CN107188214A - A kind of preparation method of yttrium oxide nano-powder and nanostructured - Google Patents
A kind of preparation method of yttrium oxide nano-powder and nanostructured Download PDFInfo
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- CN107188214A CN107188214A CN201710059321.2A CN201710059321A CN107188214A CN 107188214 A CN107188214 A CN 107188214A CN 201710059321 A CN201710059321 A CN 201710059321A CN 107188214 A CN107188214 A CN 107188214A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of yttrium oxide nano-powder and the preparation method of nanostructured, yttrium oxide nano-powder is prepared as the sonochemical method of surfactant using aloe gel.Nucleation is formed using ultrasonic resonance bubble, with the explosion of bubble, conventional chemical key can be destroyed, and the hydrophilic primary surface of the organic matter in aloe gel can be attached to Y (OH)3Precipitation, in high-temperature calcination, before organic group is departed from by evaporation, the crystallization of assisted oxidation yttrium.So, by changing ultrasonic time, supersonic frequency, pH value and the amount of Aloe Vera Gel these conditions destroy different chemical bonds, ultimately result in different pattern and microstructure.Different industries requirement different from structure to yttrium oxide nano-powder pattern is met there is provided a kind of morphology controllable, the preparation method of the yttrium oxide nano-powder of different nanostructureds can be prepared in Same Way.
Description
Technical field
The present invention relates to a kind of method for preparing yttrium oxide nano-powder, more particularly to one kind can prepare yttrium oxide powder
The preparation method of different nanostructureds.
Background technology
Yittrium oxide, with unique optics and physicochemical properties, is widely used in height as important rare earth compound
The field such as level ceramic material, fluorescent material, catalysis, laser, material doped.Yittrium oxide is a kind of water insoluble and alkali, is dissolved in acid
White rare earth oxide, its molal weight is 225.82g/mol, density 5.01g/cm3, 2410 DEG C of fusing point belongs to cubic crystal
System.
Conventional yttrium oxide powder preparation method has ammonium bicarbonate precipitation method.Ammonium hydrogen carbonate is a kind of cheap precipitating reagent.
In the method, the inorganic salt solution of yttrium is directly reacted with bicarbonate by the aqueous solution, obtains the slurries of the carbonate containing yttrium；Then
A certain amount of soluble ammonium salt is added into slurries, is stirred, yittrium oxide is adjusted by adding the amount of soluble ammonium salt
Final size, slurries stand, are aged appropriate time at a certain temperature；It is aged washing of precipitate, filtering, proper temperature after terminating
Dry, calcining obtains yittrium oxide product.This method can obtain higher yittrium oxide yield under relatively low old, and also compared with
Large-scale production is easily formed, but is due to produce substantial amounts of bubble during ammonium bicarbonate precipitation, and during precipitation reaction
PH value is non-constant, forming core speed it is fast or it is slow be unfavorable for growing up for crystal, therefore hardly result in the oxidation of desired particle size and pattern
Yttrium powder product.
In addition, also having patent CN102145913A to disclose one kind prepares ball shaped nano yittrium oxide using spray granulation
The method of powder.Its specific preparation method:Powder is dissolved with salpeter solution first, ammonia precipitation process is then added, aged processing,
Filter, wash, being dried to obtain powdered presoma, then its presoma is handled with the steady plasma gun of ionized water, to preparing nanometer
Yittrium oxide primary granule is collected by distilled water, yttria particles are added binding agent, dispersant adjusted, ball milling, through spraying
Mist drying and granulating, finally carries out atmospheric plasma spray gun sintering processes, and screening obtains final products.It this method provide a kind of warp
The method of the suitable large-scale production ball shaped nano yttrium oxide powder of Ji environmental protection, solves original particle dehydration efficiency in conventional method
Lowly, aggregate sintering densification is difficult and the problems such as low yield.
Although above method can produce yttrium oxide nano-powder with higher efficiency and yield, can not have
The pattern and structure of effect ground control yttrium oxide nano-powder, or can only be single pattern and structure.Therefore, we have invented
One kind, by changing concentration and reaction condition, can be aoxidized in Same Way by surfactant of aloe gel
The different-shape and structure of yttrium nano-powder, so meet different industries will to the difference of yttrium oxide nano-powder pattern and structure
Ask.In addition, the method can also be used to prepare other oxides and rear-earth-doped.
The content of the invention
The purpose of the present invention be meet different industries it is different from structure to yttrium oxide nano-powder pattern require there is provided one
Morphology controllable is planted, the preparation method of the yttrium oxide nano-powder of different nanostructureds can be prepared in Same Way.The present invention
Use the sonochemical method by the use of aloe gel as surfactant.In the present invention, ultrasonic resonance gas is utilized
Bubble forms nucleation, with the explosion of bubble, can destroy conventional chemical key, and the hydrophilic primary surface of the organic matter in aloe gel
Y (OH) can be attached to3Precipitation, in high-temperature calcination, before organic group is departed from by evaporation, the crystallization of assisted oxidation yttrium.This
Sample, by changing ultrasonic time, supersonic frequency, pH value and the amount of Aloe Vera Gel these conditions are destroyed different chemical bonds, finally led
The different pattern of cause and microstructure.
The preparation method of a kind of yttrium oxide nano-powder provided by the present invention and nanostructured, it is specific as follows：
(1) raw material：Y(NO3)3:H2O, ammoniacal liquor is as precipitating reagent, and aloe gel is surfactant；Distilled water conduct
Solvent；
(2) precipitation solution is prepared：First by raw material Y (NO3)3:H2O and aloe gel are uniformly mixed in aqueous, wherein,
Y3+Concentration be 0.1~0.4mol/L, the addition of aloe gel is 200~600ml/L, then by ammoniacal liquor slowly added to mixed
It is 7~9 to close in solution to pH value, and mixed solution carries out sonic oscillation in frequency for 20kHz~50kHz ultrasonic wave, and the time is
1h~6h, during which solution temperature be maintained at 50~80 DEG C, finally obtain white precipitate；
(3) precipitation of acquisition is respectively washed after 3~5 times with distilled water and absolute ethyl alcohol and carries out drying and processing, temperature is
70~120 DEG C, the time is 6h~24h；
(4) calcining heat treatment：Powder after being dried in step (3) is subjected to high-temperature calcination, calcining heat is 700~1200
DEG C, the time is 2~6h.
Beneficial effect
1. the preparation method of the different nanostructureds of yttrium oxide powder can be prepared the invention provides a kind of, to equipment requirement
Low, cost is low, yield is high, morphology controllable, epigranular.It is adapted to scale to produce in enormous quantities, product quality degree of unification is higher.
2. the method for preparing yttrium oxide nano-powder proposed by the invention, by changing supersonic frequency, ultrasonic time, PH
The addition of value and aloe gel, can finally effectively obtain the different microstructures of yttrium oxide nano-powder, typically have：
Spherical, petal, petal shape, mushroom shape etc., and then different industries can be met to yttrium oxide powder pattern and microstructure not
Same demand.
3. by the yttrium oxide powder prepared by preparation method proposed by the invention, it can effectively improve pattern and microcosmic
Structure, obtains preferable particle size uniformity, the problem of effectively improving yttrium oxide powder poor fluidity in spraying industry, and then
Effectively enhance the coating quality of yttrium oxide powder.
4. the method can also be expanded mixes oxidation for preparing other rare earth oxides (gadolinium oxide, luteium oxide etc.), rare earth
Thing etc..
Embodiment
With reference to instantiation, the present invention is described further, but the protection model of the present invention should not be limited with this
Enclose.
Embodiment 1 (ball-type)
(1) raw material Y (NO are weighed3)3:H2The quality of O and ammoniacal liquor is respectively 4g and 1.91g；
(2) Y (NO for being weighed step (1)3)3:H2O and ammoniacal liquor raw material are slowly mixed together and added with 50ml distilled water
Enter 30ml aloe gel, solution pH value remains 7；
(3) ultrasonic wave for being 20kHz with frequency carries out sonic oscillation, and the time is 6h, and during which solution temperature remains 80 DEG C,
It is final to obtain white precipitate；
(4) by the precipitation distilled water obtained in step (3) and alcohol washes 3 times, drying and processing, temperature are then carried out
For 70 DEG C, the time is 6h；
(5) powder after being dried in step (4) is subjected to high-temperature calcination, calcining heat is 700 DEG C, and the time is 2h；
(6) powder after calcining is carried out to the yttrium oxide nano-powder for finding finally to obtain after sign processing, observation with SEM
Microstructure to be spherical, its particle diameter is 30~50nm.
Embodiment 2 (petal shape)
(1) raw material Y (NO are weighed3)3:H2The quality of O and ammoniacal liquor is respectively 5g and 2.98g；
(2) Y (NO for being weighed step (1)3)3:H2O and ammoniacal liquor raw material are slowly mixed together and added with 50ml distilled water
Enter 15ml aloe gel, solution pH value remains 8；
(3) ultrasonic wave for being 26kHz with frequency carries out sonic oscillation, and the time is 5h, and during which solution temperature remains 60 DEG C,
It is final to obtain white precipitate；
(4) by the precipitation distilled water obtained in step (3) and alcohol washes 4 times, drying and processing, temperature are then carried out
For 100 DEG C, the time is 20h；
(5) powder after being dried in step (4) is subjected to high-temperature calcination, calcining heat is 1000 DEG C, and the time is 4h；
(6) powder after calcining is carried out to the yttrium oxide nano-powder for finding finally to obtain after sign processing, observation with SEM
Microstructure be petal shape, its particle diameter be 50~80nm.
Embodiment 3 (mushroom shape)
(1) raw material Y (NO are weighed3)3:H2The quality of O and ammoniacal liquor is respectively 6g and 4.3g；
(2) Y (NO for being weighed step (1)3)3:H2O and ammoniacal liquor raw material are slowly mixed together and added with 50ml distilled water
Enter 25ml aloe gel, solution pH value remains 9；
(3) ultrasonic wave for being 30kHz with frequency carries out sonic oscillation, and the time is 5h, and during which solution temperature remains 50 DEG C,
It is final to obtain white precipitate；
(4) by the precipitation distilled water obtained in step (3) and alcohol washes 5 times, drying and processing, temperature are then carried out
For 120 DEG C, the time is 24h；
(5) powder after being dried in step (4) is subjected to high-temperature calcination, calcining heat is 1100 DEG C, and the time is 5h；
(6) powder after calcining is carried out to the yttrium oxide nano-powder for finding finally to obtain after sign processing, observation with SEM
Microstructure be mushroom shape, its particle diameter be 60~100nm.
Embodiment 4 (petal)
(1) raw material Y (NO are weighed3)3:H2The quality of O and ammoniacal liquor is respectively 6g and 3.58g；
(2) Y (NO for being weighed step (1)3)3:H2O and ammoniacal liquor raw material are slowly mixed together and added with 50ml distilled water
Enter 30ml aloe gel, solution pH value remains 8；
(3) ultrasonic wave for being 50kHz with frequency carries out sonic oscillation, and the time is 5h, and during which solution temperature remains 80 DEG C,
It is final to obtain white precipitate；
(4) by the precipitation distilled water obtained in step (3) and alcohol washes 4 times, drying and processing, temperature are then carried out
For 120 DEG C, the time is 24h；
(5) powder after being dried in step (4) is subjected to high-temperature calcination, calcining heat is 1200 DEG C, and the time is 6h；
(6) powder after calcining is carried out to the yttrium oxide nano-powder for finding finally to obtain after sign processing, observation with SEM
Microstructure to be petal, its particle diameter is 40~80nm.
Examples detailed above is the present invention preferably embodiment, but embodiments of the present invention are not limited by examples detailed above
System, other it is any without departing from spirit of the invention and the modification made under principle, modification, replacement, combine, simplification is equivalent
Substitute mode, be included within protection scope of the present invention.
Claims (2)
1. the preparation method of a kind of yttrium oxide nano-powder and nanostructured, it is characterised in that use aloe gel conduct
The sonochemical method of surfactant prepares yttrium oxide nano-powder, and its step is as follows：
(1) raw material：Y(NO3)3:H2O, ammoniacal liquor is as precipitating reagent, and aloe gel is surfactant；Distilled water is as molten
Agent；
(2) precipitation solution is prepared：First by raw material Y (NO3)3:H2O and aloe gel are uniformly mixed in aqueous, wherein, Y3+'s
Concentration is 0.1~0.4mol/L, and the addition of aloe gel is 200~600ml/L, then ammoniacal liquor is slowly molten added to mixing
In liquid to pH value be 7~9, mixed solution frequency for 20kHz~50kHz ultrasonic wave carry out sonic oscillation, the time be 1h~
6h, during which solution temperature be maintained at 50~80 DEG C, finally obtain white precipitate；
(3) precipitation of acquisition is respectively washed after 3~5 times with distilled water and absolute ethyl alcohol and carries out drying and processing, temperature be 70~
120 DEG C, the time is 6h~24h；
(4) calcining heat treatment：Powder after being dried in step (3) is subjected to high-temperature calcination, calcining heat is 700~1200 DEG C,
Time is 2~6h.
2. the preparation method of a kind of yttrium oxide nano-powder according to claim 1 and nanostructured, it is characterised in that logical
Control additive concentration and reaction condition to be crossed, the yttrium oxide powder of different nanostructureds can be obtained, particle size range is 30~
100nm.It is that (1) is 500~600ml/L in the addition of aloe gel respectively, supersonic frequency is 20~30kHz, pH value control
7~8, ultrasonic time is in 5~6h condition and range, being shaped as generation is spherical；(2) it is in the addition of aloe gel
500~600ml/L, ultrasonic time is 1~5h, pH value control 7~8, supersonic frequency in 40~50kHz condition and range,
Being shaped as producing is petal；(3) it is 200~400ml/L in the addition of aloe gel, ultrasonic time is 1~5h, pH value control
System is 7~8, and supersonic frequency is in 20~30kHz condition and range, and generation is shaped as petal shape；(4) adding in aloe gel
Dosage is 500~600ml/L, and ultrasonic time is 1~5h, and supersonic frequency is 20~30kHz, condition model of the pH value control 8~9
In enclosing, generation is shaped as mushroom shape.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533157A (en) * | 2020-04-24 | 2020-08-14 | 广西科学院 | Microwave calcination preparation method of gadolinium oxide nano powder |
| CN117466251A (en) * | 2023-11-22 | 2024-01-30 | 山东科源生化有限公司 | Method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide |
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| CN101698609A (en) * | 2009-11-04 | 2010-04-28 | 中国科学院上海硅酸盐研究所 | Method for preparing spherical, monodisperse and single-size yttrium oxide nano-powder |
| CN102145913A (en) * | 2011-04-21 | 2011-08-10 | 北京矿冶研究总院 | Preparation method of nano spherical yttrium oxide powder for thermal spraying |
| CN104308177A (en) * | 2014-10-14 | 2015-01-28 | 钱景 | Preparation method of graphene-loaded nano-silver composite material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533157A (en) * | 2020-04-24 | 2020-08-14 | 广西科学院 | Microwave calcination preparation method of gadolinium oxide nano powder |
| CN117466251A (en) * | 2023-11-22 | 2024-01-30 | 山东科源生化有限公司 | Method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide |
| CN117466251B (en) * | 2023-11-22 | 2024-04-05 | 山东科源生化有限公司 | Method for preparing yttrium perchlorate by utilizing rare earth yttrium oxide |
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