CN104591303A - Micronano level metal oxide reticulate body and preparation method thereof - Google Patents
Micronano level metal oxide reticulate body and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method for a micronano level metal oxide reticulate body. The method comprises the steps of: (1) dispersing a lamellar carbon material and a metal salt precursor in water to form a mixed slurry, with the mass ratio of the lamellar carbon material to the metal salt precursor being 1:50-20:1, and the lamellar carbon material including a plurality of stacked laminar carbon structures; (2) drying the mixed slurry to remove water, thus obtaining a mixture; and (3) heating the mixture in oxygen atmosphere to obtain a micronano level metal oxide reticulate body, which comprises a plurality of metal oxide particles that are connected to each other to form a two-dimensional network structure. And the metal oxide particles have a size ranging from 3 nanometers to 400 nanometers. The invention also provides the micronano level metal oxide reticulate body prepared by the method.
Description
Technical field
The present invention relates to a kind of metal oxide and preparation method thereof, particularly relate to a kind of micro-nano metal oxide reticulate body and preparation method thereof.
Background technology
Metal oxide is the important mineral compound of a class, has broad application prospects at electrochemical energy storage and catalysis equal energy source chemical field.By metal oxide materials nanometer, because its particle has the features such as size is little, specific surface area is large, surface energy is high, surface atom proportion is large, thus there is unique performance.But after metal oxide nano, the specific surface area of its particle is large, causes between metal oxide particle easily tightly packed, forms coacervate, thus brings disadvantageous effect to practical application.Meanwhile, because the size of metal oxide particle is minimum, this also causes difficulty for materials processing.
Summary of the invention
In view of this, necessaryly a kind of particle size is provided to be micro/nano level and the micro-nano metal oxide reticulate body and preparation method thereof of not easily tightly packed formation coacervate.
The invention provides a kind of preparation method of micro-nano metal oxide reticulate body, it comprises the following steps:
(1) sheet carbon material and metal-salt presoma are scattered in water and form mixed slurry, wherein, the mass ratio of described sheet carbon material and described metal-salt presoma is 1:50 ~ 20:1, and described sheet carbon material comprises multiple stacked stratiform carbon structure;
(2) described water is removed in described mixed slurry drying, obtain a mixture;
(3) described mixture is heated for some time under oxygen atmosphere, obtain micro-nano metal oxide reticulate body, wherein, the temperature of described heating is 400 DEG C ~ 1000 DEG C, the time of described heating is 0.5 hour ~ 12 hours, described micro-nano metal oxide reticulate body comprises multiple metal oxide particle, and described multiple metal oxide particle is interconnected and in two-dimensional network structure, the size of described metal oxide particle is 3 nanometer ~ 400 nanometers.
Wherein, the mass ratio of described sheet carbon material and described metal-salt presoma is 1:5 ~ 5:1.
Wherein, the temperature of described heating is 600 DEG C ~ 700 DEG C, and the time of described heating is 3 hours ~ 6 hours.
Wherein, described sheet carbon material be selected from expanded graphite, Graphene, functionalization graphene one or more, described functionalization graphene be selected from graphene oxide, nitrogen-doped graphene, amination Graphene one or more.
Wherein, one or more in described metal-salt presoma chosen from Fe, cobalt, nickel, manganese, zinc, aluminium, copper, chromium or plumbous corresponding acetate, oxalate, nitrate, vitriol or muriate.
The present invention also provides a kind of micro-nano metal oxide reticulate body adopting above-mentioned preparation method to obtain, it comprises multiple metal oxide particle, described multiple metal oxide particle is interconnected and in two-dimensional network structure, the size of described metal oxide particle is 3 nanometer ~ 400 nanometers.
Wherein, described two-dimensional network structure comprises multiple hole.
Wherein, the size of described metal oxide particle is 3 nanometer ~ 100 nanometers.
With existing do not adopt sheet carbon material as template method compared with, the preparation method of micro-nano metal oxide reticulate body of the present invention, by adopting sheet carbon material to be template, between stratiform carbon structure metal-salt presoma being scattered in described sheet carbon material.After heating under oxygen atmosphere, described sheet carbon material can be ablated, and the described metal-salt presoma between adjacent two stratiform carbon structures can slowly occur to decompose and generate nanosize metal oxide.Along with the rising of temperature, described nanosize metal oxide on same two dimensional surface is grown up gradually, when growing up to micro-nano size, adjacent two or more nanosize metal oxides can be assembled and be interconnected to form the two-dimensional network structure on in-plane.Namely in described micro-nano metal oxide reticulate body, metal oxide particle position is in three dimensions relatively fixing, and therefore, metal oxide particle can not tightly packed formation coacervate, and the surface of described metal oxide particle can be fully utilized.Further, between multiple metal oxide particle, there is multiple hole, therefore, be conducive to rapid mass transfer.Described micro-nano metal oxide reticulate body has broad application prospects at electrochemical energy storage, catalysis and other field.Described preparation method is simple, and cost is lower, is beneficial to industrialization.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) photo of micro-nano metal oxide reticulate body prepared by the embodiment of the present invention 1.
Fig. 2 is scanning electron microscope (SEM) photo of micro-nano metal oxide reticulate body prepared by the embodiment of the present invention 2.
Fig. 3 is the SEM photo of micro-nano metal oxide reticulate body prepared by the embodiment of the present invention 3.
Fig. 4 is the TEM photo of micro-nano metal oxide reticulate body prepared by the embodiment of the present invention 4.
Fig. 5 is the SEM photo of metal oxide particle prepared by reference examples.
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Embodiment
Below with reference to accompanying drawing, micro-nano metal oxide reticulate body provided by the invention and preparation method thereof is described further.
The invention provides a kind of preparation method of micro-nano metal oxide reticulate body, it comprises following step:
S1, is scattered in sheet carbon material and metal-salt presoma in water and forms mixed slurry, and wherein, the mass ratio of described sheet carbon material and described metal-salt presoma is 1:50 ~ 20:1, and described sheet carbon material comprises multiple stacked stratiform carbon structure;
S2, removes described water by described mixed slurry drying, obtains a mixture; And
S3, described mixture is heated for some time under oxygen atmosphere, obtain micro-nano metal oxide reticulate body, wherein, the temperature of described heating is 400 DEG C ~ 1000 DEG C, and the time of described heating is 0.5 hour ~ 12 hours, and described micro-nano metal oxide reticulate body comprises multiple metal oxide particle, described multiple metal oxide particle is interconnected and in two-dimensional network structure, the size of described metal oxide particle is 3 nanometer ~ 400 nanometers.
In step sl, by sheet carbon material and metal-salt presoma are scattered in water, described metal-salt presoma can be dissolved in described water and ionize, and is dispersed between described sheet carbon material laminate carbon structure with the form of free metal ion and negatively charged ion.That is, in described mixed slurry, described metal-salt presoma is dispersed between described sheet carbon material laminate carbon structure in liquid form.
Described sheet carbon material comprises multiple mutually stacked stratiform carbon structure.Described sheet carbon material be selected from expanded graphite, Graphene, functionalization graphene one or more, described functionalization graphene be selected from graphene oxide, nitrogen-doped graphene, amination Graphene one or more.
One or more in described metal-salt presoma chosen from Fe, cobalt, nickel, manganese, zinc, aluminium, copper, chromium or plumbous corresponding acetate, oxalate, nitrate, vitriol or muriate.
The mass ratio of described sheet carbon material and described metal-salt presoma is 1:50 ~ 20:1, during to avoid described metal-salt presoma very few, be difficult to hanker forming interconnective reticulated structure in follow-up adding, and when avoiding described metal-salt presoma too much, easily there is the phenomenon of reuniting in the metal oxide of generation.Preferably, the mass ratio of described sheet carbon material and described metal-salt presoma is 1:5 ~ 5:1, now, obtains metal oxide particle size described in micro-nano metal oxide reticulate body even, adjacent metal oxide particle is interconnected in reticulated structure, does not substantially reunite.
In step s 2, by mixed slurry is dry, described metal ion and anion binding are dispersed between described sheet carbon material laminate carbon structure with solid-state metal-salt presoma.Now, between two adjacent stratiform carbon structures, accompany metal-salt presoma described in one deck, like this and by pre-dispersed for the described metal-salt presoma inside in described sheet carbon material.
The process of described drying can realize in a vacuum drying oven.The temperature of described drying is 40 DEG C ~ 80 DEG C.The time of described drying is 2 hours ~ 5 hours.
In step s3, by being heated under oxygen atmosphere by described mixture, described sheet carbon material is oxidized gradually, and described metal-salt presoma can occur to decompose and generate metal oxide.Concrete, in the starting stage of heating, the described metal-salt presoma between adjacent two stratiform carbon structures can slowly occur to decompose and generate nanosize metal oxide, and meanwhile, described sheet carbon material also can be ablated; Along with the rising of temperature, described nanosize metal oxide on same two dimensional surface is grown up gradually, when grow up the size to micro-nano time, adjacent two or more nanosize metal oxides can be assembled and be interconnected to form the two-dimensional network structure on in-plane.Described reticulated structure comprises multiple hole.By using described sheet carbon material as template, metal-salt presoma is scattered in the inside of described sheet carbon material, after heating under oxygen atmosphere, forms described micro-nano metal oxide reticulate body.
The temperature of described heating is preferably 600 DEG C ~ 700 DEG C, and the time of described heating is preferably 3 hours ~ 6 hours, to ensure that the particle diameter of the metal oxide particle in described micro-nano metal oxide reticulate body is 3 nanometer ~ 100 nanometers.
The present invention also provides a kind of micro-nano metal oxide reticulate body adopting above-mentioned preparation method to obtain, described micro-nano metal oxide reticulate body comprises multiple metal oxide particle, described multiple metal oxide particle is interconnected and in two-dimensional network structure, the size of described metal oxide particle is 3 nanometer ~ 400 nanometers.Preferably, the size of described metal oxide particle is 3 nanometer ~ 100 nanometers.
In described micro-nano metal oxide reticulate body, on two dimensional surface, described multiple metal oxide particle is interconnected to form horizontal grid construction, and in two adjacent horizontal grid construction in vertical direction, adjacent two or more metal oxide particles are interconnected and make two adjacent horizontal grid construction positions relatively fixing.
With existing do not adopt sheet carbon material as template method compared with, the preparation method of micro-nano metal oxide reticulate body of the present invention, by adopting sheet carbon material to be template, between stratiform carbon structure metal-salt presoma being scattered in described sheet carbon material.After heating under oxygen atmosphere, described sheet carbon material can be ablated, and the described metal-salt presoma between adjacent two stratiform carbon structures can slowly occur to decompose and generate nanosize metal oxide.Along with the rising of temperature, described nanosize metal oxide on same two dimensional surface is grown up gradually, when growing up to micro-nano size, adjacent two or more nanosize metal oxides can be assembled and be interconnected to form the two-dimensional network structure on in-plane.In described micro-nano metal oxide reticulate body, metal oxide particle position is in three dimensions relatively fixing, and therefore, metal oxide particle can not tightly packed formation coacervate, and the surface of described metal oxide particle can be fully utilized.Further, between multiple metal oxide particle, there is multiple hole, therefore, be conducive to rapid mass transfer.Described micro-nano metal oxide reticulate body has broad application prospects at electrochemical energy storage, catalysis and other field.Described preparation method is simple, and cost is lower, is beneficial to industrialization.
Below, will further illustrate in conjunction with specific embodiments.
Embodiment (1)
By 200mg graphene oxide, it is even that 100mg nickelous nitrate adds deionized water and stirring, makes slurry.
By above-mentioned slurry after vacuum drying oven 50 DEG C of dryings, in retort furnace, under air atmosphere, 700 DEG C of annealing can obtain micro-nano metal oxide reticulate body for 3 hours.
Fig. 1 is the TEM photo of micro-nano metal oxide reticulate body prepared by embodiment 1.Can find out, the median size of nickel oxide particle is 5 nanometer ~ 12 nanometers.
Embodiment (2)
By 100mg graphene oxide, it is even that 500mg cobaltous acetate adds deionized water and stirring, makes slurry.
By above-mentioned slurry after vacuum drying oven 60 DEG C of dryings, in retort furnace, under air atmosphere, 600 DEG C of annealing can obtain micro-nano metal oxide reticulate body for 6 hours.
Fig. 2 is the SEM photo of micro-nano metal oxide reticulate body prepared by embodiment 2.Can find out, the median size of cobalt oxide particle is 10 nanometer ~ 20 nanometers.
Embodiment (3)
By 250mg amination functionalized graphene, it is even that 50mg manganous nitrate adds deionized water and stirring, makes slurry.
By above-mentioned slurry after vacuum drying oven 50 DEG C of dryings, in tube furnace, under oxygen atmosphere, 1000 DEG C of annealing can obtain micro-nano metal oxide reticulate body for 10 hours.
Fig. 3 is the SEM photo of micro-nano metal oxide reticulate body prepared by the present embodiment 3.Can find out, the median size of manganese oxide particle is 200 nanometer ~ 300 nanometers.
Embodiment (4)
By 200mg Graphene, it is even that 10g ferrous sulfate adds deionized water and stirring, makes slurry.
By above-mentioned slurry after vacuum drying oven 50 DEG C of dryings, in tube furnace, under oxygen atmosphere, 800 DEG C of annealing can obtain micro-nano metal oxide reticulate body for 10 hours.
Fig. 4 is the TEM photo of micro-nano metal oxide reticulate body prepared by the present embodiment 4.Can find out, the median size of ferric oxide particles is about 300 nanometers.
Embodiment (5)
By 200mg expanded graphite, it is even that 10mg nickelous chloride adds deionized water and stirring, makes slurry.
By above-mentioned slurry after vacuum drying oven 50 DEG C of dryings, in retort furnace, under air atmosphere, 850 DEG C of annealing can obtain micro-nano metal oxide reticulate body for 30 minutes.
Reference examples
By 1g nickelous nitrate in retort furnace under air atmosphere 700 DEG C annealing 3h can obtain metal oxide particle.
Fig. 5 is the SEM photo of metal oxide particle prepared by comparative example.Can find out, when not with sheet carbon material template, the nickel oxide particle prepared is random distribution at random.Adjacent nickel oxide particle is piled up and is reunited, and is not interconnected to form two-dimensional network structure.Further, the size of nickel oxide particle is also extremely uneven, and the maximum particle diameter of nickel oxide particle reaches 500 nanometers.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. a preparation method for micro-nano metal oxide reticulate body, it comprises the following steps:
(1) sheet carbon material and metal-salt presoma are scattered in water and form mixed slurry, wherein, the mass ratio of described sheet carbon material and described metal-salt presoma is 1:50 ~ 20:1, and described sheet carbon material comprises multiple stacked stratiform carbon structure;
(2) described water is removed in described mixed slurry drying, obtain a mixture;
(3) described mixture is heated for some time under oxygen atmosphere, obtain micro-nano metal oxide reticulate body, wherein, the temperature of described heating is 400 DEG C ~ 1000 DEG C, the time of described heating is 0.5 hour ~ 12 hours, described micro-nano metal oxide reticulate body comprises multiple metal oxide particle, and described multiple metal oxide particle is interconnected and in two-dimensional network structure, the size of described metal oxide particle is 3 nanometer ~ 400 nanometers.
2. the preparation method of micro-nano metal oxide reticulate body as claimed in claim 1, it is characterized in that, the mass ratio of described sheet carbon material and described metal-salt presoma is 1:5 ~ 5:1.
3. the preparation method of micro-nano metal oxide reticulate body as claimed in claim 1, it is characterized in that, the temperature of described heating is 600 DEG C ~ 700 DEG C, and the time of described heating is 3 hours ~ 6 hours.
4. the preparation method of micro-nano metal oxide reticulate body as claimed in claim 1, it is characterized in that, described sheet carbon material be selected from expanded graphite, Graphene, functionalization graphene one or more, described functionalization graphene be selected from graphene oxide, nitrogen-doped graphene, amination Graphene one or more.
5. the preparation method of micro-nano metal oxide reticulate body as claimed in claim 1, it is characterized in that, one or more in described metal-salt presoma chosen from Fe, cobalt, nickel, manganese, zinc, aluminium, copper, chromium or plumbous corresponding acetate, oxalate, nitrate, vitriol or muriate.
6. one kind adopts the micro-nano metal oxide reticulate body that preparation method obtains as described in claim 1 to 5, it is characterized in that, described micro-nano metal oxide reticulate body comprises multiple metal oxide particle, described multiple metal oxide particle is interconnected and in two-dimensional network structure, the size of described metal oxide particle is 3 nanometer ~ 400 nanometers.
7. micro-nano metal oxide reticulate body as claimed in claim 6, it is characterized in that, described two-dimensional network structure comprises multiple hole.
8. micro-nano metal oxide reticulate body as claimed in claim 7, it is characterized in that, the size of described metal oxide particle is 3 nanometer ~ 100 nanometers.
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CN108996551A (en) * | 2018-08-24 | 2018-12-14 | 合肥学院 | Cr-doped α -Fe2O3Preparation method of micro-nanocrystalline |
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CN105664952B (en) * | 2016-03-02 | 2018-06-15 | 中国科学院过程工程研究所 | Copper oxide-zinc oxide composite catalyst, preparation method and purposes |
CN108862248A (en) * | 2018-08-06 | 2018-11-23 | 南京工业大学 | Method for rapidly and massively preparing graphene-metal oxide composite powder material |
CN108996551A (en) * | 2018-08-24 | 2018-12-14 | 合肥学院 | Cr-doped α -Fe2O3Preparation method of micro-nanocrystalline |
CN108996551B (en) * | 2018-08-24 | 2021-03-23 | 合肥学院 | Cr-doped alpha-Fe2O3Preparation method of micro-nanocrystalline |
CN109231172A (en) * | 2018-09-03 | 2019-01-18 | 复旦大学 | A kind of two-dimensional metallic oxide nano-slice and preparation method thereof |
CN110479274A (en) * | 2018-11-05 | 2019-11-22 | 吉林大学 | It is a kind of by aluminium powder be sacrifice agent Co3O4-CuCoO2The preparation method of nanometer net materials |
CN110479274B (en) * | 2018-11-05 | 2021-06-22 | 吉林大学 | Co taking aluminum powder as sacrificial agent3O4-CuCoO2Preparation method of nano net material |
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