CN109817973A - A kind of ultra-thin two-dimension amorphous non-noble metal oxide material and its preparation method and application - Google Patents
A kind of ultra-thin two-dimension amorphous non-noble metal oxide material and its preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of ultra-thin two-dimension amorphous non-noble metal oxide material, the following steps are included: the solid powder of inorganic salts and base metal organic compound is uniformly mixed, calcining obtains ultra-thin amorphous non-noble metal oxide nanometer sheet after deionized water washing.The present invention is using base metal organic compound as presoma, inorganic salts are template, only a series of amorphous non-noble metal oxide nanometer sheet of ultra-thin two-dimensions need to can be made by the method calcined after mixing, preparation method is simple and is widely portable to a variety of non-noble metal j elements, it is easy to operate, yield is higher, cheap, is to synthesize the general method of ultra-thin two-dimension amorphous non-noble metal oxide material.Wherein, the oxide-based nanomaterial of amorphous iron is applied to the negative electrode material of sodium-ion battery, shows excellent cyclical stability and high rate performance, facilitates the development for promoting sodium-ion battery.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of ultra-thin two-dimension amorphous non-noble metal oxide materials
And its preparation method and application.
Background technique
With social development, fossil energy is substituted using renewable energy and efficiently storage clean energy resource has become people
The significant challenge that is faced of the energy problem of research at present.In order to solve these problems, people are dedicated to development with chargeable electricity
The energy-storage system that Chi Wei is represented.Relative to lithium ion battery, due to sodium element rich reserves and cheap advantage, sodium from
Sub- battery has better development prospect.In recent years, the specific capacity of iron oxide Yin Qigao is as electrode material gradually by people
Concern, when the polyelectron redox reaction of oxidation state makes it as sodium ion battery electrode material have 600-
1000mAhg-1Specific capacity, be much higher than graphite.But this kind of material can be by very big volume during charge and discharge cycles
Expansion is so as to cause electrode material structural damage and the rapid decay of cycle performance.Iron oxide is thus improved as sodium ion
The cyclical stability of cell negative electrode material is the emphasis studied at present.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that providing a kind of ultra-thin two-dimension amorphous non-noble metal oxide
Material and its preparation method and application is widely portable to a variety of non-noble metal j elements, easy to operate.
The present invention provides a kind of preparation methods of ultra-thin two-dimension amorphous non-noble metal oxide material, including following step
It is rapid:
The solid powder of inorganic salts and base metal organic compound is uniformly mixed, is calcined, after deionized water washing, is obtained
To ultra-thin amorphous non-noble metal oxide nanometer sheet.
The present invention is organic with base metal to limit metal oxide along the growth in selected direction using inorganic salts as template
Compound is as presoma, using the stability of amorphous substance at a certain temperature, by base metal organic compound forerunner
Body is changed into amorphous material, while using inorganic salts as template, ultra-thin amorphous non-noble metal oxide nanometer is prepared
Sheet material.
Wherein, the inorganic salts are preferably NaNO3Or KBr.
The base metal organic compound is preferably the acetylacetonate of base metal ion.The base metal ion
Preferably one of Fe, Co, Ni, Cu, In, Zn and Mn or a variety of.
The i.e. described base metal organic compound is preferably Fe (C5H7O2)3、Co(C5H7O2)3、Ni(C5H7O2)2、Cu
(C5H7O2)2、In(C5H7O2)3、Zn(C5H7O2)2、Mn(C5H7O2)2One of or it is a variety of.
The mass ratio of the inorganic salts and base metal organic compound is preferably (1.5~20): 1.
Preferably, the preparation method specifically includes the following steps:
A it) disperses the solid powder of inorganic salts and base metal organic compound in ethanol solution, obtains mixing molten
Liquid;
B the mixed solution drying for) obtaining step A) is handled, and obtains consolidating for inorganic salts and base metal organic compound
Body mixed-powder;
C) the solid mixed-powder milled processed for obtaining step B) after deionized water washing, is surpassed then through calcining
Thin amorphous non-noble metal oxide nanometer sheet.
Specific flow diagram is in detail as shown in Figure 1.
The solid powder of inorganic salts and base metal organic compound is uniformly mixed first.
Specifically, dispersing the solid powder of inorganic salts and base metal organic compound in ethanol solution, mixed
Close solution;
Then by the processing of obtained mixed solution drying, the solid for obtaining inorganic salts and base metal organic compound is mixed
Close powder.
The temperature of the drying is preferably 60~90 DEG C.
Then obtained solid mixed-powder is calcined.
It is currently preferred, before being calcined, the solid mixed-powder is ground.The grinding when
Between preferably 5~10min.
The present invention is to the method for the calcining and is not particularly limited, and can be calcining side well known to those skilled in the art
Method.
In some embodiments of the invention, the solid powder after grinding is placed in porcelain boat, porcelain boat is put into pipe
Formula furnace, is calcined.
The temperature of the calcining is preferably 200~300 DEG C;Time is preferably 1~3h.
In the present invention, the calcining carries out preferably in atmosphere of inert gases.The inert gas can be N2Or Ar etc.
The inert gas of this field routine.
It after calcining and material natural cooling being cooled to room temperature, adopts and is washed with deionized, remove inorganic salts template, obtain
Ultra-thin amorphous non-noble metal oxide nanometer sheet.
The present invention is to the number of washing and is not particularly limited, preferably 2~3 times.
The present invention also provides a kind of ultra-thin amorphous non-noble metal oxide nanometer sheets, are prepared into according to method made above
It arrives.
Preferably, the ultra-thin amorphous non-noble metal oxide nanometer sheet with a thickness of 6~14nm, width is 0.5~2 μ
m。
The present invention also provides a kind of sodium-ion battery, negative electrode material is that the ultra-thin amorphous of above-mentioned preparation method preparation is non-expensive
Metal oxide nano-sheet or above-mentioned ultra-thin amorphous non-noble metal oxide nanometer sheet;Wherein, the base metal is Fe.
Above-mentioned sodium-ion battery further includes as metallic sodium, diaphragm and the organic electrolyte to electrode.
The present invention is to above-mentioned diaphragm and organic electrolyte and is not particularly limited, can for it is well known to those skilled in the art every
Film and organic electrolyte.
For the present invention using base metal organic compound as presoma, inorganic salts are template, limit the direction of growth of organic salt,
Only a series of amorphous non-noble metal oxide nanometer sheet of ultra-thin two-dimensions need to can be made by the method calcined after mixing,
Preparation method is simple and is widely portable to a variety of non-noble metal j elements, and easy to operate, yield is higher, cheap,
It is to synthesize the general method of ultra-thin two-dimension amorphous non-noble metal oxide material.
Wherein, the oxide-based nanomaterial of amorphous iron is applied to the negative electrode material of sodium-ion battery, shows excellent
Cyclical stability and high rate performance.The material is in 0.1Ag-1Current density under reach about 500mAhg-1Specific capacity, and
It there remains 260mAhg after 100 charge and discharge cycles-1Specific capacity.Therefore, ultra-thin amorphous iron prepared by the present invention
Oxide-based nanomaterial be suitable for sodium-ion battery negative electrode material, this kind of non-noble metal nano material price is cheap, stablize
Property is good, can promote the development of sodium-ion battery.Therefore, performance of the above-mentioned synthetic method for oxide in sodium-ion battery
Improvement has very big application advantage and development prospect.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of ultra-thin two-dimension amorphous non-noble metal oxide material of the present invention;
Fig. 2 is the oxide nano-slice, super of the oxide nano-slice of ultra-thin amorphous Fe prepared by the present invention, ultra-thin amorphous Ni
The transmission electron microscope of the oxide nano-slice of thin amorphous In, the bimetallic oxidate nano sheet material of ultra-thin amorphous FeNi
(TEM) figure;
Fig. 3 is X-ray diffraction (XRD) map of the oxide nano-slice of ultra-thin amorphous Fe prepared by the present invention;
Fig. 4 is atomic force microscope (AFM) figure and its thickness of the oxide nano-slice of ultra-thin amorphous Fe prepared by the present invention
Degree characterization;
When the oxide nano-slice for the ultra-thin amorphous Fe that Fig. 5 is prepared for embodiment 1 is as anode material of lithium-ion battery
Cycle performance curve graph.
Specific embodiment
In order to further illustrate the present invention, below with reference to embodiment to ultra-thin two-dimension amorphous base metal provided by the invention
Oxide material and its preparation method and application is described in detail.
Embodiment 1
1, the preparation of the oxide nano-slice of ultra-thin amorphous Fe
(1) 8mg Fe (C is weighed5H7O2)3It is scattered in ethanol solution with 24mg KBr, ultrasonic treatment is until form uniform
Stable mixed solution;
(2) obtained mixed solution is poured into open-top receptacle, and be transferred in 70 DEG C of baking oven, after solvent volatilization completely
It takes out, obtains metallo-organic compound Fe (C5H7O2)3With the solid mixed-powder of inorganic salts KBr.
(3) obtained solid mixed-powder is taken out, grinds 5min-10min in the agate mortar, is transferred in porcelain boat,
Porcelain boat is put into tube furnace sealing again and is passed through inert gas, 200-300 DEG C is warming up under an inert atmosphere, calcines 1-3h, then
Natural cooling cools to room temperature.
(4) obtained powder is collected, washs the 2-3 oxidate nano to get institute's prepared material amorphous iron with deionized water
Piece.
The structure of the oxide nano-slice of the ultra-thin amorphous iron of preparation, pattern are analyzed, as a result such as Fig. 2~Fig. 4 institute
Show.
Fig. 2 is transmission electron microscope (TEM) figure of the oxide nano-slice of ultra-thin amorphous iron prepared by embodiment 1.
Fig. 3 is X-ray diffraction (XRD) map of the oxide nano-slice of ultra-thin amorphous Fe prepared by embodiment 1.
Fig. 4 is atomic force microscope (AFM) figure and its thickness of the oxide nano-slice of ultra-thin amorphous Fe prepared by embodiment 1
Degree characterization.
It can be seen that the oxide nano-slice Product yields of made amorphous Fe and purity are higher by Fig. 2~Fig. 4, be really amorphous
State, Sample Width are about 1 μm, and thickness is about 11.3nm, meets description of the present invention.
2, the cathode of oxide nano-slice of the preparation containing ultra-thin amorphous Fe
The oxide nano-slice of the amorphous iron of above-mentioned preparation and Super P, binder sodium carboxymethylcellulose are pressed into quality
Mixed than 7:2:1, and solvent deionized water be added, by slurrying, smear, drying and etc. after obtain the oxidation containing amorphous iron
The cathode of object nanometer sheet.
3, sodium-ion battery is assembled
The oxide nano-slice cathode containing ultra-thin amorphous iron and metallic sodium of above-mentioned preparation are assembled into sodium-ion battery, electricity
It solves liquid and selects carbonic ester electrolyte (1M NaClO4PC solution).
4, sodium-ion battery is tested
0.1Ag is carried out in carbonic ester electrolyte to above-mentioned sodium-ion battery using battery test system-1Current density
Under constant current charge-discharge circulation.The cycle performance curve graph of battery is as shown in Figure 5.
From the point of view of cycle performance of battery figure, the material is in 0.1Ag-1Current density under have good cyclical stability.
Embodiment 2
(raw material are Co (C for the preparation of the oxide nano-slice of ultra-thin amorphous Co5H7O2)3、NaNO3, remaining step is the same as implementation
Example 1), Co (C5H7O2)3、NaNO3Dosage is respectively 8mg, 17mg.
Embodiment 3
(raw material are Ni (C for the preparation of the oxide nano-slice of ultra-thin amorphous Ni5H7O2)2、NaNO3, remaining step is the same as implementation
Example 1), Ni (C5H7O2)2、NaNO3Dosage is respectively 5mg, 17mg.
Electron microscope analysis is scanned to the oxide nano-slice pattern of the ultra-thin amorphous Ni of preparation, as a result as shown in Figure 2.
Embodiment 4
(raw material are Cu (C for the preparation of the oxide nano-slice of ultra-thin amorphous Cu5H7O2)2、NaNO3, remaining step is the same as implementation
Example 1), Cu (C5H7O2)2、NaNO3Dosage is respectively 5mg, 17mg.
Embodiment 5
(raw material are In (C for the preparation of the oxide nano-slice of ultra-thin amorphous In5H7O2)2、NaNO3, remaining step is the same as implementation
Example 1), In (C5H7O2)2、NaNO3Dosage is respectively 15mg, 250mg.
Electron microscope analysis is scanned to the oxide nano-slice pattern of the ultra-thin amorphous In of preparation, as a result as shown in Figure 2.
Embodiment 6
(raw material are Fe (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous FeCo5H7O2)3、Co(C5H7O2)3、
NaNO3, remaining step is with embodiment 1), Fe (C5H7O2)3、Co(C5H7O2)3、NaNO3Dosage is respectively 4mg, 4mg, 17mg.
Embodiment 7
(raw material are Fe (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous FeNi5H7O2)3、Ni(C5H7O2)2、
KBr, remaining step is with embodiment 1), Fe (C5H7O2)3、Ni(C5H7O2)2, KBr dosage be respectively 4mg, 3.3mg, 24mg.
Electron microscope analysis is scanned to the oxide nano-slice pattern of the ultra-thin amorphous FeNi of preparation, as a result as shown in Figure 2.
Embodiment 8
(raw material are Fe (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous FeCu5H7O2)3、Cu(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Fe (C5H7O2)3、Cu(C5H7O2)2、NaNO3Dosage is respectively 4mg, 4mg, 17mg.
Embodiment 9
(raw material are Fe (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous FeIn5H7O2)3、In(C5H7O2)3、
NaNO3, remaining step is with embodiment 1), Fe (C5H7O2)3、In(C5H7O2)3、NaNO3Dosage is respectively 6mg, 2mg, 17mg.
Embodiment 10
(raw material are Fe (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous FeZn5H7O2)3、Zn(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Fe (C5H7O2)3、Zn(C5H7O2)2、NaNO3Dosage is respectively 8mg, 2mg, 17mg.
Embodiment 11
(raw material are Fe (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous FeMn5H7O2)3、Mn(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Fe (C5H7O2)3、Mn(C5H7O2)2、NaNO3Dosage is respectively 6mg, 2mg, 17mg.
Embodiment 12
(raw material are Co (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous CoNi5H7O2)3、Ni(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Co (C5H7O2)3、Ni(C5H7O2)2、NaNO3Dosage is respectively 4mg, 4mg, 17mg.
Embodiment 13
(raw material are Co (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous CoCu5H7O2)3、Cu(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Co (C5H7O2)3、Cu(C5H7O2)2、NaNO3Dosage is respectively 4mg, 4mg, 17mg.
Embodiment 14
(raw material are Co (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous CoMn5H7O2)3、Mn(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Co (C5H7O2)3、Mn(C5H7O2)2、NaNO3Dosage is respectively 6mg, 2mg, 17mg.
Embodiment 15
(raw material are Ni (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous NiCu5H7O2)2、Cu(C5H7O2)2、
NaNO3, remaining step is with embodiment 1), Ni (C5H7O2)2、Cu(C5H7O2)2、NaNO3Dosage is respectively 6mg, 2mg, 17mg.
Embodiment 16
(raw material are Cu (C for the preparation of the ultra-thin bimetallic oxide nano-slice of amorphous CuIn5H7O2)2、In(C5H7O2)3、
NaNO3, remaining step is with embodiment 1), Cu (C5H7O2)2、In(C5H7O2)3、NaNO3Dosage is respectively 4mg, 4mg, 150mg.
Embodiment 17
(raw material are Fe (C for the preparation of the oxide nano-slice of ultra-thin tri- metal of amorphous FeCoNi5H7O2)3、Co
(C5H7O2)3、Ni(C5H7O2)2、NaNO3, remaining step is with embodiment 1), Fe (C5H7O2)3、Co(C5H7O2)3、Ni(C5H7O2)2、
NaNO3Dosage is respectively 4mg, 1mg, 1mg, 17mg.
Embodiment 18
(raw material are Co (C for the preparation of the oxide nano-slice of ultra-thin tri- metal of amorphous CoNiCu5H7O2)3、Ni
(C5H7O2)2、Cu(C5H7O2)2、NaNO3, remaining step is with embodiment 1), Co (C5H7O2)3、Ni(C5H7O2)2、Cu(C5H7O2)2、
NaNO3Dosage is respectively 2mg, 2mg, 2mg, 17mg.
As can be seen from the above embodiments, the present invention uses simple method, and ultra-thin two-dimension amorphous base metal has been prepared
Oxide material.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
Claims (9)
1. a kind of preparation method of ultra-thin two-dimension amorphous non-noble metal oxide material, which comprises the following steps:
The solid powder of inorganic salts and base metal organic compound is uniformly mixed, is calcined, after deionized water washing, is surpassed
Thin amorphous non-noble metal oxide nanometer sheet.
2. preparation method according to claim 1, which is characterized in that the inorganic salts are NaNO3Or KBr;Your non-gold
Belong to the acetylacetonate that organic compound is base metal ion;The base metal ion be Fe, Co, Ni, Cu, In, Zn and
One of Mn or a variety of.
3. preparation method according to claim 1, which is characterized in that the inorganic salts and base metal organic compound
Mass ratio is (1.5~20): 1.
4. preparation method according to claim 1, which is characterized in that the temperature of the calcining is 200~300 DEG C;Time
For 1~3h.
5. preparation method according to claim 1, which is characterized in that the calcining carries out in atmosphere of inert gases.
6. preparation method according to claim 1, which is characterized in that specifically:
A it) disperses the solid powder of inorganic salts and base metal organic compound in ethanol solution, obtains mixed solution;
B) the mixed solution drying for obtaining step A) is handled, and the solid for obtaining inorganic salts and base metal organic compound is mixed
Close powder;
C) the solid mixed-powder milled processed for obtaining step B), is then calcined, and after deionized water washing, obtains ultra-thin amorphous
Non-noble metal oxide nanometer sheet.
7. a kind of ultra-thin amorphous non-noble metal oxide nanometer sheet, which is characterized in that according to described in any one of claim 1~6
Preparation method be prepared.
8. ultra-thin amorphous non-noble metal oxide nanometer sheet according to claim 7, which is characterized in that with a thickness of 6~
14nm, width are 0.5~2 μm.
9. a kind of sodium-ion battery, which is characterized in that negative electrode material is the described in any item preparation method systems of claim 1~6
Standby ultra-thin amorphous non-noble metal oxide nanometer sheet or the described in any item ultra-thin amorphous of claim or claim 7~8
Non-noble metal oxide nanometer sheet;Wherein, the base metal is Fe.
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