CN103449496A - Nano cerium oxide and preparation method thereof - Google Patents
Nano cerium oxide and preparation method thereof Download PDFInfo
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- CN103449496A CN103449496A CN2012105915991A CN201210591599A CN103449496A CN 103449496 A CN103449496 A CN 103449496A CN 2012105915991 A CN2012105915991 A CN 2012105915991A CN 201210591599 A CN201210591599 A CN 201210591599A CN 103449496 A CN103449496 A CN 103449496A
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Abstract
The invention provides a preparation method of nano cerium oxide. The preparation method comprises the following steps: 1, dissolving Ce(NO3)3.6H2O, a surfactant and urea into deionized water, and then stirring to completely dissolve solutes, so as to obtain a colorless transparent mixed solution; 2, transferring the mixed solution to the inside of a stainless steel high-pressure reaction kettle of which a lining is polytetrafluoroethylene, putting into an oven after sealing, heating to 120-180 DEG C, and naturally cooling to room temperature to obtain a product after respectively reacting for 3-48 hours; 3, centrifuging white sediments in the product obtained in the step 2, and putting into the oven to obtain a cerium oxide precursor after washing by the deionized water and absolute ethyl alcohol respectively; 4, calcining the cerium oxide precursor in the step 3 for 8-12 hours at 500-600 DEG C, so as to obtain the nano cerium oxide. The invention also provides the nano cerium oxide prepared according to the preparation method.
Description
Technical field
The present invention relates to a kind of nano material and preparation method thereof, be specifically related to a kind of nano-cerium oxide and preparation method thereof.
Background technology
Because Ce has unique 4f layer electronic structure, cerium oxide belongs to isometric system, is face-centred cubic structure, has fluorite structure.Affiliated point group is the Fm3m point group.From the thermokinetics aspect, its (111) face is the most stable.CeO
2ce in structure cell
4+press the face-centered cubic battle array and arrange, O
2-occupy all tetrahedral sites, each Ce
4+by 8 O
2-surround, and each O
2-with 4 Ce
4+coordination, as shown in Figure 1.Cerium oxide after high temperature (T>950 ° C) reduction, CeO
2be converted into the CeO with oxygen room, non-stoichiometric
2-xoxide compound (0<x<0.5), and (T<450 ° C) CeO at low temperatures
2can form the different compound of a series of compositions.Even it should be noted that from lattice and lose a considerable amount of oxygen, after forming a large amount of oxygen room, CeO
2-xstill can keep the fluorite type crystalline structure, easily be oxidized to again CeO when this metastable oxide compound is exposed to well-oxygenated environment
2, thereby CeO
2there is superior storage and discharge oxygen function and redox reaction ability.Cerium oxide is pale yellow powder, and fusing point is 2600 ° of C, more stable at normal temperatures, vitriolization; Adding hydrogen peroxide in nitric acid also can dissolve; Effusion chlorine while being dissolved in hydrochloric acid; Be insoluble to diluted acid (except dilute sulphuric acid) and water.CeO
2thermostability higher, during 800 ° of C, can keep crystal formation constant, lose a part of Sauerstoffatom when 980 ° of C.
Application about cerium oxide in automotive exhaust catalysis.Along with increasing of automobile quantity, environmental pollution increases the weight of gradually, so many countries have carried out strict control to the discharge of vehicle exhaust, under this background, has produced three-way catalyst.Usually three-way catalyst is by the noble metal active component that plays katalysis, comprises CeO
2at interior catalyzed conversion auxiliary agent with for the carrier that supports active ingredient, form.In application aspect this catalysis, CeO
2mainly play the effect of two aspects: 1. good storage oxygen with put the oxygen function; 2. promote reactive behavior and the dispersion of precious metal.Cerium oxide belongs to isometric system, has fluorite structure, makes crystalline network arrange and does not closely easily form the oxygen room, when surrounding environment oxygen pressure changes, impels the cationic compound valency at Ce
3+with Ce
4+between mutual conversion, thereby cause Sauerstoffatom number in crystalline network to change, and then possessed storage oxygen and put the oxygen function.
Application about the cerium oxide micro Nano material in chemically machinery polished.Rare earth oxide CeO
2be a kind of polishing powder of excellent performance, be characterized in that polishing speed is high, high to the clearance of material, polished surfaceness and surface microscopic percent ripple are less, and pellet hardness is low, to polished surface damage a little less than.CeO
2polishing slurries is widely used in that glass is precise polished, super large-scale integration SiO
2medium layer polishing and monocrystalline silicon piece polishing etc.CeO
2it is all strong acid that polishing slurries is different from the active strong polishing slurries of traditional polishing, and it is both sexes under the alkaline polishing environment, simultaneously Liquidity limit and negatively charged ion
[8], therefore better polishing performance is arranged.
Application about cerium oxide nano materials in solid fuel cell.Solid Oxide Fuel Cell (SOFC) is a kind of energy conversion device that directly chemical energy is converted into efficiently to electric energy, a series of uniquenesses such as it has advantages of efficiently, environmental friendliness, applicable fuel range is wide, the life-span is long.Nano Ce O
2be applied to have the following advantages in the SOFC electrode: 1. CeO
2be a kind of hybrid conductor, there is higher electronics one Ar ion mixing conductive capability; 2. CeO
2be easy to store up oxygen, transmission oxygen, can assist O
2-from the ionogen anode, transmit; 3. CeO
2ionic conductance be greater than YSZ, anodic oxidation reactions can be expanded to TPB face (gas phase one electrode catalyst one ionogen three's interface) in addition, reduce interfacial resistance, accelerated oxidation speed of response.These characteristics have determined nano Ce O
2be expected to become a kind of novel anode of fuel cell material and be applied to the SOFC electrode, accelerate methane oxidation speed, and solve CH
4carbon-collecting problem on anode, can be used as the ionogen novel material of a kind of alternative YSZ.The application of cerium oxide nano materials aspect luminescent material.
CeO
2the strong receptivity in tool broadband, extremely strong to ultraviolet absorption, and visible ray is absorbed hardly, perviousness is good, can be used on the products such as coating, makeup, film and plastics.Research shows, nano Ce O
2uV-resistance is better than to TiO commonly used
2, be better uv-absorbing agent.In recent years, along with the development of nanotechnology, CeO
2application on luminescent material also more and more is subject to investigator's attention.
At present both at home and abroad to nano Ce O
2the preparation conceptual phase in laboratory still, prepare nano Ce O
2method is summed up and mainly contains: solid phase method, liquid phase method and vapor phase process.
Solid phase method is generally that metal oxide or its salt are fully mixed according to formula, after grinding, is calcined, and finally obtains the ultrafine particle of metal and metal oxide.It is generally acknowledged solid state reaction process experience four-stage: reactant diffusion-chemical reaction-product nucleation-crystal growth.When nucleation speed is greater than the speed of growth, be conducive to generate nanoparticle; If the speed of growth is greater than nucleation rate, form bulk crystals.The solid phase method equipment used is simple, easy to operate, but the gained powder often purity is inadequate, size-grade distribution is also larger, is applicable to require lower occasion.
Vapor phase process is divided into physical vapor method and chemical gas-phase method.Vapor phase process refers to that the method that chemical reaction generates the nano level new compound occurs in gas phase for two or more simple substance or compound.Generally speaking, the purity of vapor phase process gained powder is higher, it is less to reunite, sintering character is also better, its shortcoming be apparatus expensive, output lower, be difficult for universal.
Liquid phase method is mainly by controlling the condition of liquid-phase chemical reaction, as the method for the formation presomas such as reactant concn, temperature of reaction and time, stirring velocity, hydrolysis rate, co-precipitation in liquid-phase system.Mainly contain the precipitator method, sol-gel method, hydrothermal method, microemulsion method, electrochemical process etc.Liquid phase method is between vapor phase process and solid phase method, with vapor phase process, compare, liquid phase method have equipment simple, without the harsh physical conditions such as high vacuum, the easy advantage such as amplification, the powder prepared than solid phase method again is pure, reunion is few simultaneously, being easy to realize suitability for industrialized production, is to prepare at present the most frequently used method of nanoparticle.Liquid phase method mainly contains the precipitator method, sol-gel method, hydrothermal method, microemulsion method, electrochemical process etc.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of nano-cerium oxide and preparation method thereof.
Solving the technical scheme that technical problem of the present invention takes is: a kind of preparation method of nano-cerium oxide is provided, and described preparation method comprises the steps:
Step 1, by Ce (NO
3)
36h
2o, tensio-active agent, urea are dissolved in deionized water, then stir solute is all dissolved, and obtain water white mixing solutions;
Step 2, this mixing solutions is transferred in stainless steel autoclave that liner is tetrafluoroethylene again, after sealing, put into baking oven, be heated to 120-180 ° of C, after reacting respectively 3 ~ 48 hours, naturally cool to room temperature and obtain product;
Step 3, the white precipitate in the product obtained in step 2 is centrifugal, and, after using respectively deionized water, absolute ethanol washing, be placed in baking oven and obtain the cerium oxide precursor body;
Step 4, the cerium oxide precursor body in step 3 is calcined to 8 ~ 12 hours under 500 ~ 600 ° of C after, can obtain nano-cerium oxide.
Preferably, in step 1, described tensio-active agent is cetyl trimethylammonium bromide.
Preferably, in step 1, on magnetic stirring apparatus, stir 10 ~ 20 minutes.
Preferably, in step 3, use respectively deionized water, absolute ethanol washing 3-6 time, the temperature of baking oven is 80 ° of C, and be 12 hours time of drying.
Solving another technical scheme that technical problem of the present invention takes is: the nano-cerium oxide that provides the preparation method of the above nano-cerium oxide of a kind of basis to prepare.
Compared with prior art, the preparation method of nano-cerium oxide of the present invention has the following advantages: nano-cerium oxide high purity prepared by preparation method of the present invention and be difficult for to reunite, and preparation technology and required equipment simple, easy suitability for industrialized production nano-cerium oxide.
The accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
The existing CeO of Fig. 1
2crystalline structure.
The XRD figure of the cerium oxide precursor body that Fig. 2 is embodiment 6 spectrum (curve a) with calcining after the XRD figure spectrum (curve b) of the cerium oxide that obtains.
The SEM shape appearance figure that Fig. 3 is cerium oxide precursor body (basic carbonate cerium nanoparticle).
Fig. 4 is that embodiment 6 makes CeO
2the TEM of nanoparticle, HRTEM figure.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The invention provides a kind of preparation method of nano-cerium oxide, the method is with Ce (NO
3)
3.6h
2o is as the cerium source, and cetyl trimethylammonium bromide (CTAB) is as tensio-active agent, and under 150 ° of C, reaction synthesizes nano Ce (OH) CO in 14 hours
3, make nano cerium oxide powder after roasting.This cerium oxide powder is comprised of the nano particle of 5-6nm.
The concrete steps of the method are as follows:
Step 1, by Ce (NO
3)
36h
2o, CTAB, urea dissolves in ionized water, then is put on magnetic stirring apparatus and stirs 10 ~ 20 minutes, and solute is all dissolved, and obtains water white mixing solutions;
Step 2, again this mixing solutions is transferred in the stainless steel autoclave that the liner of 20ml is tetrafluoroethylene, after sealing, put into baking oven, be heated to 120 ~ 180 ° of C, after reacting respectively 3 ~ 48 hours, then naturally cool to room temperature and obtain product;
Step 3, the white precipitate in the product obtained in step 2 is centrifugal, and after using respectively deionized water, absolute ethanol washing 3 times, be put in and dryly in 80 ° of C baking ovens within 12 hours, obtain the CeOHCO that the cerium oxide precursor body is hexagonal system
3;
Step 4, the cerium oxide precursor body in step 3 is calcined to 8 ~ 12 hours under 500 ~ 600 ° of C after, can obtain nano-cerium oxide.
Reaction process is as follows: at first, in reaction mixture, urea decomposition produces ammonium radical ion and cyanic acid ion: H
2n-CO-NH
2→ NH
4++ OCN
-; When reaction soln is acidity, the cyanic acid ion of generation will react rapidly: OCN
-+ OH
-+ H
2o → CO
2+ NH
4 +; When reaction soln, while being neutral or alkaline, will react: OCN
-+ OH
-+ H
2o → NH
3+ CO
3 2-; Due to Ce
3+weakly alkaline and high electric charge, make it there is strong hydration.At first, Ce
3+the hydrolysis and with water molecules or OH
-complexing: Ce
3++ yH
2o → [Ce (OH) (H
2o)
n-1]
2++ H
3o
+along with the rising of temperature of reaction and the lengthening in reaction times, the hydrolysis rate of urea is accelerated.Along with the carrying out of reaction, CO
3 2-with OH
+start a large amount of the generation: [Ce (OH) (H
2o)
n-1]
2++ CO
3 2-→ CeOHCO
3(CeCO
3oH)+(n-1) H
2o; CeOHCO
3under 500 ° of C, thermolysis produces CeO
2: 4CeCO
3oH+O
2→ 4CeO
2+ 2H
2o+4CO
2.
Below specifically describe the preparation method of nano-cerium oxide of the present invention and the performance characterization of the nano-cerium oxide prepared by this preparation method etc. by different embodiment.
Embodiment 1
Step 1, by the Ce (NO of 2.3mmol
3)
36h
2o, the CTAB of 0.27mmol, the urea of 9.2mol is dissolved in the deionized water of 10ml, then is put on magnetic stirring apparatus and stirs 15 minutes, and solute is all dissolved, and obtains water white mixing solutions;
Step 2, again this mixing solutions is transferred in the stainless steel autoclave that the liner of 20ml is tetrafluoroethylene, after sealing, put into baking oven, be heated to 120-180 ° of C, after reacting respectively 3 hours, then naturally cool to room temperature and obtain product;
Step 3, the white precipitate in the product obtained in step 2 is centrifugal, and after using respectively deionized water, absolute ethanol washing 3 times, be put in and dryly in 80 ° of C baking ovens within 12 hours, obtain the CeOHCO that the cerium oxide precursor body is hexagonal system
3;
Step 4, the cerium oxide precursor body in step 3 is calcined to 8 ~ 12 hours under 500 ~ 600 ° of C after, can obtain nano-cerium oxide.
Embodiment 2
Step in the present embodiment 2 is substantially the same manner as Example 1, and only the reaction times in step 2 is 5 hours.
Embodiment 3
Step in the present embodiment 3 is substantially the same manner as Example 1, and only the reaction times in step 2 is 7 hours.
Embodiment 4
Step in the present embodiment 4 is substantially the same manner as Example 1, and only the reaction times in step 2 is 9 hours.
Embodiment 5
Step in the present embodiment 5 is substantially the same manner as Example 1, and only the reaction times in step 2 is 12 hours.
Embodiment 6
Step in the present embodiment 6 is substantially the same manner as Example 1, and difference is: the reaction times in step 2 is 24 hours, and Heating temperature is 180 ° of C; Calcining temperature in step 4 is 500 ° of C, and calcination time is 10h.
Embodiment 7
Step in the present embodiment 7 is substantially the same manner as Example 1, and only the reaction times in step 2 is 48 hours.
The nano-cerium oxide that embodiment 6 is finally obtained passes through XRD analysis, can find out, the cerium oxide precursor body, after calcining, changes the CeO2 of cubic-crystal into, as shown in Figure 2 fully.The SEM shape appearance figure that Fig. 3 is cerium oxide precursor body (basic carbonate cerium nanoparticle), as can be seen from Figure 3 reunion has occurred in basic carbonate cerium nanoparticle, and the size of coacervate is the 1.5-2.5 micron.Fig. 4 is TEM, the HRTEM figure that embodiment 6 makes the CeO2 nanoparticle, and as can be seen from Figure 4, this cerium oxide powder is comprised of the nano particle of 5-6nm.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. the preparation method of a nano-cerium oxide, is characterized in that, described preparation method comprises the steps:
Step 1, by Ce (NO
3)
36h
2o, tensio-active agent, urea are dissolved in deionized water, then stir solute is all dissolved, and obtain water white mixing solutions;
Step 2, this mixing solutions is transferred in stainless steel autoclave that liner is tetrafluoroethylene again, after sealing, put into baking oven, be heated to 120-180 ° of C, after reacting respectively 3 ~ 48 hours, naturally cool to room temperature and obtain product;
Step 3, the white precipitate in the product obtained in step 2 is centrifugal, and, after using respectively deionized water, absolute ethanol washing, be placed in baking oven and obtain the cerium oxide precursor body;
Step 4, the cerium oxide precursor body in step 3 is calcined to 8 ~ 12 hours under 500 ~ 600 ° of C after, can obtain nano-cerium oxide.
2. preparation method according to claim 1, is characterized in that, in step 1, described tensio-active agent is cetyl trimethylammonium bromide.
3. preparation method according to claim 1, is characterized in that, in step 1, on magnetic stirring apparatus, stirs 10 ~ 20 minutes.
4. preparation method according to claim 1, is characterized in that, in step 3, uses respectively deionized water, absolute ethanol washing 3-6 time, and the temperature of baking oven is 80 ° of C, and be 12 hours time of drying.
5. the nano-cerium oxide prepared according to the described preparation method of claim 1-4 any one.
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