CN109592721A - A kind of porous Ni (OH)2Nanocages and preparation method thereof - Google Patents
A kind of porous Ni (OH)2Nanocages and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of porous Ni (OH)2Nanocages and preparation method thereof.Include the following steps: that the first step is to obtain Ni by chemical precipitation method3[Co(CN)6]2;Second step, by Ni of the washing after dry3[Co(CN)6]2Powder ultrasonic dissolves in deionized water, and Ni is added in configured NaOH solution3[Co(CN)6]2In solution, porous Ni (OH) is obtained after ultrasonic agitation, centrifuge washing are dry2Nanocages.The preparation method raw material is cheap, and reaction condition is mildly controllable, the porous Ni (OH) of synthesis2Nanocage size is 300-400nm.Porous Ni (OH) produced by the present invention2The advantages that big open channel structure, big specific surface area and high permeability that nanocages have, has broad application prospects in catalysis, lithium ion battery and supercapacitor field.
Description
(1) technical field
Material of the invention is the function nano material as derived from organic metal framework structure, and in particular to a kind of porous Ni
(OH)2Nanocages and preparation method thereof belong to new energy materials field.
(2) background technique
Ni(OH)2Nano material be always a kind of very important energy storage conversion in transistion metal compound (including
Lithium ion battery and supercapacitor) material.For example, Ni (OH)2Because of its form low in cost, abundant and big theoretical ratio electricity
Appearance attracts wide public concern in the electrode material of fake capacitance supercapacitor.But due to Ni (OH)2Poorly conductive and limited
Reactivity site, cause empirical value far below theoretical value.With the further investigation to nano material, people increasingly recognize
Know the chemical property for being designed to material structure and pattern and nano material can be improved, such as hollow nanostructured has
The advantages such as big surface area become the object that energy catalytic field is competitively studied.Prussian blue similar object (Prussian blue
Analogues, PBAs) belong to a kind of novel porous materials, it is made of metal cation and organic ligand.Spread out by template of PBAs
Raw porous function nano material can be widely applied to catalysis, absorption, energy storage.PBAs derived material reported at present
There are transition metal hydroxide, oxide, sulfide and phosphide, the pattern of formation has hollow Nano box, nanometer frame knot
Structure and it is truncated hollow cubic nanocage of apex angle etc..The method of use has chemical etching method and annealing method etc..But it arrives
So far still without hollow Nano caged Ni (OH)2Report, and design a kind of open architecture, bigger serface and hypertonic
The Ni (OH) of saturating rate2Nano material has great importance to raising supercapacitor and battery performance.
(3) summary of the invention
The purpose of the invention is to provide a kind of porous Ni (OH)2Nanocages and preparation method thereof.The nanocages
The Ni (OH) of shape2With open channel design, catalysis and storage is can be improved in the characteristics such as big specific surface area and high permeability
Performance.The porous Ni (OH) of the present invention2The successful preparation of nanocages can provide new approach to the preparation of transistion metal compound.
To realize aforementioned invention purpose, technical solution of the present invention includes: a kind of porous Ni (OH)2The preparation side of nanocages
Method, the preparation method include the following steps:
Step 1: by K3[Co(CN)6] dissolve in deionized water, it stirs evenly and solution A is made;Again by Na3C6H5O7With
Ni(NO3)2.6H2O is successively dissolved in deionized water, stirs evenly and B solution is made, and solution A is poured into B solution, after mixing evenly
Ethyl alcohol centrifuge washing is used after standing reaction a period of time at room temperature, is dried in vacuo to obtain Ni-Co in 80 DEG C of temperature conditions
PBAs nano cubic particle.
Step 2: it takes the Ni-Co PBAs nano cubic particle ultrasound of certain mass evenly dispersed in deionized water, adds
Enter the NaOH solution of certain solubility, stirring is made into C solution.Continue that C solution certain time is stirred by ultrasonic, solution colour is by blue and white
Become light green color.With ethyl alcohol centrifuge washing 5 times, finally vacuum drying obtains jade-green Ni (OH) under the conditions of 80 DEG C2Nanometer
Particle powder.
Further, K in the step 13[Co(CN)6] concentration be 0.02mol/L, Na3C6H5O7Concentration be
0.045mol/L, Ni (NO3)2Concentration be 0.03mol/L.
Further, in the step 1, solution A quickly stirs 3-5min after mixing with B solution, stands 3-7day.
Further, in the step 2, the mass concentration of Ni-Co PBAs particle is 1-1.5mg/mL in C solution.
Further, in the step 2, the solubility of NaOH is 0.375-0.5mol/L in C solution.
Further, in the step 2, the reaction ultrasonic agitation time is 6-10hour.
A kind of porous Ni (OH)2Nanocages are the nanocages of cube structure, the surface of 6 planes of the cubic structure
Center is embedded in a similar coniform hole, and the bottom of 6 holes is mutual at the geometric center position of cubic structure
The structure of a nanocage is presented in connection;Ni(OH)2The size dimension of nanocages is 300-400nm, and the diameter of hole is with depth
Degree increases and successively decreases.
A kind of beneficial effects of the present invention: porous Ni (OH) of the present invention2Nanocages and preparation method thereof, this method raw material are honest and clean
Valence, reaction condition are mild.In addition, the porous Ni (OH)2Nanometer basket structure has open big channel design, big specific surface
The characteristics such as product, high permeability and extremely-low density are turned as absorption, catalyst, alkali metal-ion battery and super energy storage
Change ideal material.
(4) Detailed description of the invention
Fig. 1 is Ni prepared by the present invention (OH)2The material phase analysis XRD spectra of sample.
Fig. 2 is Ni prepared by the present invention (OH)2Morphology analysis (SEM and TEM) image of sample.
(5) specific embodiment
In the following with reference to the drawings and specific embodiments, the following further describes the technical solution of the present invention.
Embodiment 1:
The K that 30ml concentration is 0.02mol/L is respectively configured3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With the Ni (NO of 0.03mol/L concentration3)2B solution, solution A is poured into B solution, in room temperature after magnetic agitation 3min
Lower standing reacts 3day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.The Ni-Co PBAs nano cubic particle ultrasound of 40mg is dispersed in 20ml ionized water, 10ml solubility is added
For the NaOH solution of 0.375mol/L, after continuing ultrasonic agitation to 6hour, solution colour becomes light green color from blue and white.Use second
Alcohol centrifuge washing 5 times, finally dry our for 24 hours obtains jade-green Ni (OH) under the conditions of 80 DEG C2Powder of nanometric particles.
Fig. 1 is porous Ni (OH)2The XRD spectra of nanocages.
Fig. 2 is porous Ni (OH)2The SEM and TEM image of nanocages.
Embodiment 2:
The K that 30ml concentration is 0.02mol/L is respectively configured3[Co(CN)6] solution A, 20ml containing concentration be 0.045mol/L
The Na of concentration3C6H5O7With the Ni (NO of 0.03mol/L concentration3)2B solution, solution A is poured into B solution, magnetic agitation 3min
Afterwards, reaction 5day is stood at room temperature, then with ethyl alcohol centrifuge washing 5 times, vacuum drying obtains Ni-Co under the conditions of 80 DEG C
PBAs nano cubic particle.45mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, is added
Enter the NaOH solution that 10ml solubility is 0.4mol/L, after continuing ultrasonic agitation to 7hour, solution colour becomes light green from blue and white
Color.With ethyl alcohol centrifuge washing 5 times, finally it is dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result similar with embodiment 1.
Embodiment 3:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 3min, in room temperature
Lower standing reacts 7day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.30mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.4mol/L, after continuing ultrasonic agitation to 8hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 4:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 4min, in room temperature
Lower standing reacts 3day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.40mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.375mol/L, after continuing ultrasonic agitation to 9hour, solution colour becomes light green color from blue and white.Use ethyl alcohol
It centrifuge washing 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 5:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 4min, in room temperature
Lower standing reacts 5day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.45mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.4mol/L, after continuing ultrasonic agitation to 10hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 6:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 4min, in room temperature
Lower standing reacts 7day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.45mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.5mol/L, after continuing ultrasonic agitation to 6hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 7:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 5min, in room temperature
Lower standing reacts 3day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.40mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.375mol/L, after continuing ultrasonic agitation to 7hour, solution colour becomes light green color from blue and white.Use ethyl alcohol
It centrifuge washing 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 8:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 5min, in room temperature
Lower standing reacts 5day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.45mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.4mol/L, after continuing ultrasonic agitation to 8hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 9:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 5min, in room temperature
Lower standing reacts 7day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.40mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.5mol/L, after continuing ultrasonic agitation to 9hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 10:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 5min, in room temperature
Lower standing reacts 3day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.40mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.45mol/L, after continuing ultrasonic agitation to 9hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 11:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 5min, in room temperature
Lower standing reacts 3day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.45mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.45mol/L, after continuing ultrasonic agitation to 9hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, is finally dried to obtain under the conditions of 80 DEG C jade-green Ni (OH)2Powder of nanometric particles.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Embodiment 12:
Configure the K that 30ml concentration is 0.02mol/L3[Co(CN)6] solution A, 20ml concentration containing 0.045mol/L
Na3C6H5O7With 0.03mol/L concentration Ni (NO3)2B solution, solution A is poured into B solution, after magnetic agitation 5min, in room temperature
Lower standing reacts 5day, then with ethyl alcohol centrifuge washing 5 times, and vacuum drying obtains Ni-Co PBAs nano cubic under the conditions of 80 DEG C
Particle.45mg Ni-Co PBAs nano cubic particle ultrasound is dispersed in 20ml ionized water, 10ml solubility, which is added, is
The NaOH solution of 0.5mol/L, after continuing ultrasonic agitation to 10hour, solution colour becomes light green color from blue and white.With ethyl alcohol from
The heart washs 5 times, and 2 powder of nanometric particles of jade-green Ni (OH) is finally dried to obtain under the conditions of 80 DEG C.
It is characterized through XRD, SEM and TEM, it is as a result still similar with embodiment 1.
Therefore, a kind of porous 2 nanocages of Ni (OH) and preparation method thereof that this project is protected, the structure have open
The characteristics such as structure, big surface area and extremely-low density.Using 2 nanocages of porous Ni (OH) prepared by the present invention as super capacitor
Anode material, show the chemical property of enhancing, such as fast charging and discharging characteristic under high current.
Claims (7)
1. a kind of porous Ni (OH)2The preparation method of nanocages, it is characterised in that: the preparation method includes the following steps:
Step 1: by K3[Co(CN)6] dissolve in deionized water, it stirs evenly and solution A is made;Again by Na3C6H5O7With Ni
(NO3)2.6H2O is successively dissolved in deionized water, stirs evenly and B solution is made, and solution A is poured into B solution, is existed after mixing evenly
Ethyl alcohol centrifuge washing is used after standing reaction a period of time at room temperature, is dried in vacuo to obtain Ni-Co PBAs in 80 DEG C of temperature conditions
Nano cubic particle;
Step 2: it takes the Ni-Co PBAs nano cubic particle ultrasound of certain mass evenly dispersed in deionized water, is added one
Determine the NaOH solution of solubility, stirring is made into C solution;Continue that C solution certain time is stirred by ultrasonic, solution colour is become from blue and white
Light green color;With ethyl alcohol centrifuge washing 5 times, finally vacuum drying obtains jade-green Ni (OH) under the conditions of 80 DEG C2Nano particle
Powder.
2. a kind of porous Ni (OH) according to claim 12The preparation method of nanocages, it is characterised in that: the step 1
Middle K3[Co(CN)6] concentration be 0.02mol/L, Na3C6H5O7Concentration be 0.045mol/L, Ni (NO3)2Concentration be
0.03mol/L。
3. a kind of porous Ni (OH) according to claim 12The preparation method of nanocages, it is characterised in that: the step 1
In, solution A quickly stirs 3-5min after mixing with B solution, stand 3-7day.
4. a kind of porous Ni (OH) according to claim 12The preparation method of nanocages, it is characterised in that: the step 2
In, the mass concentration of Ni-Co PBAs particle is 1-1.5mg/mL in C solution.
5. a kind of porous Ni (OH) according to claim 12The preparation method of nanocages, it is characterised in that: the step 2
In, the solubility of NaOH is 0.375-0.5mol/L in C solution.
6. a kind of porous Ni (OH) according to claim 12The preparation method of nanocages, it is characterised in that: the step 2
In, the reaction ultrasonic agitation time is 6-10hour.
7. a kind of porous Ni (OH)2Nanocages, it is characterised in that: its be cube structure nanocages, the 6 of the cubic structure
The centre of surface of a plane is embedded in a similar coniform hole, and the bottom of 6 holes is in the geometry of cubic structure
The heart communicates with one another at position, and the structure of a nanocage is presented;Ni(OH)2The size dimension of nanocages is 300-400nm, hole
The diameter in hole increases with depth and is successively decreased.
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CN111359624A (en) * | 2020-04-21 | 2020-07-03 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Core-shell hollow Cu (OH)2@Au@Co(OH)2Composite material, preparation method and application |
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CN111359624A (en) * | 2020-04-21 | 2020-07-03 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Core-shell hollow Cu (OH)2@Au@Co(OH)2Composite material, preparation method and application |
CN111359624B (en) * | 2020-04-21 | 2022-12-02 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Core-shell hollow Cu (OH) 2 @Au@Co(OH) 2 Composite material, preparation method and application |
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