CN114408985A - Oxygen-doped nickel-cobalt sulfide material and preparation method thereof - Google Patents

Oxygen-doped nickel-cobalt sulfide material and preparation method thereof Download PDF

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CN114408985A
CN114408985A CN202210062749.3A CN202210062749A CN114408985A CN 114408985 A CN114408985 A CN 114408985A CN 202210062749 A CN202210062749 A CN 202210062749A CN 114408985 A CN114408985 A CN 114408985A
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oxygen
nickel
cobalt
sulfide
nico
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吴海伟
李燚燚
韦海茹
郭彦伯
任宣
刘汉斌
孟卿君
李志健
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Abstract

The invention provides an oxygen-doped nickel-cobalt sulfide material and a preparation method thereof, wherein the preparation method comprises the following steps of 1, adding a nickel-cobalt oxide material into a soluble sulfur salt solution to obtain a mixed system B; wherein the molar ratio of the nickel cobalt oxide to the sodium sulfide is 1 (1.15-4); and 2, carrying out hydrothermal reaction on the mixed system B at the temperature of 140-180 ℃ for 2-10h, and drying the obtained product to obtain the oxygen-doped nickel-cobalt sulfide material. The novel oxygen-sulfur co-oxidized binary metal compound obtained by the invention is combined with NiCo2O4Material and NiCo2S4The material has the advantages of chemical stability of oxide and high conductivity of sulfide, and has better effect on adsorption and catalytic reaction of lithium polysulfide in the lithium-sulfur battery.

Description

Oxygen-doped nickel-cobalt sulfide material and preparation method thereof
Technical Field
The invention relates to the technical field of oxygen-doped material preparation, in particular to an oxygen-doped nickel-cobalt sulfide material and a preparation method thereof.
Background
Nickel cobalt oxide (i.e., NiCo)2O4) With nickel cobalt sulphide (i.e. NiCo)2S4) The material is a binary metal compound with excellent conductivity and electrochemical activity, has a very wide application prospect in the fields of super capacitors and lithium ion batteries, but has respective defects. NiCo2O4The material has strong chemical stability in air, but the conductivity is similar to that of NiCo2S4The material comparison is poor; NiCo2S4The material has high conductivity, but the electrochemical stability in air is poor, and the material is easy to deteriorate. Their drawbacks limit the application of both materials.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an oxygen-doped nickel-cobalt sulfide material and a preparation method thereof, and the obtained novel oxygen-sulfur co-oxidized binary metal compound combines NiCo2O4Material and NiCo2S4The material has the advantages of chemical stability of oxide and high conductivity of sulfide, and has better effect on adsorption and catalytic reaction of lithium polysulfide in the lithium-sulfur battery.
The invention is realized by the following technical scheme:
a preparation method of an oxygen-doped nickel cobalt sulfide material comprises the following steps:
step 1, adding a nickel-cobalt oxide material into a soluble sulfur salt solution to obtain a mixed system B; wherein the molar ratio of the nickel cobalt oxide to the sodium sulfide is 1 (1.15-4);
and 2, carrying out hydrothermal reaction on the mixed system B at the temperature of 140-180 ℃ for 2-10h, and drying the obtained product to obtain the oxygen-doped nickel-cobalt sulfide material.
Preferably, in step 1, the preparation method of the nickel-cobalt oxide material comprises:
adding nickel salt, cobalt salt and weak base into water, and uniformly dispersing to obtain a mixed system A;
step (2), carrying out hydrothermal reaction on the mixed system A, and drying the obtained product to obtain a precursor of the nickel-cobalt oxide;
and (3) sintering the precursor of the nickel-cobalt oxide at high temperature to obtain the nickel-cobalt oxide material.
Further, in the step (1), carbon spheres are also added into the water.
Further, the size of the carbon sphere is 200-500 nm.
Further, in the step (1), the nickel salt is Ni (NO)3)2·6H2O, cobalt salts being Co (NO)3)2·6H2O, and the weak base is urea.
Preferably, in the step 1, the concentration of the soluble sulfur salt solution is 0.015 to 0.04 mol/L.
Preferably, in step 1, the soluble sulfur salt is one of anhydrous sodium sulfide, sodium sulfide hydrate salt and sodium thiosulfate.
The oxygen-doped nickel-cobalt sulfide material prepared by the preparation method.
Preferably, the oxygen-doped nickel cobalt sulphide material has an atomic oxygen content of more than 15%.
Compared with the prior art, the invention has the following beneficial effects:
the invention carries out hydrothermal reaction on nickel cobalt oxide and sodium sulfide, controls the proportional relation of the nickel cobalt oxide and the sodium sulfide, leads the nickel cobalt oxide to be partially vulcanized in a sodium sulfide solution, obtains an oxygen-sulfur co-oxidized binary metal compound, and has the product structure and NiCo2S4In line with, but containing a large amount of doped oxygen, the invention is named as oxygen-doped nickel cobalt sulfide (O-NiCo)2S4)。O-NiCo2S4Incorporating NiCo2O4Material and NiCo2S4The material has the advantages of chemical stability of oxide and high conductivity of sulfide, and realizes advantage complementation. The method has the advantages of good reproducibility, high yield and simplicity, and can effectively control the structure and the shape of the oxygen-doped nickel-cobalt sulfide and the doping amount of oxygen.
Furthermore, the carbon spheres are added as templates, so that the dispersibility of the nickel-cobalt oxide material can be improved.
Drawings
FIG. 1 is a graph showing the conductivity measurements of the sample and oxides and sulfides of example 1.
FIG. 2 is a XRD test pattern of the product of example 1 and oxides and sulfides after one month in air.
Figure 3 is an EDS plot of the product of example 1 and the product of example 2.
In fig. 4, a, b, c, d, e and f are SEM images of products of nickel cobalt oxide, example 4, example 5, example 1, example 2 and nickel cobalt sulfide, respectively.
FIG. 5 is an SEM image of the products of example 6 and example 7.
Fig. 6 is a plot of the lithium polysulfide absorption uv spectra of nickel cobalt oxide and nickel cobalt sulfide and the product of example 1.
Detailed Description
For a further understanding of the invention, reference will now be made to the following examples, which are provided to illustrate further features and advantages of the invention, and are not intended to limit the scope of the invention as set forth in the following claims.
The preparation method of the oxygen-doped nickel cobalt sulfide material, wherein the oxygen-doped nickel cobalt sulfide can be abbreviated as O-NiCo2S4The method comprises the following steps:
step 1, uniformly dispersing nickel salt, cobalt salt and weak base in deionized water to obtain a mixed system A.
And 2, adding the mixed system A into a hydrothermal reaction kettle, reacting at 150-200 ℃ for 2-12h, cooling to room temperature, removing impurities in the product, and drying the obtained product in vacuum to avoid the product from being oxidized and influenced by impurities to obtain a precursor of the nickel-cobalt oxide.
And 3, sintering the precursor of the nickel-cobalt oxide at 380 ℃ for 4h, and heating at the speed of 1 ℃/min to obtain the nickel-cobalt oxide material.
And 4, dissolving sodium sulfide salt in deionized water to obtain a soluble sulfate salt solution, wherein the soluble sulfate salt is selected from one of anhydrous sodium sulfide, sodium sulfide hydrate salt and sodium thiosulfate to form a uniform solution, and adding the nickel-cobalt oxide material prepared in the step 3 into the soluble sulfate salt solution to obtain a mixed system B.
And 5, carrying out hydrothermal reaction on the mixed system B at the temperature of 140-180 ℃ for 2-10h, cooling to room temperature, carrying out suction filtration and washing to remove impurities in the product, and drying the obtained product to obtain the oxygen-doped nickel-cobalt sulfide material.
In the step 1, a self-made carbon sphere can be added, and the mixture is kept stand for 48 hours to enable the carbon sphere to fully adsorb nickel ions and cobalt ions, so that a mixed system A is obtained. The nickel salt being Ni (NO)3)2·6H2O, cobalt salts being Co (NO)3)2·6H2O, weak base is urea, and the proportion of nickel salt, cobalt salt and weak base is 0.0075: 0.015: 0.1375. the carbon spheres have an approximate size of 200-500nm and a concentration in the range of 1.0-2.5 g/L.
The reaction temperature in step 2 is preferably 180 ℃ and the reaction time is preferably 10 hours.
The concentration of the soluble sulfur salt in step 4 is preferably 0.015 to 0.04mol/L, more preferably 0.02 mol/L.
The molar ratio of the nickel cobalt oxide to the soluble sulfur salt in the step 4 is 1 (1.15-4), so that NiCo2O4The powder is substituted to varying degrees, preferably 1 (2-4), more preferably 1: 2.
the reaction temperature in step 5 was 160 ℃. The reaction time in step 5 is preferably 8 h.
Example 1
One kind has O-NiCo2S4The preparation method of the material comprises the following steps:
step 1, ultrasonically dispersing 80mL of 2.5g/L carbon sphere suspension liquid until the suspension liquid is uniform, and then adding Ni (NO)3)2·6H2O and Co (NO)3)2·6H2Adding O into the carbon sphere dispersion liquid according to the molar ratio of 1:2 to dissolve, adding urea, stirring to dissolve, and standing for 24 hours to obtain a uniform suspension; ni (NO) in suspension3)2·6H2The concentration of O is 0.0075mol/L, Co (NO)3)2·6H2The concentration of O was 0.015mol/L and the concentration of urea was 0.1375 mol/L.
Step 2, transferring 80mL of suspension into a 100mL reaction kettle, reacting at 180 ℃ for 10h, naturally cooling the suspension to room temperature, performing suction filtration, and then using deionized water and ethanolWashing for 3 times to remove impurities in the product, and continuously drying for 24 hours at 60 ℃ in vacuum to obtain the carbon spheres @ NiCo2O4A precursor; carbon spheres @ NiCo2O4Putting the precursor into a porcelain boat, heating to 380 ℃ at the heating rate of 1 ℃/min under the air atmosphere, and preserving the heat for 4h to obtain NiCo2O4And (3) powder.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.02mol/L, stirring to form uniform solution, and adding 0.2g of NiCo prepared in the step 22O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 8h at 160 ℃, naturally cooling the reaction kettle to room temperature, washing for 3 times with deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12h at 80 ℃ to obtain O-NiCo2S4And (3) powder.
The O-NiCo is observed by a scanning electron microscope SEM2S4The material is in a flower cluster structure, and the oxygen content is determined by using an energy spectrum EDS, as shown in figure 3.
Example 2
O-NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, as in step 1 and step 2 of example 1 above.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.04mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 8h at 160 ℃, naturally cooling the reaction kettle to room temperature, washing a filter cake for 3 times by using deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12h at 80 ℃ to obtain O-NiCo2S4And (3) powder.
Example 3
O-NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, as in step 1 and step 2 of example 1 above.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.015mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 8h at 160 ℃, naturally cooling the reaction kettle to room temperature, washing for 3 times with deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12h at 80 ℃ to obtain O-NiCo2S4And (3) powder.
Example 4
O-NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, as in step 1 and step 2 of example 1 above.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.02mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 2h at 160 ℃, naturally cooling the reaction kettle to room temperature, washing a filter cake for 3 times by using deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12h at 80 ℃ to obtain O-NiCo2S4And (3) powder.
Example 5
O-NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, as in step 1 and step 2 of example 1 above.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.02mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 4h at 160 ℃, naturally cooling the reaction kettle to room temperature, washing a filter cake for 3 times by using deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12h at 80 ℃ to obtain O-NiCo2S4And (3) powder.
Example 6
O-NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, as in step 1 and step 2 of example 1 above.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.02mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 10h at 160 ℃, naturally cooling the reaction kettle to room temperature, washing a filter cake for 3 times by using deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12h at 80 ℃ to obtain O-NiCo2S4And (3) powder.
Example 7
O-NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, as in step 1 and step 2 of example 1 above.
Step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.02mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring.
Step 4, transferring the obtained mixed system into a 100ml reaction kettle, reacting for 8 hours at 140 ℃, naturally cooling the reaction kettle to room temperature, washing a filter cake for 3 times by using deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12 hours at 80 ℃ to obtain the O-NiCo2S4And (3) powder.
Example 8
O-NiCo2S4The preparation method of the material comprises the following steps,
step 1 and step 2, as in step 1 and step 2 of example 1 above:
step 3, preparing 80mL of sodium sulfide solution with the concentration of 0.02mol/L, stirring to form uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and stirringAnd (4) homogenizing.
Step 4, transferring the obtained mixed system into a 100ml reaction kettle, reacting for 8 hours at 180 ℃, naturally cooling the reaction kettle to room temperature, washing a filter cake for 3 times by using deionized water and absolute ethyl alcohol while performing suction filtration, and performing vacuum drying for 12 hours at 80 ℃ to obtain O-NiCo2S4And (3) powder.
Comparative example 1
NiCo2S4The preparation method of the material comprises the following steps:
step 1 and step 2, which are the same as step 1 and step 2 of example 1 above;
step 3, preparing a sodium sulfide solution with the concentration of 0.2mol/L, stirring to form a uniform solution, and mixing 0.2g of NiCo prepared in the step 12O4Adding the powder into the solution, and uniformly stirring;
step 4, transferring 80mL of the obtained mixed system into a 100mL reaction kettle, reacting for 8 hours at 160 ℃, taking out the powder after sulfur substitution after the reaction kettle is naturally cooled to room temperature, washing the filter cake for 3 times while performing suction filtration by using deionized water and absolute ethyl alcohol, and performing vacuum drying for 12 hours at 80 ℃ to obtain NiCo2S4And (3) powder.
FIG. 1 is a graph of conductivity measurements of the sample and oxides and sulfides of example 1, and it can be seen that the conductivity of pure sulfide is up to 51.2S/cm and that of pure oxide is up to 0.2S/cm, whereas the conductivity of the oxygen-doped sulfide synthesized by the present invention is close to that of sulfide, reaching about 30S/cm. It is demonstrated that this oxygen-doped sulfide synthesized by the present invention retains the high conductivity of the sulfide.
Fig. 2 is an XRD test chart of the product of example 1 and oxides and sulfides after being left in air for one month, and it can be seen that the oxides and the product of the invention maintain the original crystal forms, and the sulfides have undergone crystal form change, which indicates that the product synthesized by the invention has good stability and inherits the stability of the oxides.
In fig. 3, a and b are EDS graphs of the product of example 1 and the product of example 2, respectively, and tables 1 and 2 are data on the oxygen and sulfur contents of the product of example 1 and the product of example 2, respectively.
TABLE 1 oxygen and sulfur content data for the product of example 1
Element Wt％ At％
O 16.12 37.28
S 18.97 21.90
Table 2 oxygen and sulfur content data for the product of example 2
Element Wt％ At％
O 06.22 15.60
S 35.56 44.60
As can be seen from fig. 3, table 1 and table 2, the atomic content of oxygen in the oxygen-doped sulfide of example 1 is as high as about 37%; example 2 the oxygen-doped sulfide has an oxygen atom content as high as about 15.6%, example 1 has a higher oxygen content and the atomic ratio of oxygen to sulfur is as high as 1.7: 1.
FIG. 4 is SEM images of products of examples a, b, c, d, e and f, which are Ni-Co oxide, example 4, example 5, example 1, example 2 and Ni-Co sulfide, respectively, and it can be seen that in the products of examples 4 and 5, the structure of the products collapses due to insufficient reaction time, and the products of examples 1 and 2 have complete structures and are obviously in the shape of clusters and approach to Ni-Co sulfide; however, the products of examples 1 and 2 contain a higher oxygen atom content due to incomplete sulfidation.
FIG. 5 is an SEM image of the products of examples 7 and 8, showing that many particles are not formed at 140 ℃ and the cluster-like structure is ablated at 180 ℃ so that the optimum temperature is 160 ℃.
FIG. 6 shows the UV absorption spectra of oxides, sulfides and lithium polysulfide of the product of example 1, wherein the highly oxygen-doped sulfide has better absorption effect than the oxides and sulfides, and after 1h, it can be seen that the variation of the absorption peak intensity of the highly oxygen-doped sulfide is significantly greater than that of the oxides and sulfides, so that the highly oxygen-doped sulfide can be used as a highly efficient lithium-sulfur battery catalyst.
The above-described embodiments are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various improvements, equivalent substitutions and modifications made by the method concepts and technical solutions of the present invention should be included in the above-described embodiments.

Claims (9)

1. The preparation method of the oxygen-doped nickel-cobalt sulfide material is characterized by comprising the following steps of:
step 1, adding a nickel-cobalt oxide material into a soluble sulfur salt solution to obtain a mixed system B; wherein the molar ratio of the nickel cobalt oxide to the sodium sulfide is 1 (1.15-4);
and 2, carrying out hydrothermal reaction on the mixed system B at the temperature of 140-180 ℃ for 2-10h, and drying the obtained product to obtain the oxygen-doped nickel-cobalt sulfide material.
2. The method for preparing oxygen-doped nickel cobalt sulfide material according to claim 1, wherein in step 1, the method for preparing nickel cobalt oxide material is as follows:
adding nickel salt, cobalt salt and weak base into water, and uniformly dispersing to obtain a mixed system A;
step (2), carrying out hydrothermal reaction on the mixed system A, and drying the obtained product to obtain a precursor of the nickel-cobalt oxide;
and (3) sintering the precursor of the nickel-cobalt oxide at high temperature to obtain the nickel-cobalt oxide material.
3. The method for preparing oxygen-doped nickel cobalt sulfide material according to claim 2, wherein in the step (1), carbon spheres are further added into the water.
4. The method as claimed in claim 3, wherein the carbon spheres have a particle size of 200-500 nm.
5. The method for preparing oxygen-doped nickel cobalt sulfide material as claimed in claim 2, wherein in the step (1), the nickel salt is Ni (NO)3)2·6H2O, cobalt salts being Co (NO)3)2·6H2O, and the weak base is urea.
6. The method for preparing oxygen-doped nickel cobalt sulfide material according to claim 1, wherein in step 1, the concentration of the soluble sulfur salt solution is 0.015-0.04 mol/L.
7. The method of claim 1, wherein in step 1, the soluble sulfur salt is one of anhydrous sodium sulfide, hydrated sodium sulfide and sodium thiosulfate.
8. Oxygen-doped nickel cobalt sulphide material obtainable by the method of preparation according to any one of claims 1 to 7.
9. The oxygen doped nickel cobalt sulfide material of claim 8 wherein the oxygen doped nickel cobalt sulfide material has an atomic oxygen content of greater than 15%.
CN202210062749.3A 2022-01-19 2022-01-19 Oxygen-doped nickel-cobalt sulfide material and preparation method thereof Pending CN114408985A (en)

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