CN108640144A - A kind of yttrium oxide twin-stage nanosphere and preparation method thereof - Google Patents
A kind of yttrium oxide twin-stage nanosphere and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention discloses a kind of yttrium oxide twin-stage nanosphere, and the yttrium oxide twin-stage nanosphere is assembled by yttrium oxide level-one nanosphere and yttrium oxide two level nanosphere, a diameter of 20~150nm of two level nanosphere, and level-one nanometer bulb diameter is less than 5nm；The ratio of level-one nanosphere and two level nanosphere is 10:1~2.The ratio is mass ratio.With further, the level-one nanosphere is located at the piling up in space of two level nanosphere.The invention also discloses the preparation methods that above-mentioned yttrium oxide double-clicks nanosphere.Compared with general direct liquid-phase precipitation method, subject matter nodularization degree and crystallization degree are high, and surface is smooth, thus not only can avoid agglomeration, but also can significantly reduce the mechanical entrainment of impurity so that product excellent physical properties and chemical purity is high.
Description
Technical field
The invention belongs to technical field of material.It is related to a kind of yttrium oxide twin-stage nanosphere and preparation method thereof.
Background technology
Yttrium oxide (Y2O3) there are superior physical and chemical properties, in anticorrosive, heat-resisting, magnetic and dielectric constant etc.
Aspect shows unique superiority；The yttrium oxide of nanosizing is having outside original property, while it is exclusive to have both nano material
Characteristic makes it obtain the incomparable characteristic of regular oxidation yttrium material, and after nano yttrium oxide spheroidization, there will be higher ratio
Surface area, surface energy and better mobility and dispersibility, make the performances such as its light, electricity, magnetic, power be increased dramatically, wide
It is general to be applied to the fields such as optical material, ceramic material, catalysis material, magnetic material and micro- rare-earth alloy material.
Twin-stage nano material is because of its special structure, in electrical properties, magnetic property, optical property, mass-energy, hot
Matter, catalytic property and mechanical property etc. further show the property better than single-stage nano material, make the application neck of yttrium oxide
Domain has obtained further widening, while improving the performance of following process product.
Currently, the technique for preparing nano yttrium oxide is more, main preparation method is divided into three categories, solid phase method, vapor phase method
And liquid phase method, wherein liquid phase method be divided into for：Spray pyrolysis, hydrothermal synthesis method, microemulsion method, sol-gel method, burning are closed
At method and the precipitation method.
The report that nano yttrium oxide is prepared using the precipitation method is relatively more, and two kinds of situations are primarily present in preparation process：One
Class is that the coating materials such as activating agent, dispersant, template are added to prevent from reuniting, and promotes the formation of single dispersion powder,
Which not only improves costs, it is also possible to the purity of product be made to affect；Though another kind of do not add coating material,
Its molar ratio by expanding urea and ruthenium ion, the concentration for reducing ruthenium ion realizes the preparation of nanoscale yttrium, in the party
Under formula, preparation time is long, and the particle size distribution that low output obtains simultaneously is wide.
About the research of the spherical yttrium oxide of nanometer, mostly to prepare single stage format as main study subject.For microwave and surpass
The double outfield collaboration Liquid-phase reactor (abstraction instrument) of sound wave are chiefly used in organic extraction research, close though having ripe experimental facilities
In the research for preparing yttrium oxide twin-stage nanosphere with it there is not yet open report.
Invention content
Goal of the invention：That the purpose of the present invention is to provide a kind of nano-meter characteristics than general nano-powder is more prominent, tool
There is the yttrium oxide powder material of special twin-stage nanometer spherical structure；It is another object of the present invention to provide a kind of using simple
The method that easy liquid-phase precipitation technique can prepare the yttrium oxide twin-stage nanosphere of special construction.
Inventive principle：(1) microwave and ultrasonic synergistic liquid phase synthesis yttrium oxide forerunner's body technique are used, ultrasound is made full use of
" synergistic effect " of wave " cavitation " and microwave " interior heating " promotes feed liquid Y3+·6H2H is coordinated in O2The removing of O, precipitating reagent
Middle CO3 -2With OH-Cracking and hydroxyl radical free radical generation；In addition the technology that ammonium hydroxide is added on the basis of precipitation from homogeneous solution is taken
Measure makes OH in system-Activity increases by geometric progression, and then accelerated oxidation yttrium presoma Y (OH) CO3·xH2O (Fig. 4) nucleus
Formation, the rearrangement of lattice, the removing of hydration shell and the crystallization water, the raising of the refinement of crystal grain and spheroidization and crystallization degree.
(2) under above-mentioned synergistic effect, the primary crystal that system generates is the Y that size distribution is uniform, grain size is minimum2O3Presoma
Nanosphere, in order to reduce the huge surface free energy of system, primary crystal, that is, level-one nanosphere is spontaneous and is accumulated in an orderly manner as more
Stable two level nanosphere, i.e. self assembly are gathered into Y2O3Presoma twin-stage nanosphere；In presoma thermal decomposition process, each one
Grade and two level presoma nanosphere by being reduced with shrinking neuclear dynamics model equal proportion, in other words, as long as control is appropriate
Heat decomposition temperature, subject matter can inherit the twin-stage nanosphere structure feature of its presoma, but crystal grain can be refined further, dispersibility
It can further increase.
Technical solution：The present invention discloses a kind of yttrium oxide twin-stage nanosphere, and the yttrium oxide twin-stage nanosphere is by aoxidizing
Yttrium level-one nanosphere is assembled with yttrium oxide two level nanosphere, and a diameter of 20~150nm of two level nanosphere, level-one is received
Rice bulb diameter is less than 5nm；The ratio of level-one nanosphere and two level nanosphere is 10:1~2.The ratio is mass ratio.Follow-up
One step, the level-one nanosphere is located at the piling up in space of two level nanosphere.
The present invention provides the preparation methods of above-mentioned yttrium oxide twin-stage nanosphere, it is characterised in that includes the following steps：
(1) using yttrium chloride or yttrium nitrate solution as raw material, using urea and ammonium hydroxide as compound precipitants, the material that will centainly match
Liquid is uniformly mixed with precipitating reagent using ultrasonic wave；
(2) uniformly mixed solution is placed in microwave with ultrasonic synergistic Liquid-phase reactor, controls ultrasonic wave/microwave mode
Formula is 1:2 or 2:1；Ultrasonic power intensity is 300~1500WL-1Solution；Microwave power intensity is 300~1000WL-1
Solution；
(3) 80~90 DEG C of controlling reaction temperature, 0.5~1.5h of reaction time；
(4) heat filtering, washing are carried out to sediment；
(5) it after presoma is dry at 100~150 DEG C, is thermally decomposed at 770~850 DEG C of temperature, heat preservation 1~
2.5h obtains target product.
Specifically, in step (1), feed liquid is yttrium chloride (YCl3) or yttrium nitrate (Y (NO3)3) solution, a concentration of 0.02
~0.1molL-1。
Specifically, in step (1), compound precipitants are by urea (CO (NH2)2) and ammonium hydroxide (NH4OH it) forms, wherein c
(CO(NH2)2)：c(NH4OH)=1:0~3:10-8, (CO (NH2)2) a concentration of 2~3molL-1。
Specifically, in step (1), CO (NH2)2With Y3+Molar ratio be n (CO (NH2)2)：n(Y3+)=20~100.
Specifically, in step (1) and (2), the frequency of ultrasonic wave is 20~25kHz.
More specifically heretofore described ultrasonic wave/microwave mode 2:1 refer to ultrasonic wave work 2s after, be switched to microwave
Work 1s, and the two works alternatively, and as the period, cycle operation is until reaction terminates.
Specifically, in step (4), the filter type is heat filtering, i.e., reaction is filtered immediately after having terminated, and is washed
It is deionized water of the temperature control at 80~90 DEG C to wash with water.
Advantageous effect：(1) the yttrium oxide twin-stage nanosphere ontology D that the present invention announces50It can be adjusted within the scope of 20~150nm
Control, preferably 30~100nm, within this range, each two level nanosphere ontology is in respectively bulk (Fig. 6,9)；Constitute the level-one of ontology
Nanosphere D50It is apparent (Fig. 8) less than 5nm and its nanocrystalline feature；Compared with general single-stage nanosphere, the nanometer of twin-stage nanosphere
Characteristic is more prominent.
(2) compared with general direct liquid-phase precipitation method, subject matter nodularization degree and crystallization degree are high (Fig. 2,8), and surface is smooth,
Thus not only can avoid agglomeration, but also the mechanical entrainment of impurity can be significantly reduced so that product excellent physical properties and change
It is again high to learn purity.
(3) compared with general homogeneous precipitation method, CO (NH that the present invention uses2)2With Y3+Molar ratio smaller, that is, allow
YCl3Feed concentration higher so that its production efficiency higher；In addition, not only making reaction speed accelerate, be not necessarily to by adding ammonium hydroxide
Using the hydro-thermal method of supercharging, and can be by controlling the optimum organization of ammonia concn and condition of external field to regulate and control the grain of nanosphere
Diameter.
(4) present invention process flow is simple and operating condition is controllable (Fig. 1), is easy to industrialization promotion application.
Description of the drawings
Fig. 1 is the techniqueflow chart of the present invention.
Fig. 2 is yttrium oxide X-ray diffraction (XRD) figure that the present invention is prepared.
Fig. 3 is differential thermal-thermogravimetric (TG-DTA) curve for the yttrium oxide presoma that the present invention is prepared.
Fig. 4 is FTIR spectrum (FI-IR) figure of yttrium oxide presoma and yttrium oxide that the present invention is prepared.
Fig. 5 is presoma scanning electron microscope (SEM) figure of embodiment 1.
Fig. 6 is product transmission electron microscope (TEM) figure of embodiment 1.
Fig. 7 is transmission electron microscope (TEM) figure of the product individual particle of embodiment 1.
Fig. 8 is the electronic diffraction collection of illustrative plates of 1 product of embodiment.
Fig. 9 is product transmission electron microscope (TEM) figure of embodiment 2.
Figure 10 is transmission electron microscope (TEM) figure of the product individual particle of embodiment 2.
Figure 11 is Product scan electron microscope (SEM) figure of embodiment 3.
Figure 12 is Product scan electron microscope (SEM) figure of embodiment 3.
Specific implementation mode：
The present invention is further illustrated with case study on implementation below in conjunction with the accompanying drawings：
Embodiment 1
Take 0.025molL-1Yttrium chloride solution and 2molL-1Isometric urea liquid, wherein c (NH3·H2O)
=10-10mol·L-1, rare earth feed liquid is uniformly mixed with compound precipitants using mechanical agitation mode；It is molten by what is be uniformly mixed
Liquid is placed in microwave with ultrasonic synergistic Liquid-phase reactor, and ultrasonic frequency 25KHz, controlling ultrasonic wave/microwave mode is
2:1, ultrasonic power intensity 700WL-1, microwave power intensity 500WL-1, reaction time 1h, 90 DEG C of reaction temperature obtains
Yttrium oxide presoma；It is filtered, washed 3 times to the end of reaction and obtains filter cake；In temperature after presoma is dried at 100 DEG C
It is thermally decomposed at 800 DEG C, keeps the temperature 2h, be cooled to room temperature, you can obtain twin-stage nano yttrium oxide.
Fig. 2 is yttrium oxide X-ray diffraction (XRD) figure being prepared, and shows its well-crystallized, is typical cubic crystal
It is yttrium oxide crystallization.
Fig. 3 is differential thermal-thermogravimetric (TG-DTA) curve for the yttrium oxide presoma being prepared, and shows yttrium oxide presoma
It is divided into two stages completions, complete heat decomposition temperature is 768 DEG C.
Fig. 4 is FTIR spectrum (FI-IR) figure of the yttrium oxide presoma and yttrium oxide that are prepared, shows liquid phase
There are O-H keys and C-O keys in presoma prepared by the precipitation method, obtained presoma is basic yttrium carbonate：Y(OH)
CO3·H2O；There are Y-O keys in thermal decomposition product, and product is yttrium oxide after illustrating thermal decomposition：Y2O3。
The SEM figures of yttrium oxide product and TEM scheme such as the institutes of Fig. 5~7 after the yttrium oxide presoma being prepared and its thermal decomposition
Show, and combine obtained SEM or TEM figures, by Image Tool softwares, obtains the average grain diameter of yttrium oxide nanosphere ontology
(involved in the present invention to average grain diameter be to be calculated by this method), shows two level nanosphere D50About 80nm, with
The average grain diameter 94nm of its presoma is compared, and is slightly shunk.Multiple specks are clearly displayed by Fig. 7, each speck corresponds to one
Level-one nanosphere, by measuring two neighboring speck centre-to-centre spacing it can be confirmed that constituting the level-one nanosphere D of ontology50≤5nm.Fig. 8 is
The electronic diffraction collection of illustrative plates of particle corresponding to Fig. 7, particle surface diffraction annular in shape, the yttrium oxide further illustrated are received for twin-stage
Rice chondritic, the nanocrystalline feature of level-one nanosphere are apparent.
Embodiment 2
Take 0.05molL-1Yttrium chloride solution and 2.5molL-1Isometric urea liquid, wherein c (NH3·H2O)
=10-8mol·L-1, rare earth feed liquid is uniformly mixed with compound precipitants using the ultrasonic homogenizer of 20KHz；It will mix
Uniform solution is placed in microwave and ultrasonic synergistic Liquid-phase reactor, ultrasonic frequency 25KHz, control ultrasonic wave/micro-
Wave mode is 2:1, ultrasonic power intensity 900WL-1, microwave power intensity 700WL-1, reaction time 0.75h, reaction temperature
95 DEG C of degree, obtains yttrium oxide presoma；It is filtered, washed 3 times to the end of reaction and obtains filter cake；Presoma is done at 90 DEG C
It is thermally decomposed at 780 DEG C of temperature after dry, keeps the temperature 2.5h, be cooled to room temperature, you can obtain twin-stage nano yttrium oxide.It is prepared into
The TEM figures of the yttrium oxide arrived as shown in Figures 9 and 10, show that the average grain diameter of yttrium oxide two level nanosphere is about 30nm, if continuing to carry
High ammonia concn has the tendency that Oxygen potential and Monodispersed reduce though nanosphere particle can be made further to refine.
Embodiment 3
Take 0.075molL-1Yttrium chloride solution and 3molL-1Isometric urea liquid, wherein c (NH3·H2O)
=10-9, rare earth feed liquid is uniformly mixed with compound precipitants；The solution being uniformly mixed is placed in microwave and ultrasonic synergistic liquid
In phase reaction device, control ultrasonic wave/microwave mode is 2:1, ultrasonic power intensity 900WL-1, microwave power intensity 600W
L-1, reaction time 0.5h, 90 DEG C of reaction temperature obtains yttrium oxide presoma；2 times are filtered, washed to the end of reaction to obtain
Filter cake；By presoma at 100 DEG C it is dry after thermally decompose at 800 DEG C of temperature, keep the temperature 1.5h, be cooled to room temperature, you can
Multi-stage nano yttrium oxide is obtained, SEM figures are as shown in figure 11, and average grain diameter is about 68nm.
Embodiment 4
Take 0.05molL-1Yttrium nitrate solution and 2molL-1Isometric urea liquid, wherein c (NH3·H2O)=
10-9mol·L-1, rare earth feed liquid is uniformly mixed with compound precipitants using the ultrasonic homogenizer of 20KHz；It will mix
Even solution is placed in microwave with ultrasonic synergistic Liquid-phase reactor, and control ultrasonic wave/microwave mode is 2:1, ultrasonic frequency
For 25KHz, ultrasonic power intensity 800WL-1, microwave power intensity 400WL-1, reaction time 0.75h, reaction temperature 85
DEG C, obtain yttrium oxide presoma；It is filtered, washed 2 times to the end of reaction and obtains filter cake；Presoma is dry at 100 DEG C
It is thermally decomposed at 850 DEG C of temperature afterwards, keeps the temperature 1h, be cooled to room temperature, you can obtain twin-stage nano yttrium oxide, SEM schemes such as
Shown in Figure 12, average grain diameter is about 72nm.
In conclusion of the present invention is to cooperate with auxiliary liquid phase synthesis presoma with the double outfields of ultrasonic wave based on microwave
Method, according to the present invention the yttrium oxide powder obtained by method be Monodispersed twin-stage nanosphere, two level nanosphere ontology granularity
Controllably in 20~100nm, the level-one nanosphere grain size for constituting ontology is less than 5nm.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
It, for those skilled in the art, still can be with although describing the invention in detail with reference to the foregoing embodiments
Technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.It is all
The present invention design under the premise of, made by it is any modification, improve etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of yttrium oxide twin-stage nanosphere, it is characterised in that：The yttrium oxide twin-stage nanosphere is by yttrium oxide level-one nanometer
Ball is assembled with yttrium oxide two level nanosphere, a diameter of 20~150nm of two level nanosphere, and level-one nanometer bulb diameter is small
In 5nm；The ratio of level-one nanosphere and two level nanosphere is 10:1~2.
2. yttrium oxide twin-stage nanosphere according to claim 1, it is characterised in that：The level-one nanosphere is received positioned at two level
Rice ball is piled up in space.
3. the preparation method of yttrium oxide twin-stage nanosphere described in claim 1, it is characterised in that include the following steps：
(1) using yttrium chloride or yttrium nitrate solution as raw material, using urea and ammonium hydroxide as compound precipitants, feed liquid and precipitating reagent are used
Ultrasonic wave is uniformly mixed；
(2) uniformly mixed solution is placed in microwave and ultrasonic synergistic Liquid-phase reactor, control ultrasonic wave/microwave mode is
1:2 or 2:1；Ultrasonic power intensity is 300~1500WL-1Solution；Microwave power intensity is 300~1000WL-1It is molten
Liquid；
(3) 80~90 DEG C of controlling reaction temperature, 0.5~1.5h of reaction time；
(4) heat filtering, washing are carried out to sediment；
(5) it after presoma is dry at 100~150 DEG C, is thermally decomposed at 770~850 DEG C of temperature, keeps the temperature 1~2.5h,
Obtain target product.
4. according to the preparation method described in claim 3, it is characterised in that：In step (1), feed liquid is yttrium chloride or nitric acid
Yttrium solution, a concentration of 0.02~0.1molL-1。
5. according to the preparation method described in claim 3, it is characterised in that：In step (1), compound precipitants are by CO
(NH2)2With NH4OH is formed, wherein c (CO (NH2)2)：c(NH4OH)=1:0~3:10-8, CO (NH2)2A concentration of 2~3molL-1。
6. according to the preparation method described in claim 3, it is characterised in that：In step (1), CO (NH2)2With Y3+Mole
Than for n (CO (NH2)2)：n(Y3+)=20~100.
7. according to the preparation method described in claim 3, it is characterised in that：In step (1) and (2), the frequency of ultrasonic wave
For 20~25kHz.
8. according to the preparation method described in claim 3, it is characterised in that：Ultrasonic wave/microwave mode 2:1 refers to ultrasonic wave work
After making 2s, it is switched to microwave operational 1s, the two works alternatively, and as the period, cycle operation is until reaction terminates.
9. according to the method described in claim 3, it is characterised in that：In step (4), the filter type is hot mistake
Filter, i.e. reaction are filtered immediately after having terminated, and slurry is deionized water of the temperature control at 80~90 DEG C.
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