CN111186826A - Ni2P nanosphere and preparation method thereof - Google Patents
Ni2P nanosphere and preparation method thereof Download PDFInfo
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- CN111186826A CN111186826A CN201911378996.9A CN201911378996A CN111186826A CN 111186826 A CN111186826 A CN 111186826A CN 201911378996 A CN201911378996 A CN 201911378996A CN 111186826 A CN111186826 A CN 111186826A
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- 239000002077 nanosphere Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 42
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 24
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- 238000003786 synthesis reaction Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 7
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- -1 aromatic nitro compounds Chemical class 0.000 description 3
- 238000010531 catalytic reduction reaction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 3
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/08—Other phosphides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
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- 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
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
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Abstract
The invention discloses Ni2The P nanosphere and the preparation method thereof comprise the following steps: respectively dissolving nickel chloride hexahydrate and sodium hypophosphite in deionized water, uniformly mixing the two solutions, slowly adding the mixture into an aqueous solution of sodium hydroxide, and uniformly mixing. Then adding a certain amount of white phosphorus, fully mixing, transferring the mixed solution into a reaction kettle, and reactingAnd placing the reaction kettle in an oven for heating, reacting for a certain time, naturally cooling to room temperature, and centrifugally separating, washing and vacuum drying the reacted mixture to obtain a dark green solid. Invention realization of Ni2P nanosphere and Ni12P5Controllable synthesis of the nanospheres, uniform nanosphere size, simple and easy synthesis process and good repeatability.
Description
Technical Field
The invention relates to the field of preparation of nickel phosphide catalysts, in particular to Ni2P nanospheres and a preparation method thereof.
Background
With the development of society, sewage generated in the medicine and dye industries can have great influence on the environment. Especially, organic matters such as p-nitrophenol and o-nitrophenol contained in the sewage are always a big problem in the treatment of industrial wastewater due to high toxicity and stability.
Transition metal phosphides have been attracting much attention from researchers because of their excellent catalytic, electrochemical, and semiconductor properties. Research shows that the nano-structure of nickel phosphide and the like has remarkable catalytic activity on the reduction of certain organic small molecules or aromatic nitro compounds in aqueous solution.
The existing research shows that:
the bonding mode of the transition metal nickel and the phosphorus is special, and a nickel-phosphorus bond, a nickel-nickel bond and a phosphorus-phosphorus bond can be formed, so that transition metal phosphide Ni with different nickel-phosphorus ratios can be obtained according to different bonding modesxPy。
However, in the preparation method for preparing transition metal phosphide disclosed in the prior art, it is not easy to control NixPyPrepared to obtain NixPyMixtures of different molecular structures are not used for aromatic catalytic reduction.
Disclosure of Invention
The invention aims to provide Ni with simple method and easily controlled structure2A preparation method of the P nanosphere.
The invention solves the technical problems through the following technical scheme:
a preparation method of Ni2P nanospheres comprises the following steps:
(1) respectively dissolving nickel chloride hexahydrate and sodium hypophosphite in deionized water, uniformly mixing the two solutions, and slowly adding a sodium hydroxide aqueous solution under the condition of stirring;
(2) adding white phosphorus into the mixed solution, and uniformly stirring;
(3) transferring the mixed solution into a reaction kettle, placing the reaction kettle in an oven at the temperature of 150-180 ℃, reacting for 5-24 hours, naturally cooling to room temperature, centrifugally separating, washing and vacuum drying the reacted mixture to obtain dark green solid Ni2And (4) P nanospheres.
Preferably, 0.237g of nickel chloride hexahydrate and 0-2.65 g of sodium hypophosphite are respectively added into 20mL of deionized water in the step (1), and the two solutions are uniformly mixed; under the condition of stirring, 1-5 mL of 2mol/L sodium hydroxide solution is slowly added.
Preferably, the added mass of the white phosphorus is 0.02-0.12 g.
Preferably, the reaction kettle in the step (3) is a high-pressure reaction kettle lined with polytetrafluoroethylene.
Preferably, the reaction temperature in the step (3) is 170 ℃.
The invention also discloses Ni prepared by the preparation method of the Ni2P nanosphere2And (4) P nanospheres.
Compared with the prior art, the invention has the following advantages:
according to the invention, under the condition of not using a surfactant, Ni can be obtained respectively under hydrothermal conditions by changing the dosage of nickel chloride hexahydrate, sodium hypophosphite and white phosphorus2P nanosphere and Ni12P5The nanosphere has simple and convenient preparation process. And in the preparation method, the structure is easy to control.
By using Ni2The P nanosphere is a catalyst and has remarkable catalytic activity on reduction of aromatic nitro compounds in aqueous solution.
Drawings
FIG. 1a shows Ni obtained in example 1 of the present invention2X-ray powder diffractogram of P nanospheres;
FIG. 1b shows Ni obtained in example 1 of the present invention2Scanning electron microscope pictures of the P nanospheres.
FIG. 2 is an X-ray powder diffraction pattern of a product obtained by varying the amounts of nickel chloride hexahydrate and sodium hypophosphite in an example of the present invention;
FIG. 3 is an XRD pattern of different samples obtained by varying the quantitative ratio of nickel chloride hexahydrate to white phosphorus in the examples of the present invention;
FIG. 4a shows Ni as a precursor in example 13 of the present invention2The P nanosphere is an ultraviolet-visible spectrum diagram of the P-nitrophenol catalytically degraded by the catalyst;
FIG. 4b shows Ni as a precursor of example 13 of the present invention12P5The nanosphere is an ultraviolet-visible spectrum diagram of the catalyst for catalyzing and degrading the p-nitrophenol.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Ni2The preparation method of the P nanosphere comprises the following steps:
0.237g of nickel chloride hexahydrate and 1.06g of sodium hypophosphite are weighed into two beakers, 20ml of deionized water is added into each beaker, and the mixture is dissolved under magnetic stirring to form a uniform dispersion solution. 2mL of a 2mol/L aqueous solution of sodium hydroxide was slowly added with stirring.
The solution was then transferred to a 50mL autoclave lined with Teflon, charged with 0.06 g of white phosphorus, sealed, and reacted in an oven at 170 ℃ for 10 h. Naturally cooling to room temperature, washing with deionized water and absolute ethyl alcohol for three times, and vacuum drying at 60 ℃ for 12h to obtain a dark green solid product Ni2And (4) P nanospheres.
Ni2X-ray powder diffraction results of P nanospheres are shown in FIG. 1a, all diffraction peaks in FIG. 1a correspond to those of a standard card (JCPDS No.03-0953), and the product can be proved to be Ni2P。
Ni2The scanning electron microscope result of the P nanosphere is shown in figure 1b, and the product is of a nanosphere structure with the diameter of about 50 nm.
In this example, the mass ratio of nickel chloride hexahydrate to sodium hypophosphite was 1: 10. The amount ratio of the nickel chloride hexahydrate to the white phosphorus material is 1: 0.5.
Example 2
In this example, the amount of sodium hypophosphite was 0 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 0.
Example 3
In this example, the amount of sodium hypophosphite was 0.106 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 1.
Example 4
In this example, the amount of sodium hypophosphite was 0.318 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 3.
Example 5
In this example, the amount of sodium hypophosphite was 0.53 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 5.
Example 6
In this example, the amount of sodium hypophosphite was 1.59 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 15.
Example 7
In this example, the amount of sodium hypophosphite was 2.12 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 20.
Example 8
In this example, the amount of sodium hypophosphite was 2.65 g. Other embodiments are the same as example 1. The mass ratio of the nickel chloride hexahydrate to the sodium hypophosphite is 1: 25.
Example 9
In this example, 0g of white phosphorus was added. Other embodiments are the same as example 1. The quantity ratio of the nickel chloride hexahydrate to the white phosphorus substance is 1: 0.
Example 10
In this example, 0.03g of white phosphorus was added. Other embodiments are the same as example 1. The quantity ratio of the nickel chloride hexahydrate to the white phosphorus substance is 1: 0.25.
Example 11
In this example, 0.12g of white phosphorus was added. Other embodiments are the same as example 1. The quantity ratio of the nickel chloride hexahydrate to the white phosphorus substance is 1: 1.
Example 12 analysis of results
The following results were analyzed for the experimental results of the above examples 1 to 12:
FIG. 1a shows the preparation of pure Ni according to example 12P, all diffraction peaks in the XRD pattern correspond to standard card (JCPDS No. 03-0953).
FIG. 1b preparation of pure Ni for example 12SEM image of P, from which Ni can be seen2P is spherical, the appearance of the sample is relatively uniform, and the diameter of the nanosphere is about 50 nm.
As shown in fig. 2, by changing the amount ratio of nickel chloride hexahydrate to sodium hypophosphite, XRD patterns of different samples were obtained, as can be seen from fig. 2:
when the ratio is 1: 0, the obtained sample is Ni (OH)2；
When the ratio is 1: 1 and 1: 3, the obtained samples correspond to Ni11(HPO3)8(OH)6；
When the ratio was 1: 5, 1: 10 and 1: 15, the samples obtained corresponded to Ni2P；
When the ratio was 1: 20 and 1: 25, the samples obtained corresponded to Ni12P5。
As shown in fig. 3, by changing the amount ratio of nickel chloride hexahydrate to white phosphorus, XRD patterns of different samples were obtained, and it can be seen from fig. 3 that:
when the ratio is 1: 0, the obtained sample is Ni correspondingly;
when the ratio was 1: 0.25 and 1: 0.5, the samples obtained corresponded to Ni2P；
When the ratio is 1: 1, the obtained sample corresponds to Ni12P5。
Example 13 catalytic reduction of 4-nitrophenol
By using Ni2P nanosphere is used as catalyst for catalyzing 4-nitrophenolWhen the original is 4-aminophenol, Ni2The P nanosphere has stronger catalytic activity, and the catalytic capacities of different catalysts are as follows in sequence: ni2P nanosphere > Ni12P5Nanospheres.
FIGS. 4a and 4b are UV-VIS spectra of the above-mentioned catalytic reduction of 4-nitrophenol, and it can be seen from FIGS. 4a and 4b that:
equal amount of Ni2P nanosphere and Ni12P5When nanospheres are used as catalysts, Ni2The P nanospheres reduce and convert 4-nitrophenol to be close to 100% within 3 min; and Ni12P5Nanospheres required 5 min.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. Ni2The preparation method of the P nanosphere is characterized by comprising the following steps of:
(1) respectively dissolving nickel chloride hexahydrate and sodium hypophosphite in deionized water, uniformly mixing the two solutions, and slowly adding a sodium hydroxide aqueous solution under the condition of stirring;
(2) adding white phosphorus into the mixed solution, and uniformly stirring;
(3) transferring the mixed solution into a reaction kettle, placing the reaction kettle in an oven at the temperature of 150-180 ℃, reacting for 5-24 hours, naturally cooling to room temperature, centrifugally separating, washing and vacuum drying the reacted mixture to obtain dark green solid Ni2And (4) P nanospheres.
2. The preparation method of the Ni2P nanosphere according to claim 1, wherein in step (1), 20mL of deionized water is added to 0.237g of nickel chloride hexahydrate and 0-2.65 g of sodium hypophosphite respectively, and the two solutions are mixed uniformly; under the condition of stirring, slowly adding 1-5 mL of 2mol/L sodium hydroxide solution.
3. The method for preparing Ni2P nanospheres according to claim 2, wherein the mass of added white phosphorus is 0.02-0.12 g.
4. The method for preparing the Ni2P nanospheres according to claim 1, wherein the autoclave in step (3) is a polytetrafluoroethylene-lined autoclave.
5. The method for preparing Ni2P nanospheres according to claim 4, wherein the reaction temperature in step (3) is 170 ℃.
6. Ni prepared by the method according to any one of claims 1 to 52And (4) P nanospheres.
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Application publication date: 20200522 |