CN112194107A - Transition metal phosphide nanowire bundle, and preparation method and application thereof - Google Patents
Transition metal phosphide nanowire bundle, and preparation method and application thereof Download PDFInfo
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 53
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000002243 precursor Substances 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 16
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011574 phosphorus Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
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- 238000002156 mixing Methods 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 8
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 8
- 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 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 7
- 150000001879 copper Chemical class 0.000 claims description 7
- 229910001416 lithium ion Inorganic materials 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 6
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 6
- 239000007773 negative electrode material Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical group [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 4
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 claims description 4
- AMWVZPDSWLOFKA-UHFFFAOYSA-N phosphanylidynemolybdenum Chemical compound [Mo]#P AMWVZPDSWLOFKA-UHFFFAOYSA-N 0.000 claims description 4
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 claims description 3
- 239000011540 sensing material Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 238000001354 calcination Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 239000010949 copper Substances 0.000 description 17
- 239000011259 mixed solution Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000010406 cathode material Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005696 Diammonium phosphate Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 2
- 229940076286 cupric acetate Drugs 0.000 description 2
- 229960003280 cupric chloride Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
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- 231100000252 nontoxic Toxicity 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
-
- 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
- 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
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a transition metal phosphide nanowire bundle, and a preparation method and application thereof. Wherein, the preparation method comprises the following steps: s1, dissolving transition metal salt in an organic solvent, heating to 100-150 ℃, reacting at a constant temperature, cooling to room temperature, centrifuging, washing and drying to obtain a precursor with the shape of the nanowire bundle; and S2, mixing the precursor with a phosphorus source, heating to 200-300 ℃, reacting, and cooling to room temperature to obtain the transition metal phosphide nanowire bundle. By applying the technical scheme of the invention, the method for preparing the transition metal phosphide nanowire bundle material based on the low-temperature calcination of the precursor is simple and convenient to operate, the adopted raw materials are cheap and easy to obtain, the cost is lower, the safety is high, and in addition, any surfactant and template are not required to be used in the synthesis process, so that the method is green and environment-friendly. The prepared transition metal phosphide nanowire bundle material has a one-dimensional linear morphology, and the nanowire bundle surface is clean and easy to carry out surface modification.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a transition metal phosphide nanowire bundle, and a preparation method and application thereof.
Background
The negative electrode material of the ion battery is mainly carbon materials such as graphite, and the specific capacity of the negative electrode material is low, so that the further development and application of the lithium ion battery are limited. Therefore, it is very important to develop a negative electrode material for a high-performance lithium ion battery.
Transition metal phosphides exhibit superior properties in magnetic, catalytic and energy storage applications, and researchers have developed a variety of synthetic routes to prepare phosphides and study their potential properties. However, most of these methods are complicated, require multiple steps, are toxic, expensive, explosive, etc. in the reaction reagents, and generally require high reaction temperatures. The method for calcining the precursor at low temperature has the advantages of being mild, low in energy consumption, free of danger, environment-friendly, good in crystallinity of the obtained product and the like. Copper phosphide takes various forms (Cu)3P、CuP2、Cu2P7) But only Cu3P can exist stably in air and has been widely used as a reinforcing agent for industrial welding materials as well as high-speed steel composite materials. Recent research shows that cuprous phosphide has good cycle stability as a lithium ion battery cathode material, and is one of important subjects in the research of transition metal phosphide cathode materials.
Currently, researchers have synthesized a variety of morphologies including nanotubes, hollow spheres, nanowire bundles, hexagonal nanoparticles, etc. (C.Wei; Y.Huang, chem.Eng.J.317, (2017), 873-. At present, with respect to Cu3The synthesis of P nanowire bundles is rarely reported. Fan, M. (Chen, Y.; Xie, Y., (2016), adv.Funct.Mater.,26:5019-3P nanowire bundles.
The synthesis of copper phosphide is more complex than that of other phosphide, and some methods also need special instruments, so that the process is complicated, the manufacturing cost is higher, and the repeatability is poorer, therefore, the design of a novel process which is low in temperature, non-toxic, simple and convenient to operate and low in cost has important significance.
Disclosure of Invention
The invention aims to provide a transition metal phosphide nanowire bundle, a preparation method and application thereof, and aims to solve the technical problem of complex process in the preparation process of nanowire bundle materials in the prior art.
In order to achieve the above objects, according to one aspect of the present invention, there is provided a method for preparing transition metal phosphide nanowire bundles. The preparation method comprises the following steps: s1, dissolving transition metal salt in an organic solvent, heating to 100-150 ℃, reacting at a constant temperature, cooling to room temperature, centrifuging, washing and drying to obtain a precursor with the shape of the nanowire bundle; and S2, mixing the precursor with a phosphorus source, heating to 200-300 ℃, reacting, and cooling to room temperature to obtain the transition metal phosphide nanowire bundle.
Further, the transition metal phosphide in the transition metal phosphide nanowire bundle is one or more of cobalt phosphide, molybdenum phosphide, nickel phosphide and cuprous phosphide.
Further, the transition metal phosphide in the transition metal phosphide nanowire bundle is cuprous phosphide.
Further, when the transition metal phosphide in the transition metal phosphide nanowire bundle is cuprous phosphide, the transition metal salt is cupric salt, and the cupric salt is cupric sulfate, cupric acetate, cupric nitrate or cupric chloride; preferably, the amount of the copper salt substance is 1-5 mmol.
Further, the organic solvent is any two or a combination of at least two selected from the group consisting of N, N-dimethylformamide, ethylene glycol, ethanol, dimethyl sulfoxide and isopropanol.
Further, the isothermal reaction time in the S1 is 2 to 8 hours; the reaction temperature in S2 is 2-8 hours; preferably, the reaction temperature in S2 is 200-270 ℃.
Further, the phosphorus source is one or more selected from the group consisting of diammonium phosphate, sodium hypophosphite, and phosphine.
Further, the mass ratio of the precursor to the phosphorus source is 1:8-1: 20.
According to another aspect of the present invention, there is provided a transition metal phosphide nanowire bundle. The transition metal phosphide nanowire bundle is prepared by any preparation method.
According to another aspect of the invention, the transition metal phosphide nanowire bundle is provided for application as a lithium ion battery anode material, a catalyst, an optical material and a sensing material.
By applying the technical scheme of the invention, the method for preparing the transition metal phosphide nanowire bundle material based on the low-temperature calcination of the precursor is simple and convenient to operate, the adopted raw materials are cheap and easy to obtain, the cost is lower, the safety is high, and in addition, any surfactant and template are not required to be used in the synthesis process, so that the method is green and environment-friendly. The prepared transition metal phosphide nanowire bundle material has a one-dimensional linear morphology, and the nanowire bundle surface is clean and easy to carry out surface modification.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows Cu obtained in example 13P nanometer beam material X-ray diffraction picture; and
FIG. 2 shows Cu obtained in example 13P nanowire bundle material scanning electron microscope pictures.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
According to an exemplary embodiment of the present invention, a method for preparing transition metal phosphide nanowire bundles is provided. The preparation method comprises the following steps: s1, dissolving transition metal salt in an organic solvent, heating to 100-150 ℃, reacting at a constant temperature, cooling to room temperature, centrifuging, washing and drying to obtain a precursor with the shape of the nanowire bundle; and S2, mixing the precursor with a phosphorus source, heating to 200-300 ℃, reacting, and cooling to room temperature to obtain the transition metal phosphide nanowire bundle.
By applying the technical scheme of the invention, the method for preparing the transition metal phosphide nanowire bundle material based on the low-temperature calcination of the precursor is simple and convenient to operate, the adopted raw materials are cheap and easy to obtain, the cost is lower, the safety is high, and in addition, any surfactant and template are not required to be used in the synthesis process, so that the method is green and environment-friendly.
In the present invention, the transition metal phosphide in the transition metal phosphide nanowire bundle may be one or more of cobalt phosphide, molybdenum phosphide, nickel phosphide and cuprous phosphide, typically monometallic phosphide and bimetallic phosphide. It is important in the present invention that the transition metal phosphide in the transition metal phosphide nanowire bundle is cuprous phosphide. When the transition metal phosphide in the transition metal phosphide nanowire bundle is cuprous phosphide, the transition metal salt is cupric salt, and the cupric salt is cupric sulfate, cupric acetate, cupric nitrate or cupric chloride; preferably, the amount of the copper salt substance is 1-5 mmol.
Preferably, the organic solvent is a combination comprising any two or at least two of N, N-dimethylformamide, ethylene glycol, ethanol, dimethyl sulfoxide and isopropanol.
According to a typical embodiment of the present invention, the isothermal reaction time in S1 is 2 to 8 hours; the reaction temperature in S2 is 2-8 hours, which ensures the full reaction; preferably, the reaction temperature in S2 is 200-270 ℃.
In one embodiment of the present invention, the phosphorus source is one or more selected from the group consisting of diammonium phosphate, sodium hypophosphite, and phosphine; preferably, the mass ratio of the precursor to the phosphorus source is 1:8-1:20, and pure-phase cuprous phosphide can be obtained within the mass ratio range. Because if the mass ratio of the precursor to the phosphorus source is too low, the phosphorization may not be successful, and if the mass ratio of the precursor to the phosphorus source is too high, the risk may exist in the experimental process.
In a preferred embodiment of the present invention, the preparation method comprises:
1) dissolving copper salt (1-5 mmol) in the mixed organic solvent, and fully stirring to uniformly mix the copper salt and the organic solvent; wherein the copper salt is one or more of copper sulfate, copper acetate, copper nitrate and copper chloride; the mixed organic solvent comprises any two or the combination of at least two of N, N-dimethylformamide, ethylene glycol, ethanol, dimethyl sulfoxide and isopropanol;
2) putting the mixed solution fully dissolved in the step 1) into a closed reactor, slowly heating (the heating rate is 3-10 ℃) to 100-150 ℃, reacting for 2-8 hours at the temperature, naturally cooling to room temperature, centrifuging, washing and drying to obtain a copper-based precursor with the shape of a nanowire bundle;
3) putting the precursor obtained in the step 1) into high-temperature reaction equipment, adding a phosphorus source, heating to 200-300 ℃, reacting for 2-8 hours, and naturally cooling to room temperature to obtain Cu3P nanowire bundles. Wherein the phosphorus source is any one or the combination of at least two of diammonium hydrogen phosphate, sodium hypophosphite and phosphine; the mass ratio of the precursor to the phosphorus source is 1:8-1: 20.
According to an exemplary embodiment of the present invention, a transition metal phosphide nanowire bundle is provided. The transition metal phosphide nanowire bundle is prepared by any preparation method. The prepared transition metal phosphide nanowire bundle material has a one-dimensional linear morphology, and the nanowire bundle surface is clean and easy to carry out surface modification.
According to an exemplary embodiment of the present invention, the transition metal phosphide nanowire bundle is provided for application as a negative electrode material, a catalyst, an optical material and a sensing material of a lithium ion battery.
The following examples are provided to further illustrate the advantageous effects of the present invention.
Example 1
1) Accurately weighing 1mmol of analytically pure Cu (SO)4)2 5H2Dissolving O in a mixed solution of N, N-dimethylformamide and ethylene glycol, transferring the mixed solution into a 250mL reactor, magnetically stirring the mixed solution for 25min to form a uniform blue solution, introducing nitrogen into the solution to discharge air in the reactor, and heating the solution to 130 ℃ for 2 hours. After the reaction is finishedAnd naturally cooling to room temperature, centrifugally washing, and drying at 50-80 ℃ under a vacuum condition to obtain the precursor with the shape of the nanowire bundle.
2) Weighing 0.001g of the precursor obtained in the step 1) and putting the precursor into a reaction vessel, adding 0.008g of sodium hypophosphite, putting the precursor and the sodium hypophosphite into high-temperature reaction equipment, heating the mixture to 200 ℃, reacting for 2 hours, and naturally cooling the mixture to room temperature to obtain Cu3P nanowire bundles.
FIG. 1 is an X-ray diffraction (XRD) pattern of the material of example 1, from which it can be seen that the resulting product is phase-pure Cu3P, no other impurities are produced. FIG. 2 is a Scanning Electron Microscope (SEM) image of the material of example 1, and it can be seen that the product is bundles of surface roughened nanoparticles having a diameter of about 300nm and a length of 10-200 μm.
Example 2
The difference from example 1 is that the reaction temperature in step 1) was changed from 130 ℃ to 150 ℃ and the reaction time was changed from 2 hours to 8 hours, and the other conditions were kept the same.
Example 3
The difference from example 1 is that the reactant Cu (SO) in step 1)4)2 5H2O to Cu (NO)3)2 3H2And O, other conditions are kept consistent.
Example 4
The difference from example 1 is that the mass of sodium hypophosphite in step 2) becomes 0.02g, and the other conditions are kept the same.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
(1) a surfactant or a template agent is not introduced in the synthesis process, so that the method is green and environment-friendly, the adopted raw materials are cheap and easy to obtain, the synthesis process is simple and convenient to operate, and the cost is low;
(2) the invention adopts a precursor low-temperature calcination method to synthesize Cu3The P nanowire bundle is only required to be carried out at a low temperature of 200-270 ℃, and can be popularized to the preparation of other metal phosphide, such as cobalt phosphide, molybdenum phosphide, nickel phosphide and corresponding bimetallic phosphide;
(3) prepared Cu3The P nanowire bundle has a one-dimensional linear shape, and the surface of the nanowire bundle is clean and easy to modify;
(4) cu prepared by the invention3The P nanowire bundle is suitable for being used as a lithium ion battery cathode material, and can also be applied to other fields such as catalysis, optics, sensing and the like.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of transition metal phosphide nanowire bundles is characterized by comprising the following steps:
s1, dissolving transition metal salt in an organic solvent, heating to 100-150 ℃, reacting at a constant temperature, cooling to room temperature, centrifuging, washing and drying to obtain a precursor with the shape of the nanowire bundle;
and S2, mixing the precursor with a phosphorus source, heating to 200-300 ℃, reacting, and cooling to room temperature to obtain the transition metal phosphide nanowire bundle.
2. The method of claim 1, wherein the transition metal phosphide in the transition metal phosphide nanowire bundle is one or more of cobalt phosphide, molybdenum phosphide, nickel phosphide and cuprous phosphide.
3. The method of claim 2, wherein the transition metal phosphide in the bundle of transition metal phosphide nanowires is cuprous phosphide.
4. The method of claim 3, wherein when the transition metal phosphide in the transition metal phosphide nanowire bundle is cuprous phosphide, the transition metal salt is a copper salt, and the copper salt is copper sulfate, copper acetate, copper nitrate or copper chloride;
preferably, the amount of the copper salt substance is 1-5 mmol.
5. The production method according to any one of claims 1 to 4, wherein the organic solvent is a combination comprising any two or at least two of N, N-dimethylformamide, ethylene glycol, ethanol, dimethyl sulfoxide and isopropanol.
6. The method according to any one of claims 1 to 4, wherein the isothermal reaction time in S1 is 2 to 8 hours; the reaction temperature in the S2 is 2-8 hours;
preferably, the reaction temperature in the S2 is 200-270 ℃.
7. The production method according to any one of claims 1 to 4, characterized in that the phosphorus source is one or more selected from the group consisting of diammonium hydrogen phosphate, sodium hypophosphite, and phosphine.
8. The preparation method according to any one of claims 1 to 4, wherein the mass ratio of the precursor to the phosphorus source is 1:8 to 1: 20.
9. Transition metal phosphide nanowire bundles, characterized in that they are produced by the production method according to any one of claims 1 to 8.
10. The transition metal phosphide nanowire bundle as set forth in claim 9, and the application thereof as a negative electrode material, a catalyst, an optical material and a sensing material of a lithium ion battery.
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| US20200254395A1 (en) * | 2017-09-07 | 2020-08-13 | Kabushiki Kaisha Toyota Chuo Kenkyusho | Inorganic structure body, device, and method for manufacturing inorganic structure body |
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