CN103449496A - Nano cerium oxide and preparation method thereof - Google Patents
Nano cerium oxide and preparation method thereof Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- cerium oxide
- preparation
- nano
- hours
- deionized water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 49
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 5
- 239000010935 stainless steel Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract 4
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims abstract 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract 2
- 239000004094 surface-active agent Substances 0.000 claims abstract 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000005498 polishing Methods 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 239000007791 liquid phase Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 230000035484 reaction time Effects 0.000 description 7
- 239000012808 vapor phase Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N anhydrous cyanic acid Natural products OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910004631 Ce(NO3)3.6H2O Inorganic materials 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
Images
Landscapes
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
本发明提供一种纳米氧化铈的制备方法，所述制备方法包括如下步骤：步骤一、将Ce(NO3)3·6H2O、表面活性剂、尿素溶于去离子水中，然后搅拌使溶质全部溶解，得到无色透明的混合溶液；步骤二、再将该混合溶液转移到内衬为聚四氟乙烯的不锈钢高压反应釜内中，密封后，放入烘箱中，将其加热至120-180°C，分别反应3~48小时后，自然冷却至室温得到产物；步骤三、将步骤二中得到的产物中的白色沉淀离心，并分别用去离子水、无水乙醇洗涤后，放在烘箱中得到氧化铈前驱体；步骤四、将步骤三中的氧化铈前驱体在500~600°C下煅烧8~12小时后，即可得到纳米氧化铈。本发明还提供一种根据以上的制备方法制备的纳米氧化铈。
The present invention provides a preparation method of nano cerium oxide. The preparation method comprises the following steps: step 1, dissolving Ce(NO 3 ) 3·6 H 2 O, surfactant and urea in deionized water, and stirring The solute is completely dissolved to obtain a colorless and transparent mixed solution; step 2, transfer the mixed solution to a stainless steel high-pressure reactor lined with polytetrafluoroethylene, seal it, put it in an oven, and heat it to 120 -180°C, after reacting for 3 to 48 hours respectively, cool naturally to room temperature to obtain the product; step 3, centrifuge the white precipitate in the product obtained in step 2, wash with deionized water and absolute ethanol respectively, and put Obtain a cerium oxide precursor in an oven; step 4, calcining the cerium oxide precursor in step 3 at 500-600° C. for 8-12 hours to obtain nano-cerium oxide. The present invention also provides a nano-cerium oxide prepared according to the above 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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105915991A CN103449496A (en) | 2012-12-31 | 2012-12-31 | Nano cerium oxide and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105915991A CN103449496A (en) | 2012-12-31 | 2012-12-31 | Nano cerium oxide and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103449496A true CN103449496A (en) | 2013-12-18 |
Family
ID=49732399
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105915991A Pending CN103449496A (en) | 2012-12-31 | 2012-12-31 | Nano cerium oxide and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103449496A (en) |
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754921A (en) * | 2013-12-21 | 2014-04-30 | 安徽大学 | Preparation method of monodisperse cerium oxide loose nanospheres |
| CN103922385A (en) * | 2014-05-08 | 2014-07-16 | 宿州学院 | Preparation method of cerium oxide hexagonal nanometer sheet structure |
| CN104386731A (en) * | 2014-11-12 | 2015-03-04 | 太原理工大学 | Preparation method of pineapple-shaped nano cerium oxide by nano-bulk self-assembly |
| CN104628025A (en) * | 2015-02-15 | 2015-05-20 | 渤海大学 | Solvothermal Preparation of CeO2 Nanorod Thin Films Vertically Assembled on Silicon Surface |
| CN105498783A (en) * | 2016-01-28 | 2016-04-20 | 郑州航空工业管理学院 | Fe3O4/CeO2 Nanocomposite Material, Preparation Method and Application |
| CN105693246A (en) * | 2016-03-11 | 2016-06-22 | 九江学院 | Preparation method of yttrium oxide transparent ceramic |
| CN105731514A (en) * | 2016-01-28 | 2016-07-06 | 郑州航空工业管理学院 | Cubic nanometer CeO2 and its application in the degradation of o-aminophenol |
| CN105800665A (en) * | 2014-12-29 | 2016-07-27 | 安集微电子科技(上海)有限公司 | Preparation method for cerium oxide crystal and application thereof in chemical mechanical polishing (CMP) |
| CN106975479A (en) * | 2017-04-18 | 2017-07-25 | 南京工业大学 | Sea urchin-shaped CeO2‑MnO2Process for producing composite oxide catalyst |
| CN107456993A (en) * | 2017-07-24 | 2017-12-12 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of water process ozone catalyst and products thereof and application |
| CN107486194A (en) * | 2017-07-24 | 2017-12-19 | 安徽华亿农牧科技发展有限公司 | A kind of preparation method of the load cerium tin oxide composite microsphere photocatalyst of aquiculture waste water processing |
| CN108557863A (en) * | 2018-05-29 | 2018-09-21 | 淮北师范大学 | A kind of preparation method of lanthana |
| CN110128141A (en) * | 2019-06-10 | 2019-08-16 | 包头市沃野对外贸易有限责任公司 | A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method |
| CN110526272A (en) * | 2019-08-28 | 2019-12-03 | 贵州大学 | A kind of micro-nano structure CeCO3The preparation process of OH |
| CN111389360A (en) * | 2020-03-30 | 2020-07-10 | 中国农业大学 | A kind of biochar-supported Ce3+-rich ceria material, preparation method and application thereof |
| CN111592030A (en) * | 2020-06-10 | 2020-08-28 | 中南大学 | Spherical cerium oxide powder with uniform appearance and controllable granularity as well as preparation method and application thereof |
| CN112209422A (en) * | 2020-10-15 | 2021-01-12 | 东北大学 | A kind of method for preparing cerium oxide nanospheres |
| CN112794357A (en) * | 2021-03-29 | 2021-05-14 | 安徽景成新材料有限公司 | Method for synthesizing nano cerium oxide by hydrothermal method |
| CN113952960A (en) * | 2021-11-01 | 2022-01-21 | 徐州工程学院 | Co-CeO for preparing low-carbon alcohol from synthetic gas2Catalyst, preparation method and application |
| CN114522731A (en) * | 2021-12-30 | 2022-05-24 | 合肥学院 | Preparation method and application of photocatalyst cerium dioxide-metal organic framework |
| CN115472445A (en) * | 2022-09-29 | 2022-12-13 | 贵州民族大学 | A kind of method that utilizes ceria to prepare supercapacitor electrode material |
| CN115872704A (en) * | 2022-12-29 | 2023-03-31 | 生物炭建材有限公司 | Self-cleaning carbon negative biochar heat-insulating plastering mortar and preparation method thereof |
| CN116741549A (en) * | 2023-08-14 | 2023-09-12 | 新乡学院 | A Ce-based composite electrode material and its preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101264922A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Preparation method of cerium oxide rhombic nanosheet material |
| CN101284952A (en) * | 2007-04-12 | 2008-10-15 | 北京有色金属研究总院 | Abrasive grain CeO2 for chemical and mechanical buffing and method for preparing same |
-
2012
- 2012-12-31 CN CN2012105915991A patent/CN103449496A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284952A (en) * | 2007-04-12 | 2008-10-15 | 北京有色金属研究总院 | Abrasive grain CeO2 for chemical and mechanical buffing and method for preparing same |
| CN101264922A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Preparation method of cerium oxide rhombic nanosheet material |
Non-Patent Citations (1)
| Title |
|---|
| 崔美云: ""氧化铈微纳米材料的水热法合成及表征"", 《中国优秀硕士学位论文全文数据库（电子期刊） 工程科技I辑》 * |
Cited By (33)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103754921A (en) * | 2013-12-21 | 2014-04-30 | 安徽大学 | Preparation method of monodisperse cerium oxide loose nanospheres |
| CN103922385A (en) * | 2014-05-08 | 2014-07-16 | 宿州学院 | Preparation method of cerium oxide hexagonal nanometer sheet structure |
| CN103922385B (en) * | 2014-05-08 | 2015-09-30 | 宿州学院 | A kind of preparation method of cerium oxide hexagonal nanosheet shape structure |
| CN104386731A (en) * | 2014-11-12 | 2015-03-04 | 太原理工大学 | Preparation method of pineapple-shaped nano cerium oxide by nano-bulk self-assembly |
| CN105800665A (en) * | 2014-12-29 | 2016-07-27 | 安集微电子科技(上海)有限公司 | Preparation method for cerium oxide crystal and application thereof in chemical mechanical polishing (CMP) |
| CN104628025A (en) * | 2015-02-15 | 2015-05-20 | 渤海大学 | Solvothermal Preparation of CeO2 Nanorod Thin Films Vertically Assembled on Silicon Surface |
| CN104628025B (en) * | 2015-02-15 | 2016-06-08 | 渤海大学 | Solvothermal Preparation of CeO2 Nanorod Thin Films Vertically Assembled on Silicon Surface |
| CN105498783A (en) * | 2016-01-28 | 2016-04-20 | 郑州航空工业管理学院 | Fe3O4/CeO2 Nanocomposite Material, Preparation Method and Application |
| CN105731514A (en) * | 2016-01-28 | 2016-07-06 | 郑州航空工业管理学院 | Cubic nanometer CeO2 and its application in the degradation of o-aminophenol |
| CN105693246A (en) * | 2016-03-11 | 2016-06-22 | 九江学院 | Preparation method of yttrium oxide transparent ceramic |
| CN106975479B (en) * | 2017-04-18 | 2019-06-04 | 南京工业大学 | Sea urchin-shaped CeO2-MnO2Process for producing composite oxide catalyst |
| CN106975479A (en) * | 2017-04-18 | 2017-07-25 | 南京工业大学 | Sea urchin-shaped CeO2‑MnO2Process for producing composite oxide catalyst |
| CN107456993B (en) * | 2017-07-24 | 2019-11-29 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of water process ozone catalyst and products thereof and application |
| CN107486194A (en) * | 2017-07-24 | 2017-12-19 | 安徽华亿农牧科技发展有限公司 | A kind of preparation method of the load cerium tin oxide composite microsphere photocatalyst of aquiculture waste water processing |
| CN107456993A (en) * | 2017-07-24 | 2017-12-12 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of water process ozone catalyst and products thereof and application |
| CN108557863B (en) * | 2018-05-29 | 2020-05-05 | 淮北师范大学 | A kind of preparation method of lanthanum oxide |
| CN108557863A (en) * | 2018-05-29 | 2018-09-21 | 淮北师范大学 | A kind of preparation method of lanthana |
| CN110128141A (en) * | 2019-06-10 | 2019-08-16 | 包头市沃野对外贸易有限责任公司 | A kind of novel 2:17 type samarium-cobalt permanent-magnetic material sintering padding preparation method |
| CN110526272B (en) * | 2019-08-28 | 2022-04-15 | 贵州大学 | Micro-nano structure CeCO3Preparation process of OH |
| CN110526272A (en) * | 2019-08-28 | 2019-12-03 | 贵州大学 | A kind of micro-nano structure CeCO3The preparation process of OH |
| CN111389360A (en) * | 2020-03-30 | 2020-07-10 | 中国农业大学 | A kind of biochar-supported Ce3+-rich ceria material, preparation method and application thereof |
| CN111389360B (en) * | 2020-03-30 | 2021-04-02 | 中国农业大学 | Bio-carbon-loaded Ce-rich material3+Cerium dioxide material, preparation method and application thereof |
| CN111592030A (en) * | 2020-06-10 | 2020-08-28 | 中南大学 | Spherical cerium oxide powder with uniform appearance and controllable granularity as well as preparation method and application thereof |
| CN112209422A (en) * | 2020-10-15 | 2021-01-12 | 东北大学 | A kind of method for preparing cerium oxide nanospheres |
| CN112794357A (en) * | 2021-03-29 | 2021-05-14 | 安徽景成新材料有限公司 | Method for synthesizing nano cerium oxide by hydrothermal method |
| CN113952960A (en) * | 2021-11-01 | 2022-01-21 | 徐州工程学院 | Co-CeO for preparing low-carbon alcohol from synthetic gas2Catalyst, preparation method and application |
| CN114522731A (en) * | 2021-12-30 | 2022-05-24 | 合肥学院 | Preparation method and application of photocatalyst cerium dioxide-metal organic framework |
| CN114522731B (en) * | 2021-12-30 | 2023-12-29 | 合肥学院 | Application of ceria-metal organic framework in photocatalytic degradation of active blue 19 |
| CN115472445A (en) * | 2022-09-29 | 2022-12-13 | 贵州民族大学 | A kind of method that utilizes ceria to prepare supercapacitor electrode material |
| CN115472445B (en) * | 2022-09-29 | 2024-03-29 | 贵州民族大学 | A method for preparing supercapacitor electrode materials using cerium dioxide |
| CN115872704A (en) * | 2022-12-29 | 2023-03-31 | 生物炭建材有限公司 | Self-cleaning carbon negative biochar heat-insulating plastering mortar and preparation method thereof |
| CN116741549A (en) * | 2023-08-14 | 2023-09-12 | 新乡学院 | A Ce-based composite electrode material and its preparation method |
| CN116741549B (en) * | 2023-08-14 | 2023-10-24 | 新乡学院 | Ce-based composite electrode material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103449496A (en) | Nano cerium oxide and preparation method thereof | |
| Sun et al. | Synthesis and adsorption properties of Li1. 6Mn1. 6O4 by a combination of redox precipitation and solid-phase reaction | |
| CN104505505B (en) | The preparation method of the ternary layered positive electrode of Lithium metasilicate coated lithium ion battery | |
| CN105591080B (en) | A kind of lithium ion battery negative material SiOX-TiO2The preparation method of/C | |
| CN102208614B (en) | Method for preparing lithium ion battery cathode material coated iron sesquioxide | |
| CN109678193B (en) | A kind of preparation method of nanometer cerium oxide particles | |
| CN107601564B (en) | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere | |
| CN101113010A (en) | Microwave Assisted Preparation of Cerium Oxide Nanoparticles | |
| CN103553140B (en) | Method for preparing lanthanum ferrite nanodisk | |
| CN109119621B (en) | Lithium lanthanum titanate-lithium titanate coated nickel cobalt lithium aluminate anode material and preparation method thereof | |
| CN104362334A (en) | Preparation method of lithium metasilicate coated lithium-enriched laminar positive electrode material of lithium ion battery | |
| CN103157461A (en) | Nanometer photocatalyst bismuth tungstate and preparation method thereof | |
| CN101186287A (en) | A kind of preparation method of apatite type oxide electrolyte powder | |
| CN106784748B (en) | A kind of silicon substrate nickel cobalt manganese lithium ternary electrode material of lithium battery and preparation method thereof | |
| CN102139914A (en) | Method for preparing calcium titanate nanoparticles | |
| CN107857300B (en) | A kind of preparation method of β type bismuth oxide | |
| CN108275721A (en) | A kind of preparation method and applications of { 010 } high energy crystal face exposure BiOCl nanometer sheet materials | |
| CN107445202B (en) | A kind of preparation method of small-sized, super-dispersed nano-zirconia-based coating powder | |
| CN105271443A (en) | Method for preparing flaky nano CoO or Co3O4 through assistant microwave heating | |
| CN109546126A (en) | A kind of transition metal element doped carbon coating lithium titanate, preparation method and application | |
| CN109273289A (en) | Preparation of nickel-based magnesium cobaltate composite material by solvent method and application thereof | |
| CN102642844A (en) | Lithium chloride molten salt method for preparing lanthanum silicate electrolyte material powder with oxidapatite structure | |
| CN110190280A (en) | A kind of preparation method of antimony phosphate of fluffy polyanion negative electrode material | |
| CN102774879B (en) | Preparation method of dual-phase coexistence one-dimensional structure tin dioxide | |
| CN106207112B (en) | Graphene/overlength TiO2(B) nanometer tube composite materials and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20131218 |