CN104477978A - Method for preparing perovskite nano powder - Google Patents
Method for preparing perovskite nano powder Download PDFInfo
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- CN104477978A CN104477978A CN201410781454.7A CN201410781454A CN104477978A CN 104477978 A CN104477978 A CN 104477978A CN 201410781454 A CN201410781454 A CN 201410781454A CN 104477978 A CN104477978 A CN 104477978A
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Abstract
The invention provides a method for preparing ABO3 perovskite nano powder. The method comprises the following steps: dropwisely adding a B-site element source alcohol solution into surfactant/acetic acid-dissolved deionized water to obtain a mixed solution, adding ammonia water into the mixed solution, and reacting the reaction system at constant temperature to obtain a B-site element hydrous oxide gel; and preparing a B-site element hydrous oxide gel dispersion solution, adding an A-site element source into the dispersion solution, and carrying out hydrothermal reaction under normal pressure to obtain the ABO3 perovskite nano powder. The aqueous gel-normal pressure hydrothermal process and raw materials with lower cost are adopted, and the aqueous reaction is utilized to avoid the toxicity of the organic solvent. The pH value, surfactant amount, reaction raw material concentration, reaction time, reaction temperature and other conditions of the system are regulated to effectively control the size of the product, thereby obtaining the well-crystallized monodisperse perovskite powder with the particle size of 15-300nm.
Description
Technical field
The invention belongs to perovskite material preparation field, be specifically related to a kind of method preparing uhligite nano-powder.
Background technology
Common ABO
3the stupalith of type perovskite structure comprises BaTiO
3, CaTiO
3, PbTiO
3, Ba
xsr
1-xtiO
3, BaZr
xti
1-xo
3, Ba
xca
1-xti
yzr
1-yo
3deng.Because perovskite ceramics material has excellent dielectric, ferroelectric, piezoelectricity, and the characteristic such as photochemical catalysis, thus there is widely important application in the industry.Such as BaTiO
3in thermistor, laminated ceramic capacitor, electro-optical device etc., there is critical role; BaZr
xti
1-xo
3and Ba
xca
1-xti
yzr
1-yo
3at Y5V type dielectric material, behave and pay close attention in the fields such as leadless piezoelectric.Various perovskite ceramics is at film, and sensor, the aspects such as stored energy are all furtherd investigate.
The preparation method of ceramics powder body of perovskite mainly contains solid phase method, hydrothermal method, sol-gel method, coprecipitation method etc.The general process of solid phase method is first by titanium dioxide, the oxide compound of the B bit elements such as zirconium dioxide and barium carbonate, and the carbonate of the A bit elements such as calcium carbonate is by ball milling, and the means such as sand milling mix, and then carry out high-temperature calcination, obtain corresponding perovskite powder.Solid phase method process is simple, with low cost, is applicable to large-scale commercial production, but often particle diameter is comparatively large for the perovskite powder obtained, and size distribution is not concentrated, and easily has dephasign.Raw material is normally placed in airtight water heating kettle by hydrothermal method, reacts at higher temperature and very high pressure, the required nano-powder of synthesis.It is less that powder prepared by hydrothermal method has reunion, and the features such as particle is tiny, and dimensional homogeneity is good, raw materials cost is also relatively low.The powder of usual water heat transfer becomes phase without the need to high-temperature calcination, thus avoids grain growth, has higher sintering activity.But due to needs High Temperature High Pressure in Hydrothermal Synthesis process, there is certain danger; And the powder of Hydrothermal Synthesis to compare solid phase method defect more.Coprecipitation method adds suitable precipitation agent in the metal salt solution containing all neccessary compositions, obtains the ceramic forerunner throw out containing required element under proper condition, then by this presoma of calcining, obtain ceramic powder.But the presoma of coprecipitation method often jelly, easily reunite by calcined particle, and size distribution is wide, is also more difficult to get very tiny ceramic particle.Sol-gel method is generally prepare colloidal sol by metal alkoxide or inorganic salt hydrolysis, subsequently by collosol and gel, then gel roasting is obtained nano-powder.The diameter of particle that sol-gel method obtains is little, purity is high, centralized particle diameter, very common in the lab and important.But the raw material of sol-gel method is often expensive, organic solvent required in building-up process has toxicity, and be sintered into and easily make agglomerate grain mutually, and reaction time is long, output is less, is difficult to industrialization.
The production method of current main flow or solid phase method and hydrothermal method, especially based on solid phase method.But along with device miniaturization, the demand of with low costization, the powder that solid phase method is produced highlights gradually with inferior position on sample sintering temperature on particle diameter, and the powder impurity phase that solid phase method is produced is to more, and purity is on the low side, also has disadvantageous effect to performance.Hydrothermal method security is relatively poor, and the more difficult control of the stoichiometry of each composition when composition is more.Therefore invent that a kind of cost is lower, technique is relatively simple, security is high, and be convenient to the method synthesis small size of controlled doping composition and stoichiometric ratio, the perovskite powder of centralized particle diameter is necessary.
Summary of the invention
The present invention mainly solves and uses conventional precipitator method product to reunite seriously, and grain size distribution is disperseed, and need to be sintered into phase, and composite perofskite powder stoichiometric ratio is difficult to the problems such as control.
In order to solve the problems of the technologies described above, the invention provides a kind of ABO adopting aqueous gel-constant pressure hydro-thermal legal system detailed information crystalline substance, single dispersing, composition controlled
3the method of type uhligite nano-powder.
Preparation ABO provided by the present invention
3the method of type uhligite nano-powder, comprises the steps:
(1) alcoholic solution of B position element source is added drop-wise in the deionized water being dissolved with tensio-active agent and acetic acid obtains mixing solutions, ammoniacal liquor is added in described mixing solutions, the system obtained is designated as reaction system 1, described reaction system 1 is reacted under constant temperature, obtains B bit element hydrous oxide gel;
(2) by described B bit element hydrous oxide gel dispersion in water, obtain B bit element hydrous oxide dispersion liquid, in described dispersion liquid, add A position element source, the system obtained is designated as reaction system 2, make described reaction system 2 carry out constant pressure hydro-thermal reaction, obtain ABO
3type uhligite nano-powder.
In aforesaid method step (1), described B position element source is the mixture in titanium source, zirconium source or titanium source and zirconium source.
Described titanium source specifically can be titanium tetrachloride or tetrabutyl titanate.
Described zirconium source specifically can be zirconyl chloride or zirconium-n-butylate.
Described alcohol is selected from following at least one: ethanol, n-butyl alcohol etc.
In the alcoholic solution of described B position element source, the volumetric molar concentration of B position element source is 0.1-5mol/L, specifically can be 2.5mol/L or 3.0mol/L.
Described tensio-active agent is selected from following at least one: polyoxyethylene glycol, polyvinylpyrrolidone, glycol ether, polyacrylic-maleic acid anhydride etc.
Described tensio-active agent specifically can be Macrogol 2000-20000, as PEG2000 or PEG4000.
Describedly be dissolved with in the deionized water of tensio-active agent and acetic acid, the volumetric molar concentration of described tensio-active agent is 10
-5-0.05mol/L, specifically can be 0.000625mol/L or 0.0015mol/L.
Describedly be dissolved with in the deionized water of tensio-active agent and acetic acid, the volumetric molar concentration of described acetic acid is 0.2-3mol/L, specifically can be 0.87mol/L or 1.05mol/L.
In aforesaid method step (1), alcoholic solution and the described volume ratio being dissolved with the deionized water of tensio-active agent and acetic acid of described B position element source are 0.2-0.8: specifically can be 0.45 or 0.40.
In aforesaid method step (1), the amount of the ammoniacal liquor added is regulate the pH value of described mixing solutions to be advisable to 6.5-8.0.
In aforesaid method step (1), the temperature of described reaction is 60 DEG C-90 DEG C, specifically can be 60 DEG C or 70 DEG C.
In aforesaid method step (1), the time of described reaction is 1 hour-5.5 hours, specifically can be 1 hour or 2 hours.
In aforesaid method step (2), in described B bit element hydrous oxide dispersion liquid, the volumetric molar concentration of described B bit element hydrous oxide is 0.1mol/L-1mol/L.
Described A position element source is selected from following at least one: Ba (OH)
2, Sr (OH)
2with Ca (OH)
2, specifically can be Ba (OH)
2or Ba (OH)
2with Sr (OH)
2mixture.
The mol ratio of described A position element source and B position element source is 3.0-1.0.
When described A position element source is in above-mentioned three kinds of oxyhydroxide two or three, the amount of substance sum of described two or three oxyhydroxide and the amount of substance of described B position element source are than being 3.0-1.0.
Described constant pressure hydro-thermal reaction is carried out at 1 atmosphere pressure.
The temperature of described constant pressure hydro-thermal reaction is 60 DEG C-140 DEG C, specifically can be 90 DEG C or 120 DEG C.
The time of described constant pressure hydro-thermal reaction is 1 hour-10 hours, specifically can be 4 hours or 8 hours.
The ABO obtained
3type uhligite nano-powder well-crystallized, single dispersing particle diameter is 15-300nm, specifically can be 47.7nm or 213.0nm.
In order to promote that described reaction is carried out completely, also can add proper ammonia in described reaction system 2, also can add in described reaction system 2 can not participate in react cationic solubility highly basic as sodium hydroxide, potassium hydroxide etc.
In described reaction system 2, the volumetric molar concentration of ammoniacal liquor is 0.5-2mol/L.
In described reaction system 2, the volumetric molar concentration of described solubility highly basic is 0.1-2mol/L.
Aforesaid method, after step (2), also can comprise described ABO
3type uhligite nano-powder carries out the step of washing and drying.Concrete operations are as follows: by described ABO
3type uhligite nano-powder first with dilute acetic acid washing, then with weak ammonia washing, after using deionized water wash 2-3 time subsequently, is dried at being finally placed in 80-150 DEG C in an oven.
By the ABO that aforesaid method prepares
3type uhligite nano-powder also belongs to protection scope of the present invention.
The present invention adopts the method for aqueous gel-constant pressure hydro-thermal, and solve and use conventional precipitator method product to reunite seriously, grain size distribution is disperseed, and need to be sintered into phase, and composite perofskite powder stoichiometric ratio is difficult to the problems such as control; Adopt the raw material of relative inexpensiveness simultaneously, utilize water-based reactions to avoid the toxicity of organic solvent.Further, by conditions such as the pH value of regulation system, surfactivity agent dose, reaction raw materials concentration, reaction times and temperature of reaction, effectively can control the size of product, obtain well-crystallized, single dispersing particle diameter is the perovskite powder of 15-300nm.
Method of the present invention key is the hydrolysis rate by controls B position element source, obtains ultra-fine, good dispersity and highly active B bit element hydrous oxide presoma, while Raw price of the present invention comparatively cheap, whole preparation process cost is lower.Simultaneous reactions process CIMS is simple, and experiment condition is gentle, can complete reaction within a short period of time, be easy to industry and change into product under atmospheric low-temperature.Do not have to introduce the foreign ion being difficult to remove in reaction process, the materials such as acetic acid, tensio-active agent (as polyoxyethylene glycol) and ammoniacal liquor can be removed completely through washing and low temperature presintering.In addition, by one or several in the conditions such as the control concentration of reaction raw materials, the polymerization degree of surfactant polyethylene and content, the acetate concentration added, reaction times and temperature of reaction in reaction, can effectively control grain morphology and size, regulate and control method simple, intuitive.At the end of reaction uhligite good mutually, without the need to high-temperature calcination, powder crystallization is complete, and granularity is little, uniform particle diameter, and distribution is concentrated, good dispersity, and powder sintering activity is higher, can obtain fine and close BST ceramic at about 1250 DEG C sintering.
Accompanying drawing explanation
Fig. 1 is hydration TiO obtained in embodiment 1
2transmission electron microscope (TEM) photo of Gel Precursor.
Fig. 2 is the Ba that embodiment 1 obtains
0.6sr
0.4tiO
3scanning electronic microscope (SEM) photo of nano-powder.
Fig. 3 is the Ba that embodiment 1 obtains
0.6sr
0.4tiO
3x-ray diffraction (XRD) collection of illustrative plates of nano-powder.
Fig. 4 is the TEM photo of the hydrous oxide Gel Precursor of titanium obtained in embodiment 2 and zirconium.
Fig. 5 is the BaZr that embodiment 2 obtains
xti
1-xo
3the SEM photo of powder.
Fig. 6 is the BaZr that embodiment 2 obtains
xti
1-xo
3the XRD figure spectrum of powder.
Embodiment
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.
The experimental technique used in following embodiment if no special instructions, is ordinary method; Reagent used in following embodiment, material etc., all can obtain from commercial channels.
Embodiment 1, be B position element source with tetrabutyl titanate, Ba (OH)
28H
2o and Sr (OH)
28H
2o is A position element source, preparation Ba
0.6sr
0.4tiO
3nanocrystalline powder
Measure 10ml dehydrated alcohol with transfer pipet and be placed in beaker, take 8.5088g tetrabutyl titanate (Ti (OC
4h
9)
4) add in beaker and be stirred to formation clear yellow solution, be denoted as solution A, and moved into separating funnel; Getting 40ml deionized water joins in triangular flask, adds 0.1gPEG (molecular weight 4000) and 2ml acetic acid, stirs, be denoted as solution B; In vigorous stirring situation, solution A is slowly added drop-wise in solution B, dropwises rear maintenance and stir, add 4ml ammoniacal liquor and continue to stir.Gel is obtained after being placed on 60 DEG C of water bath heat preservation 1h, and the centrifugal hydration TiO obtained needed for constant pressure hydro-thermal reaction
2gel.
With 50mL deionized water dispersion hydration TiO
2gel, after disperseing completely, at above-mentioned TiO
26.1420g solid Ba (OH) is added in gel dispersion liquid
28H
2o and 3.4495g solid Sr (OH)
28H
2o, is heated to 60 DEG C and is stirred to oxyhydroxide dissolve completely, be transferred in the round-bottomed flask with condensation reflux unit and react, setting oil bath temperature 120 DEG C, reaction 4h.Reaction terminates the rear centrifugal insolubles obtaining generating in reaction, dries 24h, obtain Ba after being washed by this product at 80 DEG C
0.6sr
0.4tiO
3nano-powder.
Obtained hydration TiO
2the TEM image of presoma is shown in Fig. 1.
As shown in Figure 1: the granular precursor of synthesis is very tiny.
The Ba of synthesis
0.6sr
0.4tiO
3the SEM image of nanocrystalline powder is shown in Fig. 2.
As shown in Figure 2: product is the spherical particle of size uniformity, and median size is 47.7nm, and does not obviously reunite, favorable dispersity.
Fig. 3 is the Ba of synthesis
0.6sr
0.4tiO
3the XRD figure spectrum of nano-powder, as can be seen from collection of illustrative plates, powder well-crystallized, in counterfeit Emission in Cubic.
Embodiment 2, with tetrabutyl titanate and zirconium-n-butylate (commercial obtain the n-butyl alcohol solution that zirconium-n-butylate massfraction is the zirconium-n-butylate of 80%) for B position element source, Ba (OH)
28H
2o is that A position element source prepares BaZr
xti
1-xo
3nanocrystalline powder
Measure 12ml dehydrated alcohol with transfer pipet and be placed in beaker, take 7.2325g tetrabutyl titanate (Ti (OC
4h
9)
4) and the n-butyl alcohol solution of 3.2499g zirconium-n-butylate add in beaker, be stirred to formation clear yellow solution, be denoted as solution A, and moved into separating funnel; Getting 50ml deionized water joins in triangular flask, adds 0.15gPEG (molecular weight 2000) and 3ml acetic acid, stirs, be denoted as solution B; Under the condition of vigorous stirring solution B, solution A is slowly added drop-wise in solution B, dropwises rear maintenance and stir, slowly drip 5ml ammoniacal liquor with separating funnel simultaneously.Gel is obtained after being placed on 70 DEG C of water bath heat preservation 2h, and the centrifugal hydrous oxide gel obtained needed for constant pressure hydro-thermal reaction.In with three mouthfuls of round-bottomed flasks of condensation reflux unit, disperse hydration oxide gel with 40mL deionized water, after disperseing completely, in above-mentioned hydrous oxide gel dispersion liquid, add 11.0411g solid Ba (OH)
28H
2o, heating in water bath to 60 DEG C is also stirred to oxyhydroxide and dissolves completely, then bath temperature is set as 90 DEG C, reaction times 8h.Reaction terminates the rear centrifugal insolubles obtaining generating in reaction, dries 16h, namely obtain BaZr after being washed by this product at 105 DEG C
xti
1-xo
3nanocrystalline powder.
The TEM image of the hydrous oxide Gel Precursor prepared is shown in Fig. 4.
The BaZr of synthesis
xti
1-xo
3the SEM image of powder is shown in Fig. 5.
As shown in Figure 5: product is spherical particle, and median size is 213.0nm, does not obviously reunite, favorable dispersity.
Fig. 6 is the BaZr of synthesis
xti
1-xo
3the XRD figure spectrum of powder, can see, powder well-crystallized, in counterfeit Emission in Cubic from collection of illustrative plates.
Claims (10)
1. prepare a method for uhligite nano-powder, comprise the steps:
(1) alcoholic solution of B position element source is added drop-wise in the deionized water being dissolved with tensio-active agent and acetic acid obtains mixing solutions, ammoniacal liquor is added in described mixing solutions, the system obtained is designated as reaction system 1, described reaction system 1 is reacted under constant temperature, obtains B bit element hydrous oxide gel;
(2) by described B bit element hydrous oxide gel dispersion in water, obtain B bit element hydrous oxide dispersion liquid, in described dispersion liquid, add A position element source, the system obtained is designated as reaction system 2, make described reaction system 2 carry out constant pressure hydro-thermal reaction, obtain ABO
3type uhligite nano-powder.
2. method according to claim 1, is characterized in that: in step (1), and described B position element source is the mixture in titanium source, zirconium source or titanium source and zirconium source;
Described titanium source is titanium tetrachloride or tetrabutyl titanate;
Described zirconium source is zirconyl chloride or zirconium-n-butylate;
Described alcohol is selected from following at least one: ethanol and n-butyl alcohol;
In the alcoholic solution of described B position element source, the volumetric molar concentration of B position element source is 0.1mol/L-5mol/L.
3. method according to claim 1 and 2, is characterized in that: in step (1), described tensio-active agent is selected from following at least one: polyoxyethylene glycol, polyvinylpyrrolidone, glycol ether and polyacrylic-maleic acid anhydride;
Described tensio-active agent is specially Macrogol 2000-20000;
Describedly be dissolved with in the deionized water of tensio-active agent and acetic acid, the volumetric molar concentration of described tensio-active agent is 10
-5mol/L-0.5mol/L;
Describedly be dissolved with in the deionized water of tensio-active agent and acetic acid, the volumetric molar concentration of described acetic acid is 0.2mol/L-3mol/L.
4. the method according to any one of claim 1-3, is characterized in that: in step (1), and alcoholic solution and the described volume ratio being dissolved with the deionized water of tensio-active agent and acetic acid of described B position element source are 0.2-0.8.
5. the method according to any one of claim 1-4, is characterized in that: in step (1), and the temperature of described reaction is 60 DEG C-90 DEG C;
The time of described reaction is 1 hour-5.5 hours.
6. the method according to any one of claim 1-5, is characterized in that: in step (2), and in described B bit element hydrous oxide dispersion liquid, the volumetric molar concentration of described B bit element hydrous oxide is 0.1mol/L-1mol/L.
7. the method according to any one of claim 1-6, is characterized in that: described A position element source is selected from following at least one: Ba (OH)
2, Sr (OH)
2with Ca (OH)
2;
The mol ratio of described A position element source and B position element source is 3.0-1.0.
8. the method according to any one of claim 1-7, is characterized in that: the temperature of described constant pressure hydro-thermal reaction is 60 DEG C-140 DEG C; The time of described constant pressure hydro-thermal reaction is 1 hour-10 hours.
9. the method according to any one of claim 1-8, is characterized in that: obtained ABO
3the single dispersing particle diameter of type uhligite nano-powder is 15nm-300nm.
10. the ABO that method prepares according to any one of claim 1-9
3type uhligite nano-powder.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106064831A (en) * | 2016-05-13 | 2016-11-02 | 南京工业大学 | A kind of nano-particle embeds perovskite nano wire and forms the preparation method of composite |
| CN109721100A (en) * | 2019-03-21 | 2019-05-07 | 成都工业学院 | A kind of method of hydro-thermal method preparation nanometer barium zirconium phthalate |
| CN112209431A (en) * | 2020-09-28 | 2021-01-12 | 新昌中国计量大学企业创新研究院有限公司 | Functionalized BaTiO3Preparation method and application of nano material |
| CN112844354A (en) * | 2020-12-23 | 2021-05-28 | 甄崇礼 | Process for producing perovskite compound |
| CN113600169A (en) * | 2021-06-08 | 2021-11-05 | 电子科技大学长三角研究院(湖州) | Solid solution photocatalyst for photocatalytic oxidation degradation of toluene and preparation method thereof |
| CN114477273A (en) * | 2022-02-17 | 2022-05-13 | 重庆新申世纪新材料科技有限公司 | Hydrothermal preparation process of tetragonal phase nano barium titanate powder |
| CN114560496A (en) * | 2022-03-18 | 2022-05-31 | 中国科学院新疆理化技术研究所 | Method for preparing perovskite nano particles through low-temperature rheological phase |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106064831A (en) * | 2016-05-13 | 2016-11-02 | 南京工业大学 | A kind of nano-particle embeds perovskite nano wire and forms the preparation method of composite |
| CN109721100A (en) * | 2019-03-21 | 2019-05-07 | 成都工业学院 | A kind of method of hydro-thermal method preparation nanometer barium zirconium phthalate |
| CN112209431A (en) * | 2020-09-28 | 2021-01-12 | 新昌中国计量大学企业创新研究院有限公司 | Functionalized BaTiO3Preparation method and application of nano material |
| CN112844354A (en) * | 2020-12-23 | 2021-05-28 | 甄崇礼 | Process for producing perovskite compound |
| CN113600169A (en) * | 2021-06-08 | 2021-11-05 | 电子科技大学长三角研究院(湖州) | Solid solution photocatalyst for photocatalytic oxidation degradation of toluene and preparation method thereof |
| CN114477273A (en) * | 2022-02-17 | 2022-05-13 | 重庆新申世纪新材料科技有限公司 | Hydrothermal preparation process of tetragonal phase nano barium titanate powder |
| CN114560496A (en) * | 2022-03-18 | 2022-05-31 | 中国科学院新疆理化技术研究所 | Method for preparing perovskite nano particles through low-temperature rheological phase |
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|---|---|
| CN104477978B (en) | 2017-01-04 |
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