CN108675336A - The method that microwave cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave - Google Patents
The method that microwave cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 20
- 239000007791 liquid phase Substances 0.000 title claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 23
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 7
- 230000001376 precipitating effect Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000013049 sediment Substances 0.000 claims abstract description 6
- 230000002153 concerted effect Effects 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052771 Terbium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 230000009471 action Effects 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 2
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 2
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 2
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims description 2
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 20
- 239000000463 material Substances 0.000 abstract description 13
- 239000003795 chemical substances by application Substances 0.000 abstract description 11
- 230000003213 activating effect Effects 0.000 abstract description 6
- 239000002270 dispersing agent Substances 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 230000036632 reaction speed Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 10
- 239000002077 nanosphere Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 230000002195 synergetic effect Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- GEZAXHSNIQTPMM-UHFFFAOYSA-N dysprosium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Dy+3].[Dy+3] GEZAXHSNIQTPMM-UHFFFAOYSA-N 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- -1 nitric acid rare earth Chemical class 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MAYVZUQEFSJDHA-UHFFFAOYSA-N 1,5-bis(methylsulfanyl)naphthalene Chemical compound C1=CC=C2C(SC)=CC=CC2=C1SC MAYVZUQEFSJDHA-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910002110 ceramic alloy Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- BOXVSFHSLKQLNZ-UHFFFAOYSA-K dysprosium(iii) chloride Chemical compound Cl[Dy](Cl)Cl BOXVSFHSLKQLNZ-UHFFFAOYSA-K 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005393 sonoluminescence Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Geology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention has captured a kind of method that microwave cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave, specially：Using the rare-earth chlorination solution of a concentration of 0.02~0.1molL 1 as stoste, using urea as precipitating reagent, stoste and precipitating reagent are stirred evenly, obtain mixed liquor；By above-mentioned mixed liquor, microwave and the double outfield concerted reactions of ultrasonic wave are carried out, sediment is obtained；Gained sediment is subjected to heat filtering, washing, drying successively again；Then it is thermally decomposed, obtains target product.Compared with general homogeneous precipitation method, the method for the present invention, reaction speed is fast, without the hydro-thermal method of supercharging；Without adding the coating materials such as any activating agent, dispersant and template, you can obtain high purity rare earth oxides, avoid coating material and impacted to product purity.
Description
Technical field
The invention belongs to technical field of material.It is related to a kind of system of specific physical performance RE oxide powder material
Standby technology, and in particular to one kind is cooperateed with using microwave with the double outfields of ultrasonic wave using nitric acid rare earth or rare-earth chlorination liquid as raw material
The method of liquid phase synthesis nano rareearth oxidate powder body material.
Background technology
Rare earth oxide makes it have unique chemistry and physical property because of its special electron structure, light,
Electricity, magnetic, sound, power etc. show the characteristic better than non-rare earth material.And the rare earth oxide of nanosizing have it is original
Outside rare earth property, while having both the exclusive characteristic of nano material；Further, after oxide nano rare earth spheroidization, will have
Higher specific surface area, surface energy and better mobility and dispersibility, and the performances such as its light, electricity, magnetic, power is made to obtain into one
Step is promoted, to be widely used in optical material, catalysis material, magnetic material, glass and ceramic material, alloy or composite wood
Material etc. field.
At present prepare superfine rare-earth oxide method still based on liquid phase method, include the precipitation method, sol-gel method,
Hydro-thermal method, microemulsion method, spray pyrolysis etc., wherein again the most universal with the application of the precipitation method.
The common precipitation method mainly have direct precipitation method, homogeneous precipitation method, alcohol Hydrolyze method and complexed-precipitation method.It is wherein straight
It connects the precipitation method and homogeneous precipitation method is easier to industrialization.
It is well known that homogeneous precipitation method is more easy to obtain spherical oxide nano rare earth, thus researcher is numerous.But at present
There are still some technical problems for the phase precipitation method：(1) existing precipitation from homogeneous solution be by heat slowly and equably release structure crystalline substance from
Son, make its combined with rare earth ion generate presoma precipitation, thus reaction speed and its slowly, even if its use collaboration be pressurized
Hydro-thermal method also tends to take for ten a few houres；(2) this method usually requires to introduce activating agent, dispersant, inhibitor or template etc.
Dressing agent not only increases manufacturing cost, and may affect to the purity of product.
Invention content
Goal of the invention：The present invention is to solve above-mentioned homogeneous precipitation method long preparation period, the technical problems such as dressing agent need to be added,
There is provided that a kind of reaction speed is fast, prepares rare earth without be added the dressing agents such as any activating agent, dispersant, inhibitor or template
The liquid precipitation of oxide nano sphere powder body material.
Inventive principle：Microwave frequency makes polar molecule in solution is per second to generate 24.5 hundred million times up to 2450 megahertzs of height
Orientation, resonance motion, not only make heating more rapidly, evenly, no temperature gradient, without hysteresis effect etc., and and play soft template
The effect of agent avoids the agglomeration of small grains to greatly shorten liquid phase crystallization nucleation induction period and crystallization reaction time.
Ultrasonic wave refers to sound wave of the frequency range in 15k~10MHz, is mainly derived from using power in chemical field
The cavitation effect of ultrasonic wave and its strong shock wave of initiation and speed are higher than 110ms-1Microjet, and then generate machinery effect
Answer (acoustic streaming, shock wave, microjet etc.), fuel factor (5000K, 1800atm localized hyperthermia high pressure, whole to heat up), luminous effect
(sonoluminescence) and activating effect (hydroxyl radical free radical is generated in aqueous solution), four kinds of effects and non-orphaned, but interact, phase
Mutually promote, accelerates reaction process.This cavitation of ultrasonic wave greatly improves heterogeneous reaction rate, realizes heterogeneous reaction object
Between uniform mixing, accelerate the diffusion of reactants and products, promote the formation of solid cenotype, control size and the distribution of particle.
Thus ultrasonic wave plays the role of similar dispersant, activating agent in crystallization process.
Microwave generates " non-thermal effect " with the double outfield synergistic effects of ultrasonic wave, reduces nucleation activation energy, urges in other words
Change the effect of " induction " fast nucleation, it is uniform and fast for the shortening of induction period, the quick formation of nucleus, the rearrangement of lattice, crystal
Speed grows up, the removing of the crystallization water, the refinement of crystal grain create advantage.Thus, microwave acts synergistically with the double outfields of ultrasonic wave
More than single microwave or ul-trasonic irradiation, can with auxiliary liquid phase synthesis Monodispersed nanometer rare earth oxide ball.
Technical solution：Microwave provided by the present invention cooperates with auxiliary liquid phase synthesis rare earth oxide to receive with the double outfields of ultrasonic wave
The method of rice ball, specially：With a concentration of 0.02~0.1molL-1Rare-earth chlorination solution be stoste, with urea be precipitation
Agent stirs evenly stoste and precipitating reagent, obtains mixed liquor；By above-mentioned mixed liquor, microwave and the double outfields of ultrasonic wave are carried out
Concerted reaction obtains sediment；Gained sediment is subjected to heat filtering, washing, drying successively again；Then it is thermally decomposed, is obtained
To target product.
Specifically, the rare-earth chlorination solution can be lanthanum chloride, dysprosium chloride, erbium chloride etc..
Specifically, the mol ratio of the precipitating reagent urea and ammonium hydroxide is 1:0~3:10-8, and urea and rare-earth chlorination
The mol ratio of solution is 20~100.
Specifically, the microwave and the double outfield concerted reactions of ultrasonic wave, reaction condition are：70~95 DEG C of reaction temperature,
0.5~1.5h of reaction time.The Cooperative Mode of microwave/ultrasonic wave is 1:2 or 2:1, i.e., while microwave field continuous action, surpass
Sound wave is interval 1s after interval 2s or pulse 2s after pulse 1s, and as the period, cycle operation is until reaction terminates.Described is super
The frequency of sound wave is 25~40kHz.Microwave power is 500~700W.
Specifically, the thermal decomposition is to carry out 2~3h of thermal decomposition at 700~900 DEG C of temperature.
Specifically, rare earth in the nanometer rare earth oxide ball include lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium,
Any one element in holmium, erbium, thulium, ytterbium, lutetium.
Advantageous effect：(1) product regular appearance prepared by the method for the present invention, dispersion degree is high, has both nanometer and spherical rare earth
The superiority of oxide powder material.
(2) compared with general homogeneous precipitation method, the method for the present invention, reaction speed is fast, without the hydro-thermal method of supercharging；Nothing
The coating materials such as any activating agent, dispersant and template need to be added, you can obtain high purity rare earth oxides, avoid table
Face dressing agent impacts product purity.
(3) present invention process flow is simple, can directly utilize the rare earth chlorine of the extraction and separation of existing Rare Earth Separation enterprise
It is that raw material prepares spherical nano rareearth oxidate powder body material to change liquid, is easy to industrialization promotion application.
Description of the drawings
Fig. 1 is the techniqueflow chart of the present invention.
Fig. 2 is lanthana product transmission electron microscope (TEM) figure of embodiment 1.
Fig. 3 is dysprosia product transmission electron microscope (TEM) figure of embodiment 2.
Fig. 4 is erbium oxide product transmission electron microscope (TEM) figure of embodiment 3.
Specific implementation mode：
The present invention is further illustrated with reference to the accompanying drawings and examples.
Rare earth chloride stoste in the embodiment of the present invention is all obtained with south jiangxi ion type rareearth ore through full extraction and separation
Strip liquor diluted with pure water；The microwave of use cooperates with the model XH- of Liquid-phase reactor with the double outfields of ultrasonic wave
300A, ultrasonic frequency 25KHz.
It is involved in the present invention to product average grain diameter be to scheme in conjunction with its SEM or TEM, pass through Image Tool softwares and calculate
Obtained from.
Embodiment 1.
Microwave cooperates with auxiliary homogeneous precipitation method to prepare lanthana nanosphere with the double outfields of ultrasonic wave, by following steps：
(1) 0.05molL is taken-1Lanthanum chloride stoste and 2.5molL-1Each 200mL of urea liquid is sufficiently mixed uniformly,
Obtain mixed liquor；
(2) mixed liquor is put into microwave with the double outfields of ultrasonic wave in the reaction chamber of microwave synergistic extraction instrument, instills ammonia
The pH that water adjusts mixed liquor is 6.5, and control microwave/ultrasonic synergistic pattern is 2:1, ultrasonic power 900W, microwave power
650W, reaction time 0.9h, 90 DEG C of reaction temperature；
(3) reaction solution is centrifuged to the end of reaction and is that 70 DEG C of deionized water washs 3 times and obtains filter cake with temperature；Again
It is placed in 120 DEG C of drying box dry 3h, obtains lanthana presoma；
(4) then presoma is thermally decomposed in programmable high temperature furnace, controls 700 DEG C of decomposition temperature, soaking time
2h is cooled to room temperature, and obtains lanthana nanosphere.
The TEM for obtaining lanthana nanosphere schemes as shown in Fig. 2, it is about 30nm to measure its average grain diameter.
Embodiment 2.
Microwave cooperates with auxiliary homogeneous precipitation method to prepare dysprosia nanosphere with the double outfields of ultrasonic wave, by following steps：
(1) 0.075molL is taken-1Dysprosium chloride stoste and 3molL-1Each 200mL of urea liquid is mixed evenly,
Obtain mixed liquor；
(2) mixed liquor is put into microwave and the reaction chamber of the double outfields of ultrasonic wave and microwave synergistic extraction instrument, uncomfortable pH,
It is 1 to control microwave/ultrasonic synergistic pattern:2, ultrasonic power 900W, microwave power 600W, reaction time 0.75h, reaction temperature
90 DEG C of degree；
(3) reaction solution is centrifuged and washs 3 times with deionized water at a temperature of 90 °C to the end of reaction and obtain filter cake；Again
It is placed in 100 DEG C of drying box dry 4h, obtains dysprosia presoma；
(4) then presoma is thermally decomposed in programmable high temperature furnace, controls 850 DEG C of decomposition temperature, soaking time
1.5h is cooled to room temperature, and obtains dysprosia nanosphere.
The TEM for obtaining dysprosia nanosphere schemes as shown in Fig. 2, it is about 85nm to measure its average grain diameter.
Embodiment 3.
Microwave cooperates with auxiliary homogeneous precipitation method to prepare erbium oxide nanosphere with the double outfields of ultrasonic wave, by following steps：
(1) 0.05molL is taken-1Erbium chloride stoste and 2molL-1Each 200mL of urea liquid is mixed evenly, and obtains
To mixed liquor；
(2) mixed liquor is put into microwave with the double outfields of ultrasonic wave in the reaction chamber of microwave synergistic extraction instrument, instills ammonia
The pH that water adjusts mixed liquor is 6, and control microwave/ultrasonic synergistic pattern is 1:2, ultrasonic power 900W, microwave power
600W, reaction time 0.75h, 90 DEG C of reaction temperature；
(3) reaction solution is centrifuged and washs 3 times with deionized water at a temperature of 90 °C to the end of reaction and obtain filter cake；Again
It is placed in 120 DEG C of drying box dry 3h, obtains erbium oxide presoma；
(4) then presoma is thermally decomposed in programmable high temperature furnace, controls 850 DEG C of decomposition temperature, soaking time
1.5h is cooled to room temperature, and obtains erbium oxide nanosphere.
The TEM for obtaining erbium oxide nanosphere schemes as shown in figure 4, it is about 65nm to measure its average grain diameter.
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 (8)
1. the method that microwave cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave, it is characterised in that with dense
Degree is 0.02~0.1molL-1Rare-earth chlorination solution be stoste, using urea as precipitating reagent, stoste and precipitating reagent are stirred equal
It is even, obtain mixed liquor；By above-mentioned mixed liquor, microwave and the double outfield concerted reactions of ultrasonic wave are carried out, sediment is obtained；Again will
Gained sediment carries out heat filtering, washing, drying successively；Then it is thermally decomposed, obtains target product.
2. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that the mol ratio of the precipitating reagent urea and ammonium hydroxide is 1:0~3:10-8, and urea and rare-earth chlorination
The mol ratio of solution is 20~100.
3. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that the double outfield concerted reactions of the microwave and ultrasonic wave, reaction condition are：70~95 DEG C of reaction temperature,
0.5~1.5h of reaction time.
4. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that the Cooperative Mode of microwave/ultrasonic wave is 1:2 or 2:1, i.e., while microwave field continuous action, ultrasound
Wave is interval 1s after interval 2s or pulse 2s after pulse 1s, and as the period, cycle operation is until reaction terminates.
5. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that the frequency of the ultrasonic wave is 25~40kHz.
6. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that the microwave power is 500~700W.
7. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that the thermal decomposition is to carry out 2~3h of thermal decomposition at 700~900 DEG C of temperature.
8. microwave according to claim 1 cooperates with auxiliary liquid phase synthesis nanometer rare earth oxide ball with the double outfields of ultrasonic wave
Method, it is characterised in that rare earth in the nanometer rare earth oxide ball include lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium,
Any one element in holmium, erbium, thulium, ytterbium, lutetium.
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| CN111056564A (en) * | 2019-12-27 | 2020-04-24 | 广西科学院 | A kind of microwave preparation method of lanthanum cerium terbium oxide fluorescent powder |
| CN113105889A (en) * | 2021-03-26 | 2021-07-13 | 华南理工大学 | Method for preparing europium and dysprosium co-doped strontium aluminate fluorescent powder with assistance of ultrasonic waves |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
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| CN111056564A (en) * | 2019-12-27 | 2020-04-24 | 广西科学院 | A kind of microwave preparation method of lanthanum cerium terbium oxide fluorescent powder |
| CN111056564B (en) * | 2019-12-27 | 2022-05-13 | 广西科学院 | A kind of microwave preparation method of lanthanum cerium terbium oxide fluorescent powder |
| CN113105889A (en) * | 2021-03-26 | 2021-07-13 | 华南理工大学 | Method for preparing europium and dysprosium co-doped strontium aluminate fluorescent powder with assistance of ultrasonic waves |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
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| CN115286379B (en) * | 2022-08-03 | 2023-02-10 | 景德镇陶瓷大学 | Method for preparing barium titanate-based ceramic powder by external field-promoted polycondensation non-aqueous precipitation process |
| WO2025081529A1 (en) * | 2023-10-18 | 2025-04-24 | 信丰县包钢新利稀土有限责任公司 | Device and method for preparing nano rare earth oxide by means of cooperation of ultrasonic waves and microwaves |
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