CN108706626A - A kind of SrTiO3The preparation method of nano material - Google Patents
A kind of SrTiO3The preparation method of nano material Download PDFInfo
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- CN108706626A CN108706626A CN201810761296.7A CN201810761296A CN108706626A CN 108706626 A CN108706626 A CN 108706626A CN 201810761296 A CN201810761296 A CN 201810761296A CN 108706626 A CN108706626 A CN 108706626A
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- srtio
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- nano material
- ethylene glycol
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical class [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- 229910002367 SrTiO Inorganic materials 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000000084 colloidal system Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 4
- 238000005187 foaming Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 3
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 claims 1
- 238000001879 gelation Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 4
- 229910052712 strontium Inorganic materials 0.000 abstract description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- 239000013064 chemical raw material Substances 0.000 abstract 1
- 239000012453 solvate Substances 0.000 abstract 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000003980 solgel method Methods 0.000 description 5
- 239000010936 titanium Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- PWYYWQHXAPXYMF-UHFFFAOYSA-N strontium(2+) Chemical compound [Sr+2] PWYYWQHXAPXYMF-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 titanium Alkoxide Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of SrTiO3The preparation method of nano material, belongs to field of functional materials.The present invention is using methanol as solvent, it operates to obtain mixed solution by stirring and dissolving is done in citric acid, six water strontium chlorides, butyl titanate chemical raw material addition methanol solvate, by above-mentioned solution by plastic, drying, calcination processing, the strontium titanate material that can be had excellent performance.The present invention uses methanol as solvent, and the method for the invention technical process is simple, obtained strontium titanates stable quality, and purity is high, uniformity is good, and manufacturing cycle greatly shortens, while improving production efficiency.
Description
Technical field
The present invention relates to a kind of SrTiO3The preparation method of nano material, belongs to field of functional materials.
Background technology
Strontium titanates（SrTiO3）It is a kind of electronics that electronics industry purposes is relatively broad with typical perovskite structure
Ceramic material has many advantages, such as that dielectric constant is high, dielectric loss is low, thermal stability is good, is widely used in high-voltage capacitance
The fields such as device, varistor, thermistor have the characteristics that high-performance, high reliability, small.As functional material,
SrTiO3Have the characteristics that energy gap is high, photocatalytic activity is excellent, and there is unique electromagnetic property and redox catalysis
Activity.Strontium titanates is increasingly becoming a kind of very attractive functional material, has a extensive future.
Currently, strontium titanates（SrTiO3）Preparation method have very much, mainly have high temperature solid phase synthesis, hydro-thermal method, coprecipitated
Shallow lake method and sol-gel method.SrTiO made from high temperature solid phase synthesis3Powder, because its have impurity content is high, particle size is big,
Chemical composition has that fluctuation, size distribution are wide, have more serious agglomeration, sintering temperature relatively high, to strong influence
The performance of product.Hydro-thermal method reaction process is not easily controlled, and reaction is incomplete, also very high to equipment requirement.
Sol-gel method prepares that powder reaction temperature is low, and the product purity of acquisition is high, and particle diameter is small, is evenly distributed, mistake
Journey is easily controllable.But general sol-gel method prepares SrTiO3When powder, frequently with absolute ethyl alcohol, it is also necessary to add other
Reagent, and reaction process is longer, and generated time is also grown.
Invention content
The purpose of the present invention is to provide a kind of SrTiO3The preparation method of nano material, using methanol as solvent, titanium
Alkoxide and six water strontium chlorides are as solute, and for ethylene glycol as dispersant, citric acid can play inhibition titanium as chelating agent
The effect of the hydrolysis of alkoxide；Specifically include following steps：
（1）In methyl alcohol, while ethylene glycol is added as dispersant in citric acid, butyl titanate, the dissolving of six water strontium chlorides, is obtained
The addition of mixed solution, ethylene glycol is 3mL.
（2）By step（1）Gained mixed solution foams plastic at 80 ~ 90 DEG C, nothing during heating reaction to foaming plastic
Precipitation generates, 20 ~ 25 minutes the time required to plastic.
（3）By step（2）Xerogel is obtained after the drying of gained colloid；Gained xerogel obtains after carrying out calcination processing
SrTiO3Material.
Preferably, the present invention is step by step rapid（1）The addition of middle ethylene glycol is often to prepare the SrTiO of 1g31.5ml is added in material
Ethylene glycol.
Preferably, step of the present invention（3）Middle drying condition is 1 ~ 2 hour dry in 180 ~ 190 DEG C, and calcination condition is：800
~ 900 DEG C are calcined 3 ~ 5 hours.
Beneficial effects of the present invention：
（1）The sol-gel method that the present invention uses improves traditional method, prepares in powder process, need not add
Add other reagents, and experimentation is simple, easy to operation, the time used is shorter, to improve conventional efficient.
（2）The present invention is using methanol as solvent, dispersibility stronger spy smaller using methanol surface tension
Point can reduce solution viscosity during plastic, colloid is made fully to react；The SrTiO of acquisition3Particle diameter distribution is relatively narrow, particle
Tiny, purity is high；And the plastic reaction time of the present invention only needs 20 ~ 25 minutes, 1 ~ 2 hour dry, the time used will be much smaller than
SrTiO is prepared using the sol-gel process of absolute ethyl alcohol3。
Description of the drawings
Fig. 1 is 1 gained SrTiO of embodiment3The XRD spectrum of nano material.
Fig. 2 is 1 gained SrTiO of embodiment3The SEM of nano material schemes.
Fig. 3 is 2 gained SrTiO of embodiment3The SEM of nano material schemes.
Fig. 4 is the SrTiO that comparative example obtains3The SEM of nano material schemes.
Fig. 5 is the experimental phenomena that comparative example obtains.
Specific implementation mode
Invention is further described in detail with reference to the accompanying drawings and detailed description, these specific implementation modes are only
It is the purpose illustrated due to exemplary, and is not intended to limit the present invention.
Embodiment 1
A kind of SrTiO3The preparation method of nano material, specifically includes following steps：
（1）Citric acid, butyl titanate, six water strontium chlorides are dissolved in the methanol of 50mL, while ethylene glycol is added as dispersion
Agent obtains mixed solution, and the addition of citric acid is 13.7432g in mixed solution, and the addition of butyl titanate is
The addition of 3.7852g, six water strontium chlorides are 2.9207g, and the addition of ethylene glycol is 3mL.
（2）By step（1）Gained mixed solution foams plastic at 90 DEG C, without precipitation during heating reaction to foaming plastic
It generates, 20 minutes the time required to plastic.
（3）By step（2）Gained colloid is dried（It is 1 hour dry in 180 DEG C）After obtain xerogel；Gained xerogel carries out
Calcination processing（800 DEG C are calcined 5 hours）After obtain SrTiO3Material.
SrTiO manufactured in the present embodiment3The XRD spectrum of superconducting nano material is as shown in Figure 1, it can be seen that obtained sample
Without other dephasigns.
The SrTiO that the present embodiment is prepared3Material particle size narrow distribution, particle are tiny as shown in Figure 2
Embodiment 2
A kind of SrTiO3The preparation method of nano material, specifically includes following steps：
（1）Citric acid, butyl titanate, six water strontium chlorides are dissolved in the methanol of 50mL, while ethylene glycol is added as dispersion
Agent obtains mixed solution, and the addition of citric acid is 13.7432g in mixed solution, and the addition of butyl titanate is
The addition of 3.7852g, six water strontium chlorides are 2.9207g, and the addition of ethylene glycol is 3mL.
（2）By step（1）Gained mixed solution foams plastic at 80 DEG C, without precipitation during heating reaction to foaming plastic
It generates, 25 minutes the time required to plastic.
（3）By step（2）Gained colloid is dried（It is 1 hour dry in 190 DEG C）After obtain xerogel；Gained xerogel carries out
Calcination processing（900 DEG C are calcined 3.5 hours）After obtain SrTiO3Material.
The SrTiO that the present embodiment is prepared3Material particle size narrow distribution, particle is tiny, as shown in Figure 3
Comparative example 1：SrTiO is prepared using traditional sol-gal process3Material
（1）Strontium nitrate is stoichiometrically weighed up, aqueous citric acid solution is added（Sr2+Molar ratio with citric acid is 1:2）80
Stirring and dissolving at~90 DEG C is designated as A liquid with ammonium hydroxide tune pH value to 6~8.
（2）Stoichiometric ratio claims butyl titanate, and slowly pours into (Ti in the citric acid solution for mixing up pH (6~8) value4+With
The molar ratio of citric acid is 1:2), at 80~90 DEG C stirring and dissolving to transparent molten.
（3）After A and B liquid is stirred evenly xerogel is dried to obtain at 180 DEG C respectively；Xerogel is forged at 650 DEG C
It burns 5h and obtains SrTiO3Powder.
Comparative example obtains SrTiO3The SEM of material is as shown in Figure 4；It can be seen that particle is not very uniformly.
Comparative example 2：It is tested as a comparison using citric acid is added without, experimental phenomena is as shown in figure 5, figure (a), (b)
Citric acid respectively is added and is added without the experimental phenomena comparison diagram of citric acid；It can be seen that the case where being added without citric acid
Under, milky is presented in solution, and bottom has the precipitation of white, butyl titanate to produce hydrolysis, can not form solution, and then be unable to shape
At colloidal sol；And in the case where citric acid is added, butyl titanate can form solution in methanol solution, not occur precipitating
Phenomenon, and then colloidal sol can be formed.
Claims (3)
1. a kind of SrTiO3The preparation method of nano material, which is characterized in that specifically include following steps：
（1）Citric acid, butyl titanate, six water strontium chlorides are stoichiometrically dissolved in methyl alcohol, while ethylene glycol work is added
For dispersant, mixed solution is obtained；
（2）By step（1）Gained mixed solution foams plastic at 80 ~ 90 DEG C, without precipitation during heating reaction to foaming plastic
It generates, gelation time is 20 ~ 25 minutes；
（3）By step（2）Xerogel is obtained after the drying of gained colloid, gained xerogel obtains SrTiO after carrying out calcination processing3Material
Material.
2. SrTiO according to claim 13The preparation method of nano material, it is characterised in that：Step（1）Middle ethylene glycol adds
It is often to prepare the SrTiO of 1g to enter amount31.5ml ethylene glycol is added in material.
3. SrTiO according to claim 13The preparation method of nano material, it is characterised in that：Step（3）Middle drying condition is
1 ~ 2 hour dry in 180 ~ 190 DEG C, calcination condition is：800 ~ 900 DEG C are calcined 3 ~ 5 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810761296.7A CN108706626A (en) | 2018-07-12 | 2018-07-12 | A kind of SrTiO3The preparation method of nano material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810761296.7A CN108706626A (en) | 2018-07-12 | 2018-07-12 | A kind of SrTiO3The preparation method of nano material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620340A (en) * | 2021-08-27 | 2021-11-09 | 西安理工大学 | Flower-shaped SrTiO prepared by rotary evaporation method3Method for preparing nano material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239076A (en) * | 1998-06-12 | 1999-12-22 | 中国科学院青海盐湖研究所 | Process for preparing nm-class strontium titanate |
| CN104030680A (en) * | 2014-06-26 | 2014-09-10 | 天津大学 | Preparation method of barium strontium titanate dielectric film |
-
2018
- 2018-07-12 CN CN201810761296.7A patent/CN108706626A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1239076A (en) * | 1998-06-12 | 1999-12-22 | 中国科学院青海盐湖研究所 | Process for preparing nm-class strontium titanate |
| CN104030680A (en) * | 2014-06-26 | 2014-09-10 | 天津大学 | Preparation method of barium strontium titanate dielectric film |
Non-Patent Citations (2)
| Title |
|---|
| 徐明霞等: ""无机盐原料溶胶-凝胶工艺合成高纯超细钛酸锶粉料"", 《硅酸盐学报》 * |
| 贺海燕等: ""表面活性剂辅助Sol—gel法SrTiO3粉体的形状控制合成"", 《江苏陶瓷》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113620340A (en) * | 2021-08-27 | 2021-11-09 | 西安理工大学 | Flower-shaped SrTiO prepared by rotary evaporation method3Method for preparing nano material |
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