CN106745334B - A kind of method that ultrasonic wave added prepares nickel cerium solid solution material - Google Patents
A kind of method that ultrasonic wave added prepares nickel cerium solid solution material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000006104 solid solution Substances 0.000 title claims abstract description 32
- WITQLILIVJASEQ-UHFFFAOYSA-N cerium nickel Chemical compound [Ni].[Ce] WITQLILIVJASEQ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- 150000007524 organic acids Chemical group 0.000 claims abstract description 5
- 229920000620 organic polymer Chemical group 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 229910052684 Cerium Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 8
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical group O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 abstract description 12
- 239000001301 oxygen Substances 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 10
- 238000003860 storage Methods 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000002468 redox effect Effects 0.000 abstract description 3
- 239000011343 solid material Substances 0.000 abstract description 2
- 239000004449 solid propellant Substances 0.000 abstract description 2
- 150000000703 Cerium Chemical group 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 150000002815 nickel Chemical class 0.000 abstract 1
- 238000001338 self-assembly Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000009841 combustion method Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000000593 microemulsion method Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 150000003462 sulfoxides Chemical class 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- ZGMCLEXFYGHRTK-UHFFFAOYSA-N [Fe].[Ce] Chemical compound [Fe].[Ce] ZGMCLEXFYGHRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to solid material preparation technical field, method that specially a kind of ultrasonic wave added prepares nickel cerium solid solution material.The present invention utilizes the processing mode of solvent heat, nickel salts and metal cerium salt, organic acid and organic polymer structure directing agent are sufficiently interacted using under ultrasonic wave added, and acted on by self assembly, form the flower-shaped or spherical nickel cerium solid solution for having crystal phase uniform.The lower nickel content of nickel cerium solid solution materials'use prepared by the present invention, have the characteristics that specific surface area is high, metal nickle atom dispersion degree is high, crystal grain scale is small and crystal phase is uniform, there is excellent redox property and storage put oxygen performance simultaneously, oxygen storage capacity reaches 400-600 μm of ol O/g, has a good application prospect in fields such as environmental catalysis, solid fuel cell, sensors.
Description
Technical field
The invention belongs to solid material preparation technical fields, and in particular to a method of prepare nickel cerium solid solution material.
Background technique
Cerium oxide as a kind of typical rare earth oxide, existed simultaneously in fluorite crystals structure+trivalent and+4 valence ceriums from
Son makes it have excellent redox property and storage put oxygen performance, therefore the cerium based composite metal based on cerium oxide
Material is widely used in environmental catalysis and energy catalytic field, if automotive exhaust catalysis aoxidizes, volatile organic matter (VOCs)
Catalysis oxidation, steam reforming etc..Wherein, cerium based solid solution material metal ion mixing formed into cerium oxide lattice because
It is received significant attention with higher Lacking oxygen content, faster ion mobility and higher catalytic reaction activity.
The study found that the performance of cerium based solid solution material is mainly by grain size, crystal phase composition and doped metal ion
The factors such as type influence.Currently, the method for preparing cerium based solid solution material mainly has: coprecipitation, colloidal sol-gel method, chemistry
Combustion method, microemulsion method and hydrothermal crystallization method etc..Coprecipitation is easy to operate and be widely used in industrial life because of simple process
In production, but the cerium based solid solution material grains of its preparation are larger, and crystalline phase distribution is uneven, causes catalytic activity lower.Utilize change
Learning the solid solution crystal grain that the methods of combustion method, microemulsion method are prepared can achieve several nanosizeds, specific surface area and sky
Cave relative amount increased significantly, and have preferable catalytic performance.For example, Li Can (Li Can, Appl. Catal. A:Gen.,
2003,246,1) nano nickel cerium solid solution material is prepared for using combustion method of citric acid, and it was found that when nickel cerium ratio is 3: 7
When, catalyst has optimal redox property.Laguna etc. (Laguna, Appl. Catal. B:Environ.,
2011,106,621) it is prepared for Nanoscale Iron cerium solid solution material using microemulsion method, iron content may be up to 50at.%, and refer to
When iron content is 10at.%, the oxygen vacancy concentration of catalyst reaches highest while having highest redox efficiency out.
The preparation of nanometer cerium base solid-solution material largely improves the performance of cerium oxide base catalyst, but on
Stating several method, to be easy to appear crystalline phase distribution during the preparation process uneven, causes doping efficiency lower, while influencing catalyst
Overall performance.Therefore, a kind of method for preparing the uniform nanometer cerium base solid-solution material of crystal phase is developed to advanced optimizing cerium
Base catalyst material performance has very important significance.
Summary of the invention
In order to overcome the problems of prior art, the present invention provides a kind of high-performance nickel cerium solid solution that crystal phase is uniform
Preparation method, the preparation method of high-performance nickel cerium solid solution provided by the invention, for the first time using organic polymer as structure
Directed agents and ultrasonic assisted technique prepare nickel cerium solid solution material using high temperature ageing process；Wherein, by adjusting metal salt
Ratio, the temperature of solution, the time of ultrasonic treatment, the type of template and hydro-thermal process temperature and time, make to be prepared
Nickel cerium solid solution material nanoparticle accumulate composition, in flower-shaped or spherical etc., pattern is uniform and structure is uniform, and has big ratio
The features such as surface area and high storage oxygen amount, oxygen storage capacity reaches 400-600 μm of ol O/g, in environmental catalysis, solid fuel cell, biography
The fields such as sensor have a good application prospect.
The method that ultrasonic wave added provided by the invention prepares nickel cerium solid solution material, specific steps are as follows:
(1) Inorganic Cerium source and inorganic nickel source are dissolved in by a certain percentage in organic solvent dimethyl sulfoxide, and are added certain
Organic acid is measured, is stirred to uniformly mixed；Wherein, cerium nickel molar ratio is 99:1-4:1, and preferential cerium nickel molar ratio is 50:1-4:1；
(2) a certain amount of organic polymer is added as structure directing agent, and is ultrasonically treated, and keeps solution mixing equal
It is even, a certain amount of weak aqua ammonia is added later, and be sufficiently stirred；
(3) acquired solution in step (2) is transferred in water heating kettle and carries out high-temperature process, be filtered, washed, do later
Dry, roasting, pickling processes, obtain nickel cerium solid solution material.
In step (1), the Inorganic Cerium source is cerium nitrate hexahydrate (Ce (NO3)3·6H2) or seven water cerous chlorates O
(CeCl3·7H2O)；Inorganic nickel source used is six water nickel nitrate (Ni (NO3)2·6H2) or six water nickel chloride (NiCl O2·
6H2O)；The organic acid is formic acid or glycolic.
In step (2), the macromolecular structure directed agents are that (molecular weight is 10000-to polyvinylpyrrolidone
Or cetyl ammonium bromide 800000)；The ultrasonication is to be handled using 40kHz frequency ultrasonic wave solution,
The processing time is 0.5-4h, and solution temperature is 30-60 DEG C when ultrasonic.The ammonia concn is 1.5-3wt%.
In step (3), during the aging process, aging temperature is 120-180 DEG C, and ageing time is 0.5-72h；
The washing process is that obtained solid will be washed 2-3 times with distilled water and dehydrated alcohol respectively after filtering；The drying process is
Filtered solid is placed in 80 DEG C of baking ovens dry 6-8h；The roasting process be by obtained solid sample in air atmosphere
It is roasted, maturing temperature is 400-600 DEG C, and heating rate is 2-3 DEG C/min, calcining time 3-5h；The acid cleaning process
For obtained solid is placed in washing by soaking in dust technology, dust technology concentration is 5-15wt%, and soaking time is 0.5-6h, later mistake
Filter.
Advantages of the present invention:
(1) the nickel cerium solid solution crystal phase prepared by is uniform, and nickel ion doping efficiency is high, and oxygen vacancy concentration is high；
(2) the nickel cerium solid solution crystal particle scale prepared by is small, large specific surface area；
(3) the nickel cerium solid solution nickel content prepared by is lower, and metallic nickel doping efficiency is high, and raw material is cheap and easy to get, manufacture at
This is lower.
Detailed description of the invention
Fig. 1 is Scanning Electron microscope (SEM) photo of gained nickel cerium solid solution in embodiment 1 ~ 3 and comparative example 1.
Fig. 2 is the oxygen storage capacity test result of gained nickel cerium solid solution in embodiment 1 ~ 3 and comparative example 1.
Specific embodiment
The present invention will be described in further detail by example, but therefore it not limited below.
Embodiment 1
0.181g cerium chloride seven-hydrate and six water nickel chloride (molar ratio 4:1) of 0.029g are added to containing 40ml dimethyl
In the beaker of sulfoxide, and 1.0ml formic acid is added, after stirring 30min, it is in 40kHz supersonic cleaning machine, together that beaker, which is put into frequency,
When be slowly added to 1.0g polyvinylpyrrolidone (molecular weight 10000), setting ultrasonic temperature be 30 DEG C, start to be ultrasonically treated,
The processing time is 0.5h.The weak aqua ammonia that 4ml concentration is 1.5wt% is added and stirs evenly, solution is transferred to outfit polytetrafluoro later
High-temperature process is carried out in the water heating kettle of ethylene liner, treatment temperature is 120 DEG C, and the processing time is 0.5h.After high-temperature process,
Filtering solution, and washed solid 3 times with distilled water and dehydrated alcohol respectively, 6-8h is dried at 80 DEG C later, then by solid
Roasting 5h, 2 DEG C/min of heating rate are carried out under 400 DEG C of air atmospheres.Obtained solid is soaked in the dilute nitric acid solution of 5wt%
Handle 0.5h, by it is above-mentioned it is identical be filtered, washed, dry, roasting process, obtain final product nickel cerium solid solution material
(it is denoted as NiCeOn- 1), pattern is as shown in Figure 1, its oxygen storage capacity is as shown in Figure 2.
Embodiment 2
2.321g cerium nitrate hexahydrate and six water nickel nitrate (molar ratio 99:1) of 0.016g are added to containing 100ml diformazan
In the beaker of base sulfoxide, and 3.0ml glycolic is added, after stirring 30min, it is 40kHz supersonic cleaning machine that beaker, which is put into frequency,
In, while it being slowly added to 4.0g cetyl ammonium bromide, setting ultrasonic temperature is 60 DEG C, starts to be ultrasonically treated, and the processing time is
4h.The weak aqua ammonia that 8ml concentration is 3wt% is added and stirs evenly, solution is transferred to the hydro-thermal for being equipped with polytetrafluoroethyllining lining later
High-temperature process is carried out in kettle, treatment temperature is 180 DEG C, and the processing time is 72h.After high-temperature process, filtering solution, and respectively
It is washed solid 3 times with distilled water and dehydrated alcohol, 6-8h is dried at 80 DEG C later, then by solid in 600 DEG C of air atmospheres
Under carry out roasting 3h, 3 DEG C/min of heating rate.Obtained solid, which is soaked in the dilute nitric acid solution of 15wt%, handles 0.5h, is passing through
It is above-mentioned it is identical be filtered, washed, dry, roasting process, obtain final product nickel cerium solid solution material and (be denoted as NiCeOn- 2),
Pattern is as shown in Figure 1, its oxygen storage capacity is as shown in Figure 2.
Embodiment 3
0.181g cerium chloride seven-hydrate and six water nickel chloride (molar ratio 9:1) of 0.013g are added to containing 34ml dimethyl
In the beaker of sulfoxide, and 1.0ml formic acid is added, after stirring 30min, it is in 40kHz supersonic cleaning machine, together that beaker, which is put into frequency,
When be slowly added to 1.0g polyvinylpyrrolidone (molecular weight 30000), setting ultrasonic temperature be 30 DEG C, start to be ultrasonically treated, locate
The reason time is 1h.The weak aqua ammonia that 2ml concentration is 2wt% is added and stirs evenly, solution is transferred to is equipped in polytetrafluoroethylene (PTFE) later
High-temperature process is carried out in the water heating kettle of lining, treatment temperature is 160 DEG C, and the processing time is 4h.After high-temperature process, filter molten
Liquid, and washed solid 3 times with distilled water and dehydrated alcohol respectively, 6-8h is dried at 80 DEG C later, then by solid at 450 DEG C
Roasting 4h, 2 DEG C/min of heating rate are carried out under air atmosphere.Obtained solid, which is soaked in the dilute nitric acid solution of 10wt%, handles 2h,
By it is above-mentioned it is identical be filtered, washed, dry, roasting process, obtain final product nickel cerium solid solution material and (be denoted as
NiCeOn- 3), pattern is as shown in Figure 1, its oxygen storage capacity is as shown in Figure 2.
Comparative example 1
The comparative example is prepared using coprecipitation.By six water nickel chloride of 1.81g cerium chloride seven-hydrate and 0.13g, (molar ratio is
It 9:1) is added in the beaker containing 50ml distilled water, after completely dissolution, rapidly joins the ammonium hydroxide that concentration is 25wt%, adjust molten
Beaker is put into 50 DEG C of water-bath to 10 or so and continues to stir 1h, be transferred to later with polytetrafluoroethyllining lining by liquid pH value
In water heating kettle at 120 DEG C high-temperature process 4h.After high-temperature process, Temperature fall, and be filtered, washed, dried and roasted
Burning process (processing method is with embodiment 3), the nickel cerium solid solution material for obtaining coprecipitation preparation (are denoted as NiCeOn- CP).
Claims (2)
1. a kind of method that ultrasonic wave added prepares nickel cerium solid solution material, which is characterized in that specific steps are as follows:
(1) Inorganic Cerium source and inorganic nickel source are dissolved in organic solvent dimethyl sulfoxide, and organic acid is added, stirring is equal to mixing
It is even；Wherein, cerium nickel molar ratio is 99:1-4:1；
(2) organic polymer is added as structure directing agent, and is ultrasonically treated, and is uniformly mixed solution, is added later
Weak aqua ammonia, and be sufficiently stirred；
(3) acquired solution in step (2) is transferred to progress high temperature ageing processing in water heating kettle, is filtered, washed, does later
Dry, roasting, pickling and after baking processing, obtain nickel cerium solid solution material；
In step (1), the Inorganic Cerium source is cerium nitrate hexahydrate or seven water cerous chlorates；Inorganic nickel source used is six water nickel nitrates
Or six water nickel chloride；The organic acid is formic acid or glycolic；
In step (2), the macromolecular structure directed agents are the polyvinylpyrrolidone or ten that molecular weight is 10000-800000
Six alkyl bromination ammoniums；The ultrasonic treatment is to be handled using 40kHz frequency ultrasonic wave solution, and the processing time is 0.5-
4h, solution temperature is 30-60 when ultrasonicoC；The ammonia concn is 1.5-3wt%.
2. the method according to claim 1, wherein in step (3), the high temperature ageing treatment process, aging
Temperature is 120-180oC, ageing time are 0.5-72h；The washing is that obtained solid will use distilled water and nothing respectively after filtering
Water-ethanol washs 2-3 times；The drying is that filtered solid is placed in 80oDry 6-8h in C baking oven；The roasting is by institute
It obtains solid to be roasted in air atmosphere, maturing temperature is 400-600oC, heating rate 2-3oC/min, calcining time are
3-5h；The pickling is will to roast obtained solid to be placed in washing by soaking in dust technology, and dust technology concentration is 5-15wt%, when immersion
Between be 0.5-6h, filter later.
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| CN1791554A (en) * | 2003-05-21 | 2006-06-21 | 韩华石油化学株式会社 | Metal oxide solid solution, preparation and use thereof |
| CN106058241A (en) * | 2016-07-21 | 2016-10-26 | 天津巴莫科技股份有限公司 | Ce1-xZrxO2 nano solid solution homogenate modified lithium ion battery anode material and preparation method thereof |
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