CN109592721B - Porous Ni (OH)2Nano cage and preparation method thereof - Google Patents
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Abstract
The invention discloses a porous Ni (OH)2Nanometer cage and its preparation method are provided. The method comprises the following steps: the first step is to obtain Ni by chemical precipitation3[Co(CN)6]2(ii) a Second, washing and drying the Ni3[Co(CN)6]2Ultrasonically dissolving the powder in deionized water, adding Ni into the prepared NaOH solution3[Co(CN)6]2In the solution, obtaining porous Ni (OH) after ultrasonic stirring, centrifugal washing and drying2A nanocage. The preparation method has the advantages of cheap raw materials, mild and controllable reaction conditions, and synthesized porous Ni (OH)2The size of the nano cage is 300-400 nm. Porous Ni (OH) produced by the invention2The nanocage has the advantages of large open channel structure, large specific surface area, high permeability and the like, and has wide application prospects in the fields of catalysis, lithium ion batteries and supercapacitors.
Description
(I) technical field
The material of the invention is a functional nano material derived from an organic metal framework structure, in particular to porous Ni (OH)2A nano cage and a preparation method thereof belong to the field of new energy materials.
(II) background of the invention
Ni(OH)2Nanomaterials have been a very important class of energy storage and conversion (including lithium ion batteries and supercapacitors) materials in transition metal compounds. For example, Ni (OH)2Due to the low cost, rich form and large theoretical specific capacitance, the electrode material of the pseudo-capacitor super capacitor draws wide attention. But due to Ni (OH)2Poor conductivity and limited reactive sites, leading to experimental values far below the theoretical value. With the intensive research on the nano material, people are more and more aware that the electrochemical performance of the nano material can be improved by designing the structure and the shape of the material, and for example, the advantage that the hollow nano structure has a large surface area and the like becomes a competitive research object in the field of energy catalysis. Prussian Blue Analogues (PBAs) belong to a novel class of porous materials, consisting of metal cations and organic ligands. To be provided withThe porous functional nano material derived by taking PBAs as the template can be widely applied to catalysis, adsorption and energy storage. The PBAs derivative materials reported at present comprise transition metal hydroxides, oxides, sulfides and phosphides, and the formed appearance comprises a hollow nano box, a nano framework structure, a hollow cubic nano cage with truncated vertex angles and the like. The adopted method comprises a chemical etching method, an annealing treatment method and the like. However, until now, no hollow nanocage-shaped Ni (OH) has been found2To design an open structure, a large specific surface area and a high permeability of Ni (OH)2The nano material has important significance for improving the performance of the super capacitor and the battery.
Disclosure of the invention
The invention aims to provide porous Ni (OH)2Nanometer cage and its preparation method are provided. The nano cage-shaped Ni (OH)2Has the characteristics of open channel structure, large specific surface area, high permeability and the like, and can improve the catalytic and storage performances. Porous Ni (OH) of the invention2The successful preparation of the nanocages provides a new approach for the preparation of transition metal compounds.
In order to achieve the purpose, the technical scheme of the invention comprises the following steps: porous Ni (OH)2The preparation method of the nano cage comprises the following steps:
the method comprises the following steps: will K3[Co(CN)6]Dissolving in deionized water, and stirring to obtain solution A; then adding Na3C6H5O7With Ni (NO)3)2.6H2Dissolving O in deionized water in sequence, stirring uniformly to prepare a solution B, pouring the solution A into the solution B, stirring uniformly, standing at room temperature for reaction for a period of time, then centrifugally washing with ethanol, and drying in vacuum at the temperature of 80 ℃ to obtain Ni-Co PBAs nano cubic particles.
Step two: taking Ni-Co PBAs nano cubic particles with certain mass, uniformly dispersing in deionized water by ultrasonic, adding NaOH solution with certain solubility, and stirring to prepare C solution. And continuing to stir the solution C by ultrasound for a certain time, and changing the color of the solution from blue white to light green. Washing with ethanol for 5 times, and centrifuging at 80 deg.CVacuum drying to obtain light green Ni (OH)2A nanoparticle powder.
Further, K in the first step3[Co(CN)6]Has a concentration of 0.02mol/L, Na3C6H5O7Has a concentration of 0.045mol/L, Ni (NO)3)2The concentration of (B) is 0.03 mol/L.
Further, in the first step, the solution A and the solution B are mixed, rapidly stirred for 3-5min and kept stand for 3-7 day.
Further, in the second step, the mass concentration of the Ni-Co PBAs particles in the C solution is 1-1.5 mg/mL.
Further, in the second step, the solubility of NaOH in the solution C is 0.375-0.5 mol/L.
Further, in the second step, the reaction ultrasonic stirring time is 6-10 hours.
Porous Ni (OH)2The nano cage is a nano cage with a cubic structure, the centers of the surfaces of 6 planes of the cubic structure are embedded with a hole similar to a cone, and the bottoms of the 6 holes are mutually communicated at the position of the geometric center of the cubic structure to form a nano cage-shaped structure; ni (OH)2The side length of the nano cage is 300-400nm, and the diameter of the hole decreases with the increase of the depth.
The invention has the beneficial effects that: the invention relates to a porous Ni (OH)2The nano cage and the preparation method thereof have the advantages of cheap raw materials and mild reaction conditions. In addition, the porous Ni (OH)2The nano cage structure has the characteristics of an open large channel structure, a large specific surface area, high permeability, ultralow density and the like, and is an ideal material for storage and conversion of adsorption, catalysts, alkali metal ion batteries and super energy sources.
(IV) description of the drawings
FIG. 1 shows Ni (OH) produced by the present invention2Phase analysis XRD spectrum of the sample.
FIG. 2 shows Ni (OH) prepared according to the present invention2Morphology analysis (SEM and TEM) images of the samples.
(V) detailed description of the preferred embodiments
The technical solution of the present invention is further described with reference to the accompanying drawings and specific embodiments.
Example 1:
respectively preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And Ni (NO) at a concentration of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 3min, standing at room temperature for reaction for 3day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 40mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.375mol/L, and continuously stirring by ultrasonic wave until 6hour, wherein the color of the solution is changed from blue white to light green. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C for 24 hours to obtain light green Ni (OH)2A nanoparticle powder.
FIG. 1 shows porous Ni (OH)2XRD spectrum of nanocage.
FIG. 2 shows porous Ni (OH)2SEM and TEM images of nanocages.
Example 2:
respectively preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na in a concentration of 0.045mol/L3C6H5O7And Ni (NO) at a concentration of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 3min, standing at room temperature for 5day of reaction, centrifugally washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 45mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.4mol/L, and continuously stirring by ultrasonic wave until the solution color is changed from blue white to light green after 7 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
Characterization by XRD, SEM and TEM gave results similar to those of example 1.
Example 3:
preparing 30ml of 0.02mol/L of K3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 3min, standing at room temperature for reaction for 7day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 30mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.4mol/L, and continuously stirring the mixture by ultrasonic wave until the solution color is changed from blue-white to light green after 8 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 4:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 4min, standing at room temperature for reaction for 3day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 40mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.375mol/L, and continuously stirring the mixture by ultrasonic wave until the solution color is changed from blue white to light green after 9 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 5:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2The solution B of (4) is prepared by pouring the solution A into the solution B, magnetically stirring for 4min, standing at room temperature for 5day, and reacting with the solution BAlcohol is centrifugally washed for 5 times, and the Ni-Co PBAs nano cubic particles are obtained by vacuum drying at the temperature of 80 ℃. Uniformly dispersing 45mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.4mol/L, and continuously stirring by ultrasonic wave until 10hour, wherein the color of the solution is changed from blue-white to light green. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 6:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 4min, standing at room temperature for reaction for 7day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 45mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.5mol/L, and continuously stirring by ultrasonic wave until the solution color is changed from blue-white to light green after 6 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 7:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 5min, standing at room temperature for reaction for 3day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 40mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.375mol/L, and continuously stirring the mixture by ultrasonic wave to 7hour, wherein the color of the solution is changed from blue white to light green. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 8:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 5min, standing at room temperature for 5day, centrifugally washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 45mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.4mol/L, and continuously stirring the mixture by ultrasonic wave until the solution color is changed from blue-white to light green after 8 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 9:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 5min, standing at room temperature for reaction for 7day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 40mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.5mol/L, and continuously stirring by ultrasonic wave until 9 hours, wherein the color of the solution is changed from blue-white to light green. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 10:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 5min, standing at room temperature for reaction for 3day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 40mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.45mol/L, and continuously stirring the mixture by ultrasonic wave until the solution color is changed from blue-white to light green after 9 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 11:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2And (3) pouring the solution A into the solution B, magnetically stirring for 5min, standing at room temperature for reaction for 3day, centrifuging and washing with ethanol for 5 times, and vacuum-drying at 80 ℃ to obtain Ni-Co PBAs (poly (butylene adipate/terephthalate)) nano cubic particles. Uniformly dispersing 45mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.45mol/L, and continuously stirring the mixture by ultrasonic wave until the solution color is changed from blue-white to light green after 9 hours. Washing with ethanol by centrifugation for 5 times, and drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Example 12:
preparing 30ml of K with the concentration of 0.02mol/L3[Co(CN)6]20ml of the solution A of (1), containing Na at a concentration of 0.045mol/L3C6H5O7And a concentration of Ni (NO) of 0.03mol/L3)2The solution A is poured into the solution B, and after magnetic stirring is carried out for 5min, the solution B is addedStanding at room temperature for 5day, centrifuging and washing with ethanol for 5 times, and vacuum drying at 80 deg.C to obtain Ni-Co PBAs nano cubic particles. Uniformly dispersing 45mg of Ni-Co PBAs nano cubic particles in 20ml of deionized water by ultrasonic wave, adding 10ml of NaOH solution with the solubility of 0.5mol/L, and continuously stirring by ultrasonic wave until 10hour, wherein the color of the solution is changed from blue-white to light green. Washing with ethanol by centrifugation for 5 times, and finally drying at 80 ℃ to obtain light green Ni (OH)2 nanoparticle powder.
The results were still similar to example 1, as characterized by XRD, SEM and TEM.
Therefore, the porous Ni (OH)2 nanocage and the preparation method thereof have the characteristics of open structure, large surface area, ultralow density and the like. The porous Ni (OH)2 nano cage prepared by the method is used as an anode material of a super capacitor, and shows enhanced electrochemical performance, such as characteristics of rapid charge and discharge under large current and the like.
Claims (5)
1. Porous Ni (OH)2The preparation method of the nano cage is characterized by comprising the following steps: the preparation method comprises the following steps:
the method comprises the following steps: will K3[Co(CN)6]Dissolving in deionized water, and stirring to obtain solution A; then adding Na3C6H5O7With Ni (NO)3)2.6H2Dissolving O in deionized water in sequence, stirring uniformly to prepare a solution B, pouring the solution A into the solution B, stirring uniformly, standing at room temperature for reaction for a period of time, then centrifugally washing with ethanol, and drying in vacuum at the temperature of 80 ℃ to obtain Ni-Co PBAs nano cubic particles;
step two: uniformly dispersing Ni-Co PBAs nano cubic particles with certain mass in deionized water by ultrasonic, adding a NaOH solution with certain solubility, and stirring to prepare a C solution; continuing to ultrasonically stir the solution C for a certain time, wherein the color of the solution is changed from blue-white to light-green; centrifuging with ethanol for 5 times, and vacuum drying at 80 deg.C to obtain light green Ni (OH)2A nanoparticle powder;
in the first step, the solution A and the solution B are mixed and then rapidly stirred for 3-5min, and then the mixture is kept stand for 3-7 day;
in the second step, the reaction ultrasonic stirring time is 6-10 hours.
2. A porous ni (oh) according to claim 12The preparation method of the nano cage is characterized by comprising the following steps: k in the step one3[Co(CN)6]Has a concentration of 0.02mol/L, Na3C6H5O7Has a concentration of 0.045mol/L, Ni (NO)3)2The concentration of (B) is 0.03 mol/L.
3. A porous ni (oh) according to claim 12The preparation method of the nano cage is characterized by comprising the following steps: in the second step, the mass concentration of the Ni-Co PBAs particles in the C solution is 1-1.5 mg/mL.
4. A porous ni (oh) according to claim 12The preparation method of the nano cage is characterized by comprising the following steps: in the second step, the solubility of NaOH in the solution C is 0.375-0.5 mol/L.
5. Porous Ni (OH)2Nanometer cage, its characterized in that: the structure is a nanocage with a cubic structure, the centers of the surfaces of 6 planes of the cubic structure are embedded with a hole similar to a cone, and the bottoms of the 6 holes are mutually communicated at the geometric center of the cubic structure to form a nanocage structure; ni (OH)2The side length of the nano cage is 300-400nm, and the diameter of the hole decreases with the increase of the depth.
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