CN110385121A - A kind of microwave burning preparation method of cerium-based composite oxides - Google Patents
A kind of microwave burning preparation method of cerium-based composite oxides Download PDFInfo
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- CN110385121A CN110385121A CN201910679009.2A CN201910679009A CN110385121A CN 110385121 A CN110385121 A CN 110385121A CN 201910679009 A CN201910679009 A CN 201910679009A CN 110385121 A CN110385121 A CN 110385121A
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- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 42
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 29
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 13
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 238000002485 combustion reaction Methods 0.000 claims abstract description 9
- 235000019441 ethanol Nutrition 0.000 claims abstract description 8
- 239000002671 adjuvant Substances 0.000 claims abstract description 7
- 150000002739 metals Chemical class 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 18
- 239000012266 salt solution Substances 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 238000009938 salting Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000001939 inductive effect Effects 0.000 abstract 1
- 229910001960 metal nitrate Inorganic materials 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000010355 oscillation Effects 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000009841 combustion method Methods 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical group [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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Abstract
The present invention discloses a kind of microwave burning preparation method of cerium-based composite oxides, it is related to inorganic nonmetallic nanometer material field, comprise the following steps that (1) prepares mixed metal nitrate solution, cerous nitrate, doping metals source are mixed with solvent, doping metals source includes zinc nitrate, copper nitrate, zirconium nitrate, cobalt nitrate, nickel nitrate, and solvent is water or ethyl alcohol；(2) combustion adjuvant is added to be uniformly mixed, the optional ethylene glycol of combustion adjuvant or glycerol；(3) mixed solution heated in micro-wave oven and the inducing combustion in 2min, the honeycomb sprills of bulk multi-hole is made；(4) by honeycomb sprills in 450 DEG C~800 DEG C calcining 1h to get.Cerium-based composite oxides prepared by the present invention have porosity and looseness three-dimensional structure, the good dispersion of product.The preparation method simple process, aggregate velocity are fast, low energy consumption, is easy to industrialization.
Description
Technical field
The present invention relates to the preparation methods of cerium-based composite oxides micro-nano powder, and in particular to a kind of cerium base combined oxidation
The microwave burning preparation method of object belongs to inorganic nonmetallic nanometer material field.
Background technique
CeO2It is a kind of important rare earth oxide, storage and release oxygen ability, ionic conductivity with higher, especially
It is the porous oxidation cerium of bigger serface, because it combines the advantages of porous material density is low, porosity is high, good dispersion, tool
The characteristics of having reinforcing material surface-active and improving the absorption of material surface molecules, thus it is net to be widely used in vehicle exhaust
Change, ultraviolet shielded absorption, fuel cell, sewage catalytic degradation etc..Largely studies have shown that carrying out certain journey to cerium oxide
The modification of degree can make the property of material have greatly changed, thus the demand of further satisfaction difference research field.Transition
Metallic element is compared with noble metal, more inexpensively, is easy to get, advantage of lower cost.Therefore it prepares transient metal doped more
Hole cerium base oxide is of great significance.
Currently, the method for preparing porous cerium-based composite oxides has template, hydrothermal/solvent thermal method, solution combustion method etc.,
Due to template, hydrothermal/solvent thermal method preparation process is cumbersome, the production cycle is long, low efficiency, and is unsuitable for industrialized production.It is molten
Liquid combustion synthesis nano material has many advantages, such as that process is simple, and obtained substance is pure, but it uses Electric heating, material
Uneven heating is even, and final product is caused phenomena such as local grain roughening and crystal grain stick to each other, reunite occur.Chinese patent CN
106946282B obtains foam and produces by adding surfactant in the aqueous solution that cerous nitrate, zirconium nitrate and silicon source are configured to
Object obtained porous cerium-based composite oxides for foam product high-temperature calcination 4~6 hours.This method is low in cost, but deficiency
Being in needs long-time heating in precursor solution and calcination time is long, and energy consumption is high.
Microwave-assisted combustion method have many advantages, such as rapidly and efficiently, energy conservation and environmental protection, Chinese patent CN 108654597A discloses
A kind of method of microwave-assisted armorphous nano bimetallic catalyst of the combustion method preparation with doped structure, passes through heating water bath
Precursor solution obtains jelly, and jelly is moved into the burning of microwave stove heating, prepares while having nanostructure and metal
The bimetallic catalyst of doped structure.But the deficiency of the patent is that the solution gels time is long, production efficiency is low.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of microwave burning preparation method of cerium-based composite oxides, should
Method and process is simple, production cost is low, short preparation period, and obtained product has bigger serface and porous structure, dispersion
Effect is good.
Technical solution of the present invention is as follows:
A kind of microwave burning preparation method of cerium-based composite oxides, using cerous nitrate as cerium source, doping metals source is selected from nitre
One or both of sour zinc, copper nitrate, zirconium nitrate, cobalt nitrate, nickel nitrate, the optional ethylene glycol of combustion adjuvant or glycerol, including step
It is rapid as follows:
(1) one or both of cerous nitrate, doping metals source is taken to be dissolved in ethyl alcohol or aqueous solution；
Wherein, cerium source is cerous nitrate, and the molar ratio of doping metals source and cerous nitrate is 0.01~0.5:1, metal salt solution
Molar concentration 0.1mmol/L~1mmol/L；
Molar concentration 0.2mmol/L~0.5mmol/L of preferred metal salt solution；
(2) combustion adjuvant is added in Xiang Shangshu material system, is uniformly mixed, the molar feed ratio of the combustion adjuvant and metal salt
Are as follows: 1~10:1；
The molar feed ratio of preferred combustion adjuvant and metal salt are as follows: 2~3:1；
(3) metal salt solution that step (2) obtains is placed in the micro-wave oven that frequency is 2.45Hz, 400~1000W's
0.5min~5min is heated under firm power, is boiled, and evaporation, plastic burns, obtains honeycomb sprills；
Powder obtains porous cerium-based composite oxides through 450~800 DEG C of calcining 1h.
Beneficial effects of the present invention
1. the present invention directly carries out microwave heating to precursor solution, it is not necessarily to gel process, simple process, aggregate velocity
Fastly, production cost is low；
2. the present invention uses microwave heating, low energy consumption, and precursor solution and material are heated evenly, and powder obtained is dredged
Loose porous, good dispersion.
Detailed description of the invention
Fig. 1 is the XRD diagram of cerium-based composite oxides prepared by embodiment 1.
Fig. 2 is the SEM photograph of cerium-based composite oxides prepared by embodiment 1.
Fig. 3 is the N of cerium-based composite oxides prepared by embodiment 12Adsorption/desorption curve.
Specific embodiment
Below in conjunction with specific embodiment and in conjunction with attached drawing, the present invention is described in detail, but is not intended to limit the present invention.
Embodiment 1
Weigh 2.00g cerous nitrate, 0.15g zinc nitrate is dissolved in 15ml ethyl alcohol, add 0.9g glycerol, sonic oscillation
10min obtains clear metal salt solution；Metal salt solution is placed in the microwave that frequency is 2.45GHz in corundum crucible
In furnace, 2min is heated under 700W power, solution obtains honeycomb powder through fast boiling, evaporation, plastic and burning；By bee
Nest shape powder is placed in Muffle furnace, and in air atmosphere, 700 DEG C of calcining 1h obtain Ce after furnace cooling4+:Zn2+Molar ratio is
The cerium base oxide powder of 9:1.The X-ray diffraction spectrogram and CeO of the cerium base oxide2Characteristic peak match, according to Scherrer
It is 26.5nm that formula, which calculates its crystallite dimension,；The cerium base oxide pattern is porous three-dimensional reticular structure, according to N2Adsorption/desorption
It is 31.96m that curve, which measures its specific surface area,2/g。
Embodiment 2
It weighs 2.00g cerous nitrate and is dissolved in 8ml ethyl alcohol and obtain solution A, weigh 0.15g cobalt nitrate and be dissolved in 5ml water and obtain
Solution A, B are mixed, add 1.2g ethylene glycol, sonic oscillation 10min obtains clear metal salt solution by solution B；It will be golden
Belong to salting liquid to be placed in corundum crucible in the micro-wave oven that frequency is 2.45GHz, 2min, solution warp are heated under 600W power
Fast boiling, evaporation, plastic and burning obtain honeycomb powder；Honeycomb powder is placed in Muffle furnace, in air atmosphere
Under, 600 DEG C of calcining 1h obtain Ce after furnace cooling4+:Co4+Molar ratio is the cerium base oxide powder of 9:1.The cerium base oxide
X-ray diffraction spectrogram and CeO2Characteristic peak match, according to Scherrer formula calculate its crystallite dimension be 27.4nm；According to N2
It is 29.60m that adsorption/desorption curve, which measures its specific surface area,2/g。
Embodiment 3
Weigh 1.00g cerous nitrate, 0.06g copper nitrate is dissolved in 8ml ethyl alcohol, add 0.45g glycerol, sonic oscillation
10min obtains clear metal salt solution；Metal salt solution is placed in the microwave that frequency is 2.45GHz in corundum crucible
In furnace, 2min is heated under 600W power, solution obtains honeycomb powder through fast boiling, evaporation, plastic and burning；By bee
Nest shape powder is placed in Muffle furnace, and in air atmosphere, 700 DEG C of calcining 1h obtain Ce after furnace cooling4+:Cu2+Molar ratio is
The cerium base oxide powder of 9:1.The X-ray diffraction spectrogram and CeO of the cerium base oxide2Characteristic peak match, according to Scherrer
It is 29.2nm that formula, which calculates its crystallite dimension,；The cerium base oxide pattern is porous three-dimensional reticular structure, according to N2Adsorption/desorption
It is 28.16m that curve, which measures its specific surface area,2/g。
Embodiment 4
Weigh 1.00g cerous nitrate, 0.11g zirconium nitrate is dissolved in 8ml ethyl alcohol, add 0.50g glycerol, sonic oscillation
10min obtains clear metal salt solution；Metal salt solution is placed in the microwave that frequency is 2.45GHz in corundum crucible
In furnace, 2min is heated under 700W power, solution obtains honeycomb powder through fast boiling, evaporation, plastic and burning；By bee
Nest shape powder is placed in Muffle furnace, and in air atmosphere, 800 DEG C of calcining 1h obtain Ce after furnace cooling4+:Zr4+Molar ratio is
The cerium base oxide powder of 9:1.The X-ray diffraction spectrogram and CeO of the cerium base oxide2Characteristic peak match, according to Scherrer
It is 17.82nm that formula, which calculates its crystallite dimension,；The cerium base oxide pattern is porous three-dimensional reticular structure, according to N2Adsorption/desorption
It is 23.27m that curve, which measures its specific surface area,2/g。
Embodiment 5
Weigh 2.00g cerous nitrate, 0.15g nickel nitrate is dissolved in 15ml ethyl alcohol, add 0.60g ethylene glycol, ultrasound vibration
It swings 10min and obtains clear metal salt solution；It is the micro- of 2.45GHz that metal salt solution is placed in frequency in corundum crucible
In wave furnace, 2min is heated under 600W power, solution obtains honeycomb powder through fast boiling, evaporation, plastic and burning；
Honeycomb powder is placed in Muffle furnace, in air atmosphere, 600 DEG C of calcining 1h obtain Ce after furnace cooling4+:
Ni2+Molar ratio is the cerium base oxide powder of 9:1.The X-ray diffraction spectrogram and CeO of the cerium base oxide2Characteristic peak kissing
It closes, calculating its crystallite dimension according to Scherrer formula is 29.20nm；According to N2Adsorption/desorption curve measures its specific surface area
33.15m2/g。
It above are only five specific embodiments of the invention, but the design concept of the present invention is not limited to this, according to this
Any type of simple modification to the above embodiments of the technical spirit of invention, equivalent variations, still fall within the technology of the present invention
The protection scope of scheme.
Claims (8)
1. a kind of microwave burning preparation method of cerium-based composite oxides, which is characterized in that by cerium source, doping metals source and solvent
Mixing, is added combustion adjuvant and is uniformly mixed, metal salt solution is made, and metal salt solution is moved into micro-wave oven, microwave furnace parameters are arranged,
So that metal salt solution is completed boiling, evaporation, plastic, combustion process in 2min, honeycomb sprills, powder are obtained after burning
Cerium-based composite oxides are obtained through 450~800 DEG C of calcining 1h.
2. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that the doping
Source metal is one or both of zinc nitrate, copper nitrate, zirconium nitrate, cobalt nitrate, nickel nitrate.
3. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that the cerium source
For cerous nitrate, the molar ratio of the doping metals source and cerous nitrate is 0.01~0.5:1.
4. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that the solvent
For one or both of water and ethyl alcohol.
5. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that the metal
Molar concentration 0.1mmol/L~1mmol/L of salting liquid.
6. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that described combustion-supporting
Agent is ethylene glycol or glycerol.
7. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that described combustion-supporting
The molar feed ratio of agent and metal salt are as follows: 1~10:1.
8. the microwave burning preparation method of cerium-based composite oxides according to claim 1, which is characterized in that use microwave
Cause burning, the microwave furnace parameters are as follows: heating power is 400w~1000w, heating time is 0.5min~5min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112811457A (en) * | 2021-03-03 | 2021-05-18 | 甘肃农业大学 | Preparation method of loose porous nano cerium oxide |
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| CN112811457A (en) * | 2021-03-03 | 2021-05-18 | 甘肃农业大学 | Preparation method of loose porous nano cerium oxide |
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