution by controlling
In rate of addition, further regulate and control Li doping SrTiO3The pattern of square particle.
Preferably, in the step 3) titanium hydroxide precipitation, strontium nitrate solution, potassium hydroxide solution and lithium sulfate
The mixed proportion of solution is：0.6~1g：10~15ml：10~15ml：15-20ml.The Li doping of gained under the mixed proportion
SrTiO3The pattern of square particle is 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, deionized water
Cleaning.
Preferably, the method that the hydroxide precipitation of titanium is prepared in the step 1) is：Preparing molar concentration respectively is
The titanium sulfate solution of 0.11~0.13mol/L and the potassium hydroxide solution of 7~9mol/L；By potassium hydroxide solution with rate of addition
2~4 drops/sec are added drop-wise in titanium sulfate solution, and the hydroxide precipitation of titanium is obtained by filtration；Strontium nitrate solution in the step 2)
Molar concentration is 0.15~0.18mol/L, and the molar concentration of lithium sulfate solution is 0.38~0.42mol/L, potassium hydroxide solution
Molar concentration be 0.9~1.1mol/L；By the hydroxide of the 0.7~0.9g titaniums cleaned precipitation, 14 in the step 3)
~16ml strontium nitrate solutions, 9~11ml potassium hydroxide solutions and 14~16ml lithium sulfate solutions are added in reaction kettle, 190
20~21h is kept the temperature at~200 DEG C.Under these conditions, gained Li adulterates SrTiO3Square nano particle, pattern is good, quality
Stablize, purity is high, powder granule good dispersion.
The present invention also provides a kind of Li of preparation method synthesis as described above to adulterate SrTiO3Square nano particle.
Compared with the existing technology, beneficial effects of the present invention are embodied in：Li provided by the present invention adulterates SrTiO3It is square
The preparation method of body nano particle, preparation process is simple, and pattern is easy to regulate and control, and has excellent photoluminescence performance, and apply
Extensively.
Description of the drawings
Fig. 1 is that the Li that embodiment 1 is prepared adulterates SrTiO3The XRD diagram of square nano particle；
Fig. 2 is that the Li that embodiment 1 is prepared adulterates SrTiO3The SEM figures of square nano particle；
Fig. 3 is the SrTiO that comparative example 1 is prepared3The SEM figures of elliposoidal nano particle；
Fig. 4 is that the Li that comparative example 2 is prepared adulterates SrTiO3The SEM figures of porous surface nano particle；
Fig. 5 is that the Li that comparative example 2 is prepared adulterates SrTiO3The TEM figures of porous surface nano particle；
Fig. 6 is embodiment 1 and the PL spectrograms of 1 products therefrom of comparative example.
Specific embodiment
Below in conjunction with specific embodiment and Figure of description, the invention will be further described.
Embodiment 1
1) 6mmol titanium sulfates and 0.16mol potassium hydroxide are dissolved separately in deionized water, adjust titanium sulfate solution
Molar concentration 0.12mol/L, the molar concentration of potassium hydroxide solution is 8mol/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, potassium hydroxide and lithium sulfate are dissolved separately in deionized water, the molar concentration of strontium nitrate solution
For 0.165mol/L, the molar concentration of potassium hydroxide solution is 1mol/L, a concentration of 0.4mol/L of lithium sulfate solution.
4) by the hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrate solutions, 10ml potassium hydroxide solutions and
15ml lithium sulfate solutions are added in 50ml reaction kettles, and it is the 40% of reaction kettle liner to adjust total volume with deionized water, stirring
After 2h, at 200 DEG C keeping the temperature 20 hours is heat-treated.Then, room temperature is down to, takes out reaction product, filtering, successively with dilute vinegar
Acid, deionized water are cleaned, and are dried at a temperature of 60 DEG C, obtain Li doping SrTiO3Square nano particle.
It is the XRD diagram of 1 products therefrom of embodiment as shown in Figure 1, does not have impurity peaks appearance in XRD diagram, it is pure to show product
The SrTiO of phase3。
Scanning electron microscope SEM photograph is as shown in Fig. 2, the Li doping SrTiO prepared3The size of square nano particle
Between 300nm or so, pattern is square particle.
Embodiment 2
1) 7mmol titanium sulfates and 0.16mol potassium hydroxide are dissolved separately in deionized water, adjust titanium sulfate solution
Molar concentration 0.14mol/L, the molar concentration of potassium hydroxide solution is 8mol/L.
2) 20ml potassium hydroxide solutions are slowly added dropwise in 50ml 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, potassium hydroxide and lithium sulfate are dissolved separately in deionized water, the molar concentration of strontium nitrate solution
For 0.165mol/L, the molar concentration of potassium hydroxide solution is 1mol/L, a concentration of 0.5mol/L of lithium sulfate solution.
4) by the hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrate solutions, 10ml potassium hydroxide solutions and
15ml lithium sulfate solutions are added in 50ml reaction kettles, and it is the 40% of reaction kettle liner to adjust total volume with deionized water, stirring
After 2h, at 200 DEG C keeping the temperature 12 hours is heat-treated.Then, room temperature is down to, takes out reaction product, filtering, successively with dilute vinegar
Acid, deionized water are cleaned, and are dried at a temperature of 60 DEG C, obtain Li doping SrTiO3Square nano particle.
Embodiment 3
1) 7mmol titanium sulfates and 0.16mol potassium hydroxide are dissolved separately in deionized water, adjust titanium sulfate solution
Molar concentration 0.14mol/L, the molar concentration of potassium hydroxide solution is 8mol/L.
2) 20ml potassium hydroxide solutions are slowly added dropwise in 50ml 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, potassium hydroxide and lithium sulfate are dissolved separately in deionized water, the molar concentration of strontium nitrate solution
For 0.165mol/L, the molar concentration of potassium hydroxide solution is 1mol/L, a concentration of 0.4mol/L of lithium sulfate solution.
4) by the hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrate solutions, 10ml potassium hydroxide solutions and
15ml lithium sulfate solutions are added in 50ml reaction kettles, and it is the 40% of reaction kettle liner to adjust total volume with deionized water, stirring
After 2h, at 200 DEG C keeping the temperature 6 hours is heat-treated.Then, room temperature is down to, takes out reaction product, filtering, successively with dilute vinegar
Acid, deionized water are cleaned, and are dried at a temperature of 60 DEG C, obtain Li doping SrTiO3Square nano particle.
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 are dissolved separately in deionized water, the molar concentration of strontium nitrate solution is
0.1mol/L, a concentration of 0.1mol/L of potassium hydroxide solution.
4) hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrate solutions and 10ml potassium hydroxide solutions are distinguished
It is 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
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, obtain SrTiO3Elliposoidal nano particle, scanning electron microscope SEM photograph is as shown in figure 3, nothing
Method obtains square nano particle.
Comparative example 2
1) 6mmol titanium sulfates and 0.16mol potassium hydroxide are dissolved separately in deionized water, adjust titanium sulfate solution
Molar concentration 0.12mol/L, the molar concentration of potassium hydroxide solution is 8mol/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, potassium hydroxide and lithium sulfate are dissolved separately in deionized water, the molar concentration of strontium nitrate solution
For 0.165mol/L, the molar concentration of potassium hydroxide solution is 1mol/L, a concentration of 0.05mol/L of lithium sulfate solution.
4) by the hydroxide of the 0.8g titaniums cleaned precipitation, 15ml strontium nitrate solutions, 10ml potassium hydroxide solutions and
15ml lithium sulfate solutions are added in 50ml reaction kettles, and it is the 40% of reaction kettle liner to adjust total volume with deionized water, stirring
After 2h, at 200 DEG C keeping the temperature 20 hours is heat-treated.Then, room temperature is down to, takes out reaction product, filtering, successively with dilute vinegar
Acid, deionized water are cleaned, and are dried at a temperature of 60 DEG C, obtain Li doping SrTiO3Porous surface nano particle.
Scanning electron microscope SEM photograph is as shown in figure 4, Li obtained adulterates SrTiO3The ruler of porous surface nano particle
It is very little that between 300~350nm, pattern is the porous cube of rounding off, while it can be seen that there are many ducts on surface.
Transmission electron microscope TEM photos are as shown in Figure 5, it was demonstrated that Li obtained adulterates SrTiO3Porous surface nano particle, duct
Particle surface is existed only in, inside occurs without duct.
Performance test
As shown in fig. 6, embodiment 1 and the photoluminescence performance of 1 products therefrom of comparative example are measured by PL spectrums, it is known that embodiment
The product of 1 gained is compared with the product of comparative example 1, and photoluminescence performance improves 3 times, and doped sulfuric acid lithium is obviously improved
The photoluminescence performance of product.
Claims (5)
1. a kind of Li adulterates SrTiO3The preparation method of square nano particle, 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, lithium sulfate solution, potassium hydroxide solution are prepared respectively；The molar concentration 0.1 of the strontium nitrate solution
~0.3mol/L, the molar concentration of lithium sulfate solution are 0.3~0.5mol/L, the molar concentration of potassium hydroxide solution for 0.5~
1.5mol/L；
3) hydroxide of titanium precipitation, strontium nitrate solution, potassium hydroxide solution and lithium sulfate solution are stirred to obtain forerunner
Body carries out hydro-thermal reaction, filters, cleaning, is dried to obtain Li doping SrTiO3Square nano particle；The hydro-thermal reaction it is anti-
Temperature is answered as 190~210 DEG C, the reaction time for 20~for 24 hours；The hydroxide precipitation of the titanium, strontium nitrate solution, potassium hydroxide
The mixed proportion of solution and lithium sulfate solution is：0.6~1g：10~15mL：10~15mL：15-20mL .
2. Li according to claim 1 adulterates SrTiO3The preparation method of square nano particle, which is characterized in that described
Prepared in step 1) titanium hydroxide precipitation method be：The sulfuric acid that molar concentration is 0.06~0.18mol/L is prepared respectively
The potassium hydroxide solution of titanium solution and 5~10mol/L；Potassium hydroxide solution is added drop-wise in titanium sulfate solution, titanium is obtained by filtration
Hydroxide precipitation.
3. Li according to claim 2 adulterates SrTiO3The preparation method of square nano particle, which is characterized in that described
2~4 drops/sec of rate of addition.
4. Li according to claim 1 adulterates SrTiO3The preparation method of square nano particle, which is characterized in that described
Cleaning method is in step 3)：The product being obtained by filtration is cleaned successively with spirit of vinegar, deionized water.
5. Li according to claim 1 adulterates SrTiO3The preparation method of square nano particle, which is characterized in that described
Prepared in step 1) titanium hydroxide precipitation method be：The sulfuric acid that molar concentration is 0.11~0.13mol/L is prepared respectively
The potassium hydroxide solution of titanium solution and 7~9mol/L；Potassium hydroxide solution is added drop-wise to titanium sulfate for 2~4 drops/sec with rate of addition
In solution, the hydroxide precipitation of titanium is obtained by filtration；
The molar concentration of strontium nitrate solution is 0.15~0.18mol/L in the step 2), and the molar concentration of lithium sulfate solution is
0.38~0.42mol/L, the molar concentration of potassium hydroxide solution is 0.9~1.1mol/L；
In the step 3) by the hydroxide of the 0.7~0.9g titaniums cleaned precipitation, 14~16mL strontium nitrate solutions, 9~
11mL potassium hydroxide solutions and 14~16ml lithium sulfate solutions are added in reaction kettle, at 190~200 DEG C keep the temperature 20~
21h。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105727922A (en) * | 2016-03-24 | 2016-07-06 | 浙江大学 | Li-doped SrTiO3 octadecahedron nano-particles and preparation method thereof |
| CN105883910A (en) * | 2016-05-13 | 2016-08-24 | 浙江大学 | Preparation method and product for perovskite SrTiO3 porous nano particles |
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|---|---|---|---|---|
| CN105727922A (en) * | 2016-03-24 | 2016-07-06 | 浙江大学 | Li-doped SrTiO3 octadecahedron nano-particles and preparation method thereof |
| CN105883910A (en) * | 2016-05-13 | 2016-08-24 | 浙江大学 | Preparation method and product for perovskite SrTiO3 porous nano particles |
Non-Patent Citations (1)
| Title |
|---|
| "SrTiO3纳米晶多面体可控生长及其生物学行为研究";董灵庆;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20140815(第8期);B020-25 * |
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