CN104860357B - Mono-dispersed nano sheet and/or nano-rings and preparation thereof and application - Google Patents
Mono-dispersed nano sheet and/or nano-rings and preparation thereof and application Download PDFInfo
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Abstract
The invention discloses a kind of mono-dispersed nano sheet and/or nano-rings and preparation thereof and application.The component of described mono-dispersed nano sheet and/or nano-rings is β Co (OH)2.The preparation method of described nanometer sheet is to use mixed solvent liquid-phase precipitation method, i.e.: first stoichiometrically cobalt salt, distilled water, organic solvent and alkali are added in beaker, wherein the volume ratio of distilled water and organic solvent is 3:1～9:1, the concentration of cobalt salt is 2.5mM～10mM, alkali is 6:1～24:1 with the ratio of the amount of cobalt salt material, it is stirred for 10～20min, then 70～100 DEG C of agitated back flow reaction 0.5～2h, through washing, filtering and be dried to obtain single dispersing β Co (OH) after cooling2Nanometer sheet.The present invention is simple to operate, temperature is low, less demanding to equipment, low cost, and efficiency is high, it is easy to commercial Application is promoted.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to one and prepare monodispersed β-Co (OH)2Nanometer sheet and nano-rings
Simple and easy method.
Background technology
Stratiform cobalt hydroxide is the hydrotalcite-like materials of a kind of single metal, has structure adjustable as conventional hydrotalcite material
Degeneration and the performance such as interlayer anion is commutative.The performance that stratiform cobalt hydroxide is unique so that its lithium ion battery, catalysis,
The aspects such as detection, absorption, magnetic will have broad application prospects.Two difficult problems of existence during producing cobalt hydroxide: (1)
Easily form colloid or floccule and be difficult to filter during cobalt hydroxide precipitation；(2) cobalt hydroxide cannot not react completely under the conditions of low alkalinity
Entirely, impurity content is high, is easily become the Co (OH) of brownish black by the dioxygen oxidation in air3.Patent [CN101696039B] is announced
Under the protection of antioxidant, it is prepared for spherical cobalt hydroxide with NaOH for precipitant；Patent [CN200810120911.2]
Disclose under the protection of antioxidant, NaOH solution and protective agent solution are continuously injected in turbid solution, displace cobalt alkali formula
Anion in salt, and by regulation pH value, make α-Co (OH)2Change into peach β-Co (OH)2, the hydroxide of gained
Cobalt is fine and close crystal particle.
On the other hand, circulus because of its special configuration and unique physical and chemical performance at optical, electrical, magnetic, be catalyzed, deposit
The fields such as storage and microwave absorption have broad application prospects.The performance of nano-rings relies primarily on its pattern, size and composition.For
This, and different preparation method (e.g., liquid phase chemical etching method, physical etchings technology, molten-salt growth method, template and molecular beam epitaxy
Deng) be used to synthesize nano-rings (include, TiO2, ZnO, Graphene, GaAs/AlGaAs, Co/CoO, Fe3O4/ polyphenyl second
Alkene, K2Ti6O13, Ag, Co, Au, Ni, Si, Pt, Cu, Pb etc.).Its performance and application are had by the pattern of cobalt hydroxide
Important impact.People have the most successfully synthesized cobalt hydroxide nanometer sheet, nano flower, nano wire, nanometer rods at present, receive
Mitron, and the preparation about cobalt hydroxide nano-rings is still rarely reported.Physical etchings technology needs special template and large-scale equipment,
And because of complex process, relatively costly and be restricted.The advantage that chemical synthesis has low cost, simple to operate, yield is high,
But typically it is only applicable to special material and the synthesis of specific nanometer circulus.
In the present invention, we use mixed solvent-precipitation-ageing process, by changing the volume ratio of mixed solvent, digestion time
Regulate and control the size of nano-rings.Nanometer sheet and the nano-rings of the present invention have the characteristics such as monodispersity, size adjustable, these materials
Have broad application prospects in fields such as catalysis, electrode material, biosensor, detections.
Summary of the invention
It is desirable to provide one has monodispersity and homogeneity is good, the nanometer sheet of the characteristics such as size adjustable and nano-rings；Also
There is provided that technique is simple, mild condition, environmental protection, the energy-conservation chemical liquid phase reaction preparing dispersed nano ring；The single dispersing provided
Nanometer sheet and nano-rings have broad application prospects.
The present invention solves its technical problem and uses following technical scheme:
The mono-dispersed nano sheet of present invention offer and/or nano-rings, its component is β-Co (OH)2。
Described dispersed nano sheet and/or nano-rings, it is mono-crystalline structures, and profile is hexagon, and the length of side is 0.2～4.62 μm,
Thickness is 120～260nm, and the internal diameter of ring is 0.12～1.47 μm.
The preparation method of the mono-dispersed nano sheet that the present invention provides, specifically: use mixed solvent liquid-phase precipitation method, the most first press
Cobalt salt, distilled water, organic solvent and alkali are added in beaker by stoichiometric proportion, wherein, and distilled water and the volume of organic solvent
Ratio is 3:1～9:1, and the concentration of cobalt salt is 2.5mM～10mM, and alkali and the ratio of the amount of cobalt salt material are 6:1～24:1, then stirs
Mix 10～20min, then 70～100 DEG C of agitated back flow reaction 0.5～2h, wash after cooling, filter, after through dry
Dry obtain single dispersing β-Co (OH)2Nanometer sheet.
In said method, described organic solvent is the one in ethanol, propanol, acetone, DMF.
The preparation method of the mono-dispersed nano ring that the present invention provides, is to use mixed solvent liquid-phase precipitation-aging method, the method
Step is:
A) cobalt salt, distilled water, dehydrated alcohol and alkali are stoichiometrically added in beaker, stir 10～20min；Subsequently
70～100 DEG C of agitated back flow reaction 0.5～2h, obtain solution A；The volume ratio of water and ethanol is 3:1～9:1, cobalt salt
Concentration be 2.5～10mM, alkali is 6:1～24:1 with the ratio of the amount of cobalt salt material；
B) in solution A, at room temperature drip a certain amount of distilled water, continue ageing 24～48h；Finally wash, filter, do
Described single dispersing β-Co (OH) is obtained after dry2Nano-rings；After regulation, the volume ratio of distilled water and dehydrated alcohol is 3:1～39:1；Old
Change process uses and continuously or intermittently stirs.
Described employing mixed solvent liquid-phase precipitation-aging method, it may be assumed that the nanometer sheet forming liquid-phase precipitation, utilizes Oswald ripe
Change principle and β-Co (OH)2Different solubility in different solvents, by controlling the ratio of solvent, the response time regulates
β-Co(OH)2The dissolving of nanometer sheet and crystallization behavior, thus prepare single dispersing β-Co (OH)2Nano-rings.
In said method, described cobalt salt uses cobaltous chloride, cobalt nitrate, the one in cobaltous acetate.
In said method, described alkali is hexamethylenetetramine.
Single dispersing β-Co (OH) prepared by said method that the present invention provides2Nanometer sheet and/or nano-rings, it is at catalysis, electrode
Application in material, biosensor, detection.
Due to the fact that and have employed above-mentioned technical scheme, be allowed to compared with prior art, have the following advantages that and good effect:
(1) characteristics such as the nano-rings provided and nanometer sheet have monodispersity and homogeneity is good, size adjustable.
(2) the nano-rings that prepared by this method and nanometer sheet, it is not necessary to protective agent, particularly nano-rings formation mechenism are novel, it is easy to work
Industry application.
(3) nano-rings and the size of nanometer sheet that prepared by this method are controlled, size range wider (length of side is 0.2～4.62 μm,
Thickness is 120～260nm, and the internal diameter of ring is 0.12～1.47 μm).
(4) this method is raw materials used cheap and easy to get, and reaction temperature is low, and preparation cost is low, and efficiency is high.
(5) this method preparation process is simple, reproducible.
(6) application is wide: the cobalt hydroxide nano-rings provided and nanometer sheet are in catalysis, electrode material, biosensor, detection
Have broad application prospects in field.
In a word.Formation mechenism of the present invention is unique, simple to operate, temperature is low, less demanding to equipment, low cost, and efficiency is high,
It is prone to commercial Application promote.It is high that the nanometer sheet of the present invention and nano-rings have purity, and impurity content is few, monodispersity and homogeneity
Good, the characteristic such as size adjustable.These materials have wide answering in fields such as catalysis, electrode material, biosensor, detections
Use prospect.
Accompanying drawing explanation
The XRD phase structure collection of illustrative plates of products therefrom in Fig. 1～Fig. 3 respectively embodiment 1, the pattern observed under scanning electron microscope
Figure and the SEAD collection of illustrative plates observed under transmission electron microscope.
Fig. 4～Figure 16 respectively embodiment 2～the pattern observed under scanning electron microscope of embodiment 14 products therefrom.
Figure 17～Figure 20 is respectively the XRD phase structure collection of illustrative plates of products therefrom in embodiment 15, at scanning electron microscope and transmission electron microscope
Under the shape appearance figure that observes and SEAD collection of illustrative plates.
Shape appearance figure that in Figure 21～Figure 22 respectively embodiment 16, products therefrom observes under scanning electron microscope and to variable concentrations
NO2 -The Electrochemical Detection figure of ion.
Figure 23～Figure 27 respectively embodiment 17～the shape appearance figure observed under scanning electron microscope of embodiment 21 products therefrom.
Detailed description of the invention
The present invention is a kind of mono-dispersed nano sheet and/or nano-rings and preparation thereof and application.Described nanometer sheet and nano-rings are single
β-the Co (OH) of crystal structure2, its profile is hexagon, and the length of side is 0.2～4.62 μm, and thickness is 120～260nm, ring interior
Footpath is 0.12～1.47 μm.Use mixed solvent-low temperature liquid phase sedimentation method, by changing reaction temperature (70～100 DEG C), time
(0.5～2h), concentration, water regulate and control β-Co (OH) with volume ratio and the alkali ratio of organic solvent2The size of nanometer sheet.Will
β-Co(OH)2Nanometer sheet at room temperature further ripening 24～48h can get β-Co (OH)2Nano-rings.β-Co(OH)2Receive
Rice ring uses mixed solvent-precipitation-ageing process to prepare, it may be assumed that the β-Co (OH) that will be obtained2Nanometer sheet is the oldest in room temperature liquid phase
Change processes 24～48h and can get β-Co (OH)2Nano-rings.
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but present disclosure is not
It is limited only to the following examples.
Embodiment 1
First by 0.237g cobalt chloride hexahydrate (amount of material is 0.001mol, and concentration is 5mM), 180mL distilled water, 20mL
[alkali with the ratio (being called for short alkali ratio) of the amount of cobalt salt material is for ethanol and 1.68g hexamethylenetetramine (amount of material is 0.012mol)
12:1] join in the beaker of 400mL, stir 10min, then beaker is put in oil bath pan, react 1h at 90 DEG C, with
After at room temperature cool down, the most scrubbed, filter, be dried to obtain described single dispersing β-Co (OH)2Nanometer sheet.Products therefrom is
Pink, its thing phase and the pattern observed under scanning electron microscope, structure and SEAD collection of illustrative plates are the most as Figure 1-3.
Visible, product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet.This nanometer sheet is mono-crystalline structures, and size is uniform, rib
Angle is clearly clearly demarcated, the length of side 1.51～3.27 μm.
Embodiment 2:
Identical with embodiment 1 step, but reaction temperature is 70 DEG C.Products therefrom is pink, observes under scanning electron microscope
Pattern is as shown in Figure 4, it is seen then that product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet, size is uniform, and corner is relatively
For mellow and full, the length of side 0.72～1.99 μm, thickness 0.12～0.26 μm.
Embodiment 3:
Identical with embodiment 1 step, but reaction temperature is 100 DEG C.Products therefrom is pink, observes under scanning electron microscope
Pattern as shown in Figure 5, it is seen that, product majority is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet, sharpness of border,
Corner angle are clearly demarcated, the length of side 1.0～1.92 μm.
Embodiment 4:
Identical with embodiment 1 step, but cobalt salt concentration is 2.5mM.Products therefrom is pink, observes under scanning electron microscope
Pattern as shown in Figure 6, it is seen then that product is monodispersed hexagon β-Co (OH)2Nanometer sheet, size is uniform, and corner angle are clearly demarcated,
Minor face length 0.20～0.51 μm, the long length of side 0.45～0.91 μm.
Embodiment 5:
Identical with embodiment 1 step, but the response time be 0.5h.Products therefrom is pink, observes under scanning electron microscope
Pattern is as shown in Figure 7.Visible product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet, corner is mellow and full, the size of sheet
Uniformly, the length of side 0.89～1.89 μm.
Embodiment 6:
Identical with embodiment 1 step, but the response time be 2h.Products therefrom is pink, the shape observed under scanning electron microscope
Looks are as shown in Figure 8.Product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet, corner angle are clearly demarcated, the length of side 1.06～1.85 μm.
Embodiment 7:
Identical with embodiment 1 step, but H2O/EtOH volume ratio is 3:1.Products therefrom is pink, sees under scanning electron microscope
The pattern measured is as shown in Figure 9.Visible product is monodispersed regular hexagonal β-Co (OH) of uniform size2Nanometer sheet, chi
Very little relatively big, corner angle are clearly clearly demarcated, the length of side 1.88～4.62 μm.
Embodiment 8:
Identical with embodiment 1 step, but alkali (amount of material is 0.012mol) (amount of material is 0.002mol, dense with cobalt salt
Degree is for 10mM) ratio of the amount of material is 6:1.Products therefrom is pink, the pattern observed under scanning electron microscope such as Figure 10
Shown in.Visible, product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet, corner angle are clearly demarcated, the length of side 1.03～3.57 μm,
Thickness 0.18～0.23 μm.
Embodiment 9:
Identical with embodiment 1 step, but alkali (amount of material is 0.024mol) (amount of material is 0.001mol, dense with cobalt salt
Degree is for 5mM) ratio of the amount of material is 24:1.Products therefrom is pink, the pattern observed under scanning electron microscope such as Figure 11
Shown in.Visible, product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet.Corner angle are clearly clearly demarcated, and size ratio is more uniform,
The length of side 1.33～2.30 μm.
Embodiment 10:
Identical with embodiment 1 step, but cobalt salt is cobalt nitrate (concentration is 5mM for quality 0.2910g, 0.001mol).Institute
Obtaining product is pink, and the pattern observed under scanning electron microscope is as shown in figure 12.Visible, product is monodispersed regular six limits
Shape β-Co (OH)2Nanometer sheet, corner angle are clearly demarcated, and size is uniform, the length of side 0.50～1.87 μm.
Embodiment 11:
Identical with embodiment 1 step, but cobalt salt is cobaltous acetate (concentration is 5mM for quality 0.2491g, 0.001mol).Institute
Obtaining product is Fructus Citri tangerinae pink colour, and the pattern observed under scanning electron microscope is as shown in figure 13.Visible, product is for by from same center
Multi-slice β-Co (OH) that is staggeredly stacked of hexagon spiral2Nano flower, flower is in monodisperse status and size is more uniform,
Diameter 1.50～3.0 μm of flower.
Embodiment 12:
Identical with embodiment 10 step, but organic solvent is propanol.Products therefrom is pink, observes under scanning electron microscope
Pattern is as shown in figure 14, it is seen then that product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet, corner angle are clearly demarcated, the length of side 0.89～
2.90μm。
Embodiment 13:
Identical with embodiment 10 step, but organic solvent is acetone, and products therefrom is pink, observes under scanning electron microscope
As shown in figure 15, product is monodispersed relatively regular hexagon β-Co (OH) to pattern2Nanometer sheet, corner angle are clearly clearly demarcated, the length of side
0.64～2.24 μm.
Embodiment 14:
Identical with embodiment 10 step, but organic solvent is DMF.Products therefrom is taupe, in scanning
As shown in figure 16, product is monodispersed regular hexagonal β-Co (OH) to the pattern observed under Electronic Speculum2Nanometer sheet, corner angle are mellow and full,
Size is uniform, the length of side 1.47～2.15 μm.
Embodiment 15:
Identical with embodiment 10 step, but H2O/EtOH volume ratio is 3:1, and at room temperature continuous stirring 24h.Gained produces
Thing is pink, its thing phase and the pattern observed under scanning electron microscope and transmission electron microscope, structure and SEAD collection of illustrative plates
The most as shown in figures 17 to 20.Visible, product is monodispersed regular hexagonal β-Co (OH)2Nano-rings, this nano-rings is single
Crystal structure, edge is the most coarse, the length of side 1.02～2.63 μm, aperture 0.31～1.28 μm.
Embodiment 16:
Identical with embodiment 15 step, but H2O/EtOH volume ratio is 6:1.Products therefrom is pink, under scanning electron microscope
The pattern observed is as shown in figure 21.Visible, product is monodispersed regular hexagonal β-Co (OH)2Nanometer loop, edge is relatively
For coarse, the length of side 1.13～2.42 μm, aperture 0.32～1.23 μm.This nano-rings Electrochemical Detection such as figure to nitrite anions
Shown in 22.Visible, β-Co (OH)2Nanometer loop has obvious electrocatalytic effect to nitrite anions, and this characteristic can be used
Inspection in nitrite anions.
Embodiment 17:
Identical with embodiment 10 step, but extract reaction solution 50mL, be added dropwise over 50mL distilled water so that final distilled water and
The ratio of ethanol is intermittent stirring 24h under 19:1, and room temperature.Products therefrom is pink, the pattern observed under scanning electron microscope
As shown in figure 23, product is monodispersed regular hexagonal β-Co (OH)2Nanometer sheet and the mixture of nano-rings, wherein nano-rings
Size is more uniform, and corner angle are the most smooth, the length of side 1.12～2.40 μm, aperture 0.12～0.49 μm.
Embodiment 18:
Identical with embodiment 17 step, but the distilled water added is 150mL so that and the ratio of final distilled water and ethanol is 39:1.
Products therefrom is pink, and as shown in figure 24, product is monodispersed regular hexagonal to the pattern observed under scanning electron microscope
β-Co(OH)2Nanometer loop, the size of sheet is uniform, and corner is smooth, the length of side 1.07～2.64 μm, and pore size is the most homogeneous,
About 0.24～0.62 μm.
Embodiment 19:
Identical with embodiment 18 step, but at room temperature continuous stirring 24h.Products therefrom is pink, sees under scanning electron microscope
As shown in figure 25, product is monodispersed regular hexagonal β-Co (OH) to the pattern measured2Nanometer loop, corner angle are relatively rough,
The length of side 1.07～2.89 μm, aperture 0.29～0.84 μm.
Embodiment 20:
Identical with embodiment 19 step, but H2O/EtOH volume ratio is 6:1 so that the ratio of final distilled water and ethanol is 27:1.
Products therefrom is pink, and as shown in figure 26, product is monodispersed regular hexagonal to the pattern observed under scanning electron microscope
β-Co(OH)2Nanometer loop, corner is relatively rough, the length of side 1.09～2.41 μm, aperture 0.30～1.47 μm.
Embodiment 21:
Identical with embodiment 20 step, but at room temperature continuous stirring 48h.Products therefrom is pink, sees under scanning electron microscope
As shown in figure 27, product is monodispersed hexagon β-Co (OH) to the pattern measured2Nanometer loop, edge roughness, aperture is relatively big,
About 0.42～1.28 μm.
Single dispersing β-Co (OH) prepared by above-described embodiment2Nanometer sheet and/or nano-rings, it is in catalysis, electrode material, biological biography
Application in sensor, detection.
Claims (8)
1. the preparation method of mono-dispersed nano sheet, it is characterised in that use mixed solvent liquid-phase precipitation method, specifically: first press
Cobalt salt, distilled water, organic solvent and alkali are added in beaker by stoichiometric proportion, wherein, and distilled water and the body of organic solvent
Long-pending ratio is 3:1～9:1, and the concentration of cobalt salt is 2.5mM～10mM, and alkali and the ratio of the amount of cobalt salt material are 6:1～24:1,
It is stirred for 10～20min, then 70～100 DEG C of agitated back flow reaction 0.5～2h, washs after cooling, filter,
By being dried to obtain single dispersing β-Co (OH)2Nanometer sheet.
2. preparation method as claimed in claim 1, it is characterised in that: described organic solvent be ethanol, propanol, acetone,
One in DMF.
3. preparation method as claimed in claim 1, it is characterised in that: described cobalt salt uses cobaltous chloride, cobalt nitrate, vinegar
One in acid cobalt.
4. preparation method as claimed in claim 1, it is characterised in that: described alkali is hexamethylenetetramine.
5. the preparation method of mono-dispersed nano ring, it is characterised in that use mixed solvent liquid-phase precipitation-aging method, its step
Suddenly:
A) cobalt salt, distilled water, dehydrated alcohol and alkali are stoichiometrically added in beaker, stir 10～20min；With
After 70～100 DEG C of agitated back flow reaction 0.5～2h, obtain solution A；The volume ratio of water and ethanol is 3:1～9:1,
The concentration of cobalt salt is 2.5～10mM, and alkali is 6:1～24:1 with the ratio of the amount of cobalt salt material；
B) in solution A, at room temperature drip a certain amount of distilled water, continue ageing 24～48h；Finally wash, filter,
Obtain described single dispersing β-Co (OH) after drying2Nano-rings；After regulation the volume ratio of distilled water and dehydrated alcohol be 3:1～
39:1；Ageing process uses and continuously or intermittently stirs.
6. preparation method as claimed in claim 5, it is characterised in that use mixed solvent liquid-phase precipitation-aging method, it may be assumed that
The nanometer sheet forming liquid-phase precipitation, utilizes Oswald ripening principle and β-Co (OH)2Different solubility in different solvents,
By controlling the ratio of solvent, the response time regulates β-Co (OH)2The dissolving of nanometer sheet and crystallization behavior, thus prepare list
Dispersion β-Co (OH)2Nano-rings.
7. preparation method as claimed in claim 5, it is characterised in that: described cobalt salt uses cobaltous chloride, cobalt nitrate, vinegar
One in acid cobalt.
8. preparation method as claimed in claim 5, it is characterised in that: described alkali is hexamethylenetetramine.
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| CN106920932B (en) * | 2017-03-10 | 2019-12-03 | 上海应用技术大学 | A kind of leaf of bamboo shape Co (OH)2/ graphene combination electrode material and preparation method thereof |
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