CN105037407A - Preparation method for micro-nano cerium oxalate sheet aggregate - Google Patents
Preparation method for micro-nano cerium oxalate sheet aggregate Download PDFInfo
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- CN105037407A CN105037407A CN201510407102.XA CN201510407102A CN105037407A CN 105037407 A CN105037407 A CN 105037407A CN 201510407102 A CN201510407102 A CN 201510407102A CN 105037407 A CN105037407 A CN 105037407A
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- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229960001759 cerium oxalate Drugs 0.000 title abstract 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 17
- 239000013543 active substance Substances 0.000 claims description 14
- CQGVSILDZJUINE-UHFFFAOYSA-N cerium;hydrate Chemical compound O.[Ce] CQGVSILDZJUINE-UHFFFAOYSA-N 0.000 claims description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 14
- 239000011541 reaction mixture Substances 0.000 claims description 14
- 230000005291 magnetic effect Effects 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001149 thermolysis Methods 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound 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 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 239000002086 nanomaterial Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 241000124033 Salix Species 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000004001 molecular interaction Effects 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000019552 anatomical structure morphogenesis Effects 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method for micro-nano cerium oxalate sheet aggregate. The preparation method comprises: under the room temperature condition, stirring cerium nitrate hexahydrate, oxalic acid and a surfactant in certain volume of deionized water or a water-alcohol mixed solution in certain proportion for certain time; filtering recants, and washing and drying white solids, thereby obtaining micro-nano cerium oxalate sheet aggregate; and carrying out thermal decomposition reaction on the micro-nano cerium oxalate sheet aggregate in an air atmosphere, thereby obtaining micro-nano cerium dioxide sheet aggregate with feature similar with that of the cerium oxalate sheet aggregate. According to the preparation method, the raw materials are easily available, the process is simple and the reaction conditions are gentle; the prepared micro-nano cerium oxalate sheet aggregate not only has a relatively large specific surface area, but also has a good function of shielding ultraviolet rays, and can emit fluorescent light; and a novel way of preparing a micro-nano cerium dioxide material is provided.
Description
Technical field
After the present invention relates to the preparation method of micro-nano Sedemesis sheet aggregate and thermolysis thereof, preparation has the application of similar pattern micro-nano cerium dioxide sheet aggregate to it.
Background technology
Metal complexes molecule, because of its high symmetry and diversified profile and abundant magnetics, electricity and Photophysical Behaviors, is subject to the close attention of chemists always.Particularly since the eighties in 20th century, the various Opto-Electronic Coordination Compounds molecule with unique spatial configuration and topology effect is synthesized by successful design, makes metal complexes be carried out comprehensively in the research of the bases such as information storage, chemical sensitisation and biosimulation and Application Areas and deepen continuously.And nano material bring the change of physical property also to make the dimensional effect of people to functional materials accelerate research step.
Micro nano structure metal complex materials organic ligand and metal ion is carried out assembling under controllable condition obtain, this kind of material integrates the advantage of organic ligand, metal complexes and micro Nano material three, spatially there is one dimension, two dimension or three-dimensional structure, pattern is unique and size is positioned at micro-nano rank in shape, they often show amazing peculiar performance, therefore become the study frontier of current coordination chemistry and nano science.
In the past few years, use different step method, the metal complexes micro Nano material of many different-shapes is obtained, as various patterns such as nanometer rod, nano wire, nanometer ball, shuttle shape, triangular shape and dendroids.But, above-mentionedly be operated in research method, general only pay close attention to the impact of external conditions change on micro-nano metal complexes pattern, size and process of growth thereof, and do not relate to the effect for the micro-nano metal complexes pattern of control of the crystalline structure of title complex itself and accumulation mode.In fact, title complex micro Nano material morphogenesis is a complex process, it is subject to the impact of the molecular interaction of title complex own and complex molecule and other molecular interactions of surrounding, both relevant with the structure of complex molecule itself, relevant with the environment of surrounding again.
For this reason, the metal complexes nano material how preparing corresponding pattern according to metal complexes crystalline structure and accumulation mode thereof is just becoming the study hotspot of vast materials chemistry worker.
Summary of the invention
The object of the invention is to: the preparation method that a kind of micro-nano Sedemesis sheet aggregate is provided, larger specific surface area is not only had with the micro-nano Sedemesis sheet aggregate that this preparation method obtains, also have and good cover ultraviolet function, and energy emitting fluorescence, raw material of the present invention is easy to get, technique is simple, and reaction conditions is gentle, and provides the new way preparing micro-nano ceria material.
Technical solution of the present invention is that this preparation method is as follows: under room temperature condition, in 30 ~ 40mL deionized water or 30 ~ 40mL water-ol mixing solutions, first add 0.25 ~ 0.30mmol six nitric hydrate cerium, then add 0.1 ~ 1.0g tensio-active agent polyvinylpyrrolidone, stir and make them dissolve completely, then add the oxalic acid of 0.75 ~ 1.0mmol, continue stirring 3 ~ 15 minutes, then filtered by reaction mixture, white solid, through washing, oven dry, obtains micro-nano Sedemesis sheet aggregate.
Wherein, the mol ratio of six nitric hydrate ceriums and oxalic acid is 1:3 ~ 1:3.5.
Wherein, alcohol is ethylene glycol or glycerol; Water in water-ol mixing solutions and the volume ratio of alcohol are V (water): V (alcohol) 1:1 ~ 1:3.
Wherein, alr mode is magnetic agitation or ultrasonic agitation.
Wherein, white solid bake out temperature is 60 ~ 80
oc.
Wherein, the micro-nano Sedemesis sheet aggregate molecular formula obtained is (C
6o
12ce
26H
2o) n × 4nH
2o, n be greater than 3 integer, the pattern of every blocks of shape basic architecture block is rectangle like, class wicker leaf shape or class toothed edge rectangle.
Wherein, the Sedemesis sheet aggregate obtained is through pyrolysis in air atmosphere, and obtain the micro-nano cerium dioxide sheet aggregate similar to Sedemesis sheet aggregate pattern, its thermolysis condition is: temperature 500
oCheat 5 hours.
The reason that the present invention can obtain the different-shape micro-nano Sedemesis sheet aggregate taking flap as basic architecture block mainly comes from following factors:
1, the crystalline structure of Sedemesis title complex own is with structure cell
acinner plane sheet structure edge, face
baxle constantly grows and obtains, and this structure of matter itself determines the present invention and can obtain taking flap as the different-shape micro-nano Sedemesis sheet aggregate of basic architecture block;
2, in deionized water or water-ol mixing solutions, interaction between water molecules and water molecules hinder the random growth of Sedemesis complex molecule to any direction from the intermolecular interaction of different alcoholic solvent, make the every blocks of shape building block pattern of micro-nano Sedemesis sheet aggregate be rectangle like, class wicker leaf shape or class toothed edge rectangle;
3, the micro-nano Sedemesis sheet aggregate pattern that the cavitation that ultrasonic stirring produces also makes the pattern of micro-nano Sedemesis sheet aggregate and simple magnetic agitation obtain changes.
Advantage of the present invention is:
1, Sedemesis is a kind of ligand polymer of rare-earth element cerium, and its synthesis material is easy to get, and synthesis condition is gentle, and control easily, X-ray single crystal diffraction measurement result shows, and Sedemesis crystalline structure shows as adjacent Ce
3+first ion is interconnected to form one-dimensional chain by oxalate; Then, at structure cell
acin face, the Ce in contiguous chain
3+ion forms two dimensional surface sheet structure by oxalic acid molecule with the mode bridging of face-to-face chelating again; Finally, different two dimensional surface sheet structure again along
baxle constantly grows into three-dimensional space configuration; This structure Sedemesis not only has larger specific surface area, has good uv-absorbing function, and can emitting fluorescence.
2, planar sheet packed structures Sedemesis is utilized, carried out thermolysis, the micro-nano cerium dioxide sheet aggregate of what further preparation and micro-nano Sedemesis sheet aggregate had similar pattern with flap is basic architecture block, provides the new way preparing micro-nano ceria material.
Accompanying drawing explanation
Fig. 1 is the experiment XRD(ExperimentalXRD of embodiment 1 gained micro-nano Sedemesis sheet aggregate) and the simulation XRD(SimulationXRD that obtains according to Sedemesis crystalline structure).
Fig. 2 is the SEM of embodiment 1 gained micro-nano Sedemesis sheet aggregate.
Fig. 3 is the SEM of embodiment 2 gained micro-nano Sedemesis sheet aggregate.
Fig. 4 is the SEM of embodiment 3 gained micro-nano Sedemesis sheet aggregate.
Fig. 5 is the SEM of obtained cerium dioxide after the thermolysis of embodiment 3 gained micro-nano Sedemesis sheet aggregate.
Fig. 6 is the XRD of obtained cerium dioxide after the thermolysis of embodiment 3 gained micro-nano Sedemesis sheet aggregate
Fig. 7 is the SEM of embodiment 4 gained micro-nano Sedemesis sheet aggregate.
Fig. 8 is the SEM of embodiment 5 gained micro-nano Sedemesis sheet aggregate.
Embodiment
Be described further technical scheme of the present invention below in conjunction with drawings and the specific embodiments, these embodiments can not be interpreted as it is restriction to technical scheme.
embodiment 1:under room temperature condition, in 30mL deionized water, first add 0.25mmol six nitric hydrate cerium, then add 0.2g tensio-active agent polyvinylpyrrolidone, after magnetic agitation makes them dissolve completely, then add the oxalic acid of 0.75mmol, continue stirring 3 minutes, then filtered by reaction mixture, white solid passes through washing, and 60
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
It tests XRD(ExperimentalXRD) and the simulation XRD(SimulationXRD that obtains according to Sedemesis crystalline structure) as shown in Figure 1, SEM figure as shown in Figure 2.
As can be seen from Figure 1, the white solid of gained consists of Sedemesis; As can be seen from Figure 2, the every blocks of shape building block pattern of gained micro-nano Sedemesis sheet aggregate is rectangle like, length in micron level, about about 5um.
embodiment 2:under room temperature condition, in 10ml deionized water and 20ml glycerol mixing solutions, first add 0.25mmol six nitric hydrate cerium, then add 0.2g tensio-active agent polyvinylpyrrolidone, ultrasonic agitation makes them dissolve completely, then adds the oxalic acid of 0.75mmol, continue stirring 7 minutes, then filtered by reaction mixture, white solid passes through washing, and 60
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
Its SEM schemes as shown in Figure 3; As can be seen from Figure 3, the every blocks of shape building block pattern of gained micro-nano Sedemesis sheet aggregate is class toothed edge rectangle, and the rectangle length of side is micron level, about about 3-5um.
embodiment 3:under room temperature condition, in 10ml deionized water and 20ml ethylene glycol mixing solutions, first add 0.30mmol six nitric hydrate cerium, then add 0.2g tensio-active agent polyvinylpyrrolidone, ultrasonic agitation makes them dissolve completely, then adds the oxalic acid of 0.90mmol, continue stirring 5 minutes, then filtered by reaction mixture, white solid passes through washing, and 70
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
Its SEM schemes as shown in Figure 4; As can be seen from Figure 4, the every blocks of shape building block pattern of gained micro-nano Sedemesis sheet aggregate is class wicker leaf shape, and willow leaf is about as about 5-10um, and willow leaf center the widest part is about 2-4um.
With embodiment 3 gained micro-nano Sedemesis sheet aggregate in air atmosphere 500
oCheat 5 hours, prepare cerium dioxide; Gained cerium dioxide XRD figure as shown in Figure 5, proves that it is cerium dioxide; Gained cerium dioxide SEM as shown in Figure 6; As can be seen from Figure 6, obtained cerium dioxide is also sheet aggregate, and the every blocks of shape building block pattern of cerium dioxide aggregate is also approximately class wicker leaf shape, and it is grown and wide size is all less than corresponding micro-nano Sedemesis sheet aggregate size.
embodiment 4:under room temperature condition, in 15mL deionized water and 15ml glycerol, first add 0.25mmol six nitric hydrate cerium, then add 0.2g tensio-active agent polyvinylpyrrolidone, magnetic agitation makes them dissolve completely, then adds the oxalic acid of 0.80mmol, continue stirring 7 minutes, then filtered by reaction mixture, white solid passes through washing, and 75
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
Its SEM schemes as shown in Figure 7; As can be seen from Figure 4, the every blocks of shape building block pattern of gained micro-nano Sedemesis sheet aggregate is rectangle like, and length and width are in micron level, and length is about about 2-3um, wide about about 1um.
embodiment 5:under room temperature condition, in 20mL deionized water and 20ml glycerol, first add 0.3mmol six nitric hydrate cerium, then add 0.3g tensio-active agent polyvinylpyrrolidone, magnetic agitation makes them dissolve completely, then adds the oxalic acid of 0.90mmol, continue stirring 15 minutes, then filtered by reaction mixture, white solid passes through washing, and 75
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
Its SEM schemes as shown in Figure 8; As can be seen from Figure 8, the every blocks of shape building block pattern of gained micro-nano Sedemesis sheet aggregate is still rectangle like, but length and width are not etc., and size distribution is not exclusively even.
embodiment 6:under room temperature condition, in 40mL deionized water, first add 0.25mmol six nitric hydrate cerium, then add 1.0g tensio-active agent polyvinylpyrrolidone, ultrasonic agitation makes them dissolve completely, then adds the oxalic acid of 0.80mmol, continue stirring 15 minutes, then filtered by reaction mixture, white solid passes through washing, and 80
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
embodiment 7:under room temperature condition, in 35mL deionized water, first add 0.25mmol six nitric hydrate cerium, then add 0.3g tensio-active agent polyvinylpyrrolidone, ultrasonic agitation makes them dissolve completely, then adds the oxalic acid of 0.80mmol, continue stirring 10 minutes, then filtered by reaction mixture, white solid passes through washing, and 75
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
embodiment 8:under room temperature condition, in 10mL deionized water and 30ml glycerol, first add 0.25mmol six nitric hydrate cerium, then add 0.1g tensio-active agent polyvinylpyrrolidone, magnetic agitation makes them dissolve completely, then adds the oxalic acid of 0.875mmol, continue stirring 15 minutes, then filtered by reaction mixture, white solid passes through washing, and 70
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
embodiment 9:under room temperature condition, in 20mL deionized water and 20ml ethylene glycol, first add 0.285mmol six nitric hydrate cerium, then add 0.1g tensio-active agent polyvinylpyrrolidone, ultrasonic agitation makes them dissolve completely, then adds the oxalic acid of 1.0mmol, continue stirring 7 minutes, then filtered by reaction mixture, white solid passes through washing, and 65
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
embodiment 10:under room temperature condition, in 10mL deionized water and 30ml ethylene glycol, first add 0.25mmol six nitric hydrate cerium, then add 0.2g tensio-active agent polyvinylpyrrolidone, magnetic agitation makes them dissolve completely, then adds the oxalic acid of 0.75mmol, continue stirring 7 minutes, then filtered by reaction mixture, white solid passes through washing, and 60
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
embodiment 11:under room temperature condition, in 15mL deionized water and 20ml ethylene glycol, first add 0.26mmol six nitric hydrate cerium, then add 0.3g tensio-active agent polyvinylpyrrolidone, ultrasonic agitation makes them dissolve completely, then adds the oxalic acid of 0.91mmol, continue stirring 10 minutes, then filtered by reaction mixture, white solid passes through washing, and 65
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
embodiment 12:under room temperature condition, in 15mL deionized water and 20ml glycerol, first add 0.285mmol six nitric hydrate cerium, then add 0.2g tensio-active agent polyvinylpyrrolidone, magnetic agitation makes them dissolve completely, then adds the oxalic acid of 1.0mmol, continue stirring 10 minutes, then filtered by reaction mixture, white solid passes through washing, and 70
oc is dried, and obtains micro-nano Sedemesis sheet aggregate.
Claims (7)
1. the preparation method of micro-nano Sedemesis sheet aggregate, it is characterized in that this preparation method is: under room temperature condition, in 30 ~ 40mL deionized water or 30 ~ 40mL water-ol mixing solutions, first add 0.25 ~ 0.30mmol six nitric hydrate cerium, then 0.1 ~ 1.0g tensio-active agent polyvinylpyrrolidone is added, stirring makes them dissolve completely, add the oxalic acid of 0.75 ~ 1.0mmol again, continue stirring 3 ~ 15 minutes, then reaction mixture is filtered, white solid, through washing, oven dry, obtains micro-nano Sedemesis sheet aggregate.
2. the preparation method of micro-nano Sedemesis sheet aggregate according to claim 1, is characterized in that: the mol ratio of six nitric hydrate ceriums and oxalic acid is 1:3 ~ 1:3.5.
3. the preparation method of micro-nano Sedemesis sheet aggregate according to claim 1, is characterized in that: alcohol is ethylene glycol or glycerol; Water in water-ol mixing solutions and the volume ratio of alcohol are V (water): V (alcohol) 1:1 ~ 1:3.
4. the preparation method of micro-nano Sedemesis sheet aggregate according to claim 1, is characterized in that: alr mode is magnetic agitation or ultrasonic agitation.
5. the preparation method of micro-nano Sedemesis sheet aggregate according to claim 1, is characterized in that: white solid bake out temperature is 60 ~ 80
oc.
6. the preparation method of micro-nano Sedemesis sheet aggregate according to claim 1, is characterized in that: the micro-nano Sedemesis sheet aggregate molecular formula obtained is (C
6o
12ce
26H
2o) n × 4nH
2o, n be greater than 3 integer, the pattern of every blocks of shape basic architecture block is rectangle like, class wicker leaf shape or class toothed edge rectangle.
7. the preparation method of micro-nano Sedemesis sheet aggregate according to claim 1, it is characterized in that: the Sedemesis sheet aggregate obtained in air atmosphere through pyrolysis, obtain the micro-nano cerium dioxide sheet aggregate similar to Sedemesis sheet aggregate pattern, its thermolysis condition is: temperature 500
oc heats 5 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117510888A (en) * | 2024-01-04 | 2024-02-06 | 中国科学院合肥物质科学研究院 | Adsorption-assisted coagulation defluorination polymeric material and preparation method and application thereof |
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 |
| CN102502839A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing flaky bismuth molybdate nano material with uniform thickness |
-
2015
- 2015-07-13 CN CN201510407102.XA patent/CN105037407A/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 |
| CN102502839A (en) * | 2011-11-07 | 2012-06-20 | 河北联合大学 | Method for preparing flaky bismuth molybdate nano material with uniform thickness |
Non-Patent Citations (2)
| Title |
|---|
| LIU W. ET AL: ""A facile hydrothermal synthesis of 3D flowerlike CeO2 via a cerium oxalate precursor"", 《J. MATER. CHEM. A》 * |
| ZHANG G J. ET AL: ""Synthesis and Characterization of Mesoporous Ceria with Hierarchical Nanoarchitecture Controlled by Amino Acids"", 《J. PHYS. CHEM. B》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117510888A (en) * | 2024-01-04 | 2024-02-06 | 中国科学院合肥物质科学研究院 | Adsorption-assisted coagulation defluorination polymeric material and preparation method and application thereof |
| CN117510888B (en) * | 2024-01-04 | 2024-04-02 | 中国科学院合肥物质科学研究院 | Adsorption-assisted coagulation defluorination polymeric material and preparation method and application thereof |
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