CN111039269A - Preparation method of lithium phosphide powder, lithium phosphide powder and application - Google Patents
Preparation method of lithium phosphide powder, lithium phosphide powder and application Download PDFInfo
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- CN111039269A CN111039269A CN202010054988.5A CN202010054988A CN111039269A CN 111039269 A CN111039269 A CN 111039269A CN 202010054988 A CN202010054988 A CN 202010054988A CN 111039269 A CN111039269 A CN 111039269A
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- lithium
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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
- C01B25/081—Other phosphides of alkali metals, alkaline-earth metals or magnesium
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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
- C01P2002/70—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
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention provides a preparation method of lithium phosphide powder, which comprises the following steps: under the protective atmosphere, adding mixed lithium metal and red phosphorus into a reactor; sealing the reactor; heating the reactor to cause chemical reaction between the lithium metal and the red phosphorus; and taking out the reaction product in the reactor, thereby obtaining the lithium phosphide powder. The preparation method provided by the invention is a one-step calcination method, does not need inert gas protection in the calcination process, can accurately control the stoichiometric ratio of the lithium phosphide powder, and realizes the purpose of preparing high-purity lithium phosphide powder in batches at lower cost.
Description
Technical Field
The invention relates to the technical field of lithium phosphide, and particularly relates to a preparation method of lithium phosphide powder, lithium phosphide powder and application of the lithium phosphide powder.
Background
Lithium phosphide (Li)3P) is a semiconductor material, and has wide application prospect in the field of high-energy and high-frequency semiconductor laser diodes. In addition, since lithium phosphide (Li)3P) has a layered structure with a Li layer sandwiched between two Li layers2Good lithium ion transmission channel is formed between the P layers, so that Li3P has a high lithium ion conductivity. Thus, Li3P is hopeful to be applied to the solid electrolyte of the lithium ion battery.
The existing preparation method of lithium phosphide mainly comprises a ball milling method and a high-temperature calcination method. However, the crystallinity of the lithium phosphide powder prepared by the ball milling method was not good. At present, most of high-temperature calcining methods are multi-step calcining methods, but the method has complex process, needs to complete the processes of material mixing, solid-phase reaction and the like in inert atmosphere and high-temperature environment, has high energy consumption and high danger, is easy to mix impurities, and is not suitable for industrial batch production.
Disclosure of Invention
In view of the above, there is a need for a method for preparing lithium phosphide powder, which is a one-step calcination method, and which does not require inert gas protection during calcination and can precisely control the stoichiometric ratio of lithium phosphide powder, thereby achieving the purpose of batch preparation of high-purity lithium phosphide powder at a low cost.
In addition, it is also necessary to provide a lithium phosphide powder prepared by the preparation method.
In addition, the application of the lithium phosphide powder is also needed to be provided.
The invention provides a preparation method of lithium phosphide powder, which comprises the following steps:
under the protective atmosphere, adding mixed lithium metal and red phosphorus into a reactor;
sealing the reactor;
heating the reactor to cause chemical reaction between the lithium metal and the red phosphorus; and
and taking out the reaction product in the reactor, thereby obtaining the lithium phosphide powder.
The invention also provides an application of the lithium phosphide powder.
The preparation method of the lithium phosphide powder provided by the invention is a one-step calcination method, does not need inert gas protection in the calcination process, can accurately control the stoichiometric ratio of the lithium phosphide powder, and realizes the purpose of batch preparation of high-purity lithium phosphide powder at lower cost.
Drawings
FIG. 1 is a flow chart of a method for preparing lithium phosphide powder in a preferred embodiment of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) image of lithium phosphide powder prepared in the first example of the present invention.
FIG. 3 is an X-ray diffraction (XRD) pattern of the lithium phosphide powder shown in FIG. 2 and the lithium phosphide powder prepared in example two.
FIG. 4 is a Scanning Electron Microscope (SEM) image of lithium phosphide powder prepared in example III of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Referring to fig. 1, a method for preparing lithium phosphide powder according to a preferred embodiment of the present invention includes the following steps:
and step S11, under a protective atmosphere, adding the mixed lithium metal and red phosphorus into the reactor.
In the present embodiment, the mass ratio of the metallic lithium to the red phosphorus is 3: 1. Wherein the metallic lithium includes at least one of lithium powder, lithium particles, lithium flakes, and lithium blocks. The red phosphorus is dried powder.
The protective atmosphere is used to protect the lithium metal from oxidation. The protective atmosphere may be an inert atmosphere. Specifically, the inert atmosphere may include at least one of argon and helium. In this embodiment, the operation of mixing and adding the metallic lithium and the red phosphorus to the reactor may be performed in a glove box. Wherein the glove box is filled with the protective atmosphere.
In this embodiment, the reactor is a stainless steel reactor.
Step S12, the reactor is sealed.
Specifically, the reactor is screwed and sealed so that it ensures that internal gas does not escape and external air does not enter at high temperatures.
Step S13, heating the reactor to make the lithium metal and the red phosphorus chemically react.
Specifically, the reactor is placed into a muffle furnace or a tubular furnace to be heated to 500-700 ℃, and heat preservation is carried out for 2-12 hours.
Step S14, taking out the reaction product in the reactor, thereby obtaining the lithium phosphide powder.
And taking out the reaction product in the reactor under a protective atmosphere, and grinding the reaction product under the protective atmosphere after taking out the reaction product, thereby obtaining the high-purity lithium phosphide powder.
The present invention is further illustrated by the following examples.
Example one
In the first step, 1.00g of lithium metal powder and 1.49g of red phosphorus powder were mixed in a glove box filled with argon gas, and then charged into a stainless steel reactor having a volume of 5mL, and then tightened and sealed.
And secondly, taking the stainless steel reactor out of the glove box, putting the stainless steel reactor into a muffle furnace, setting the heating rate of the muffle furnace to be 5 ℃/min, heating to 600 ℃, and preserving heat for 8 hours.
And step three, naturally cooling to room temperature after the reaction is finished.
Fourthly, opening the stainless steel reactor in the glove box, taking out a product, and grinding to obtain the lithium phosphide (Li)3P) powder.
Example two
The difference between the second embodiment and the first embodiment is that: in the second step the incubation was carried out for 10 hours.
EXAMPLE III
In the first step, 3.00g of metallic lithium block and 4.47g of red phosphorus powder were mixed in a glove box filled with argon gas, and then charged into a stainless steel reactor having a volume of 15mL, and then tightened and sealed.
And step two, taking the stainless steel reactor out of the glove box, putting the stainless steel reactor into a muffle furnace, setting the heating rate to be 5 ℃/min, heating to 500 ℃, and preserving heat for 1 hour.
And thirdly, taking out the unreacted reactant in the glove box, grinding, putting into the stainless steel reactor, screwing and sealing.
Fourthly, the stainless steel reactor is heated to 600 ℃ again, and the temperature is kept for 8 hours.
And fifthly, naturally cooling to room temperature after the reaction is finished.
Sixthly, opening the stainless steel reactor in the glove box, taking out a product, and grinding to obtain the lithium phosphide (Li)3P) powder.
Referring to fig. 2, the lithium phosphide powder prepared in the first embodiment is granular, and the particle size is 3 to 15 μm.
Referring to fig. 3, fig. 3 shows characteristic diffraction peaks of lithium phosphide, which indicates that the lithium phosphide powder prepared in both the first and second examples was successful and had good crystallinity.
Referring to fig. 4, the lithium phosphide powder prepared in example three is roughly granular in shape.
The invention also provides lithium phosphide powder prepared by the preparation method of the lithium phosphide powder.
The invention also provides an application of the lithium phosphide powder.
The preparation method of the lithium phosphide powder provided by the invention is a one-step calcination method, does not need inert gas protection in the calcination process, can accurately control the stoichiometric ratio of the lithium phosphide powder, and realizes the purpose of batch preparation of high-purity lithium phosphide powder at lower cost.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (10)
1. The preparation method of the lithium phosphide powder is characterized by comprising the following steps of:
under the protective atmosphere, adding mixed lithium metal and red phosphorus into a reactor;
sealing the reactor;
heating the reactor to cause chemical reaction between the lithium metal and the red phosphorus; and
and taking out the reaction product in the reactor, thereby obtaining the lithium phosphide powder.
2. The method of claim 1, wherein the mass ratio of the lithium metal to the red phosphorus is 3: 1.
3. The method of claim 1, wherein heating the reactor comprises heating the reactor to a temperature of 500-700 ℃ and maintaining the temperature for 2-12 hours.
4. The method of claim 1, wherein the removing of the reaction product from the reactor is performed under a protective atmosphere, and further comprising:
grinding the reaction product under the protective atmosphere.
5. The method of claim 1, wherein the lithium metal comprises at least one of lithium powder, lithium particles, lithium flakes, and lithium blocks.
6. The method of claim 1, wherein the red phosphorus is a dried powder.
7. The method of claim 1, wherein the reactor is a stainless steel reactor.
8. The method of claim 1, wherein the protective atmosphere comprises at least one of argon and helium.
9. A lithium phosphide powder prepared by the method for preparing lithium phosphide powder according to any one of claims 1 to 8.
10. Use of the lithium phosphide powder as defined in claim 9.
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| CN202010054988.5A CN111039269A (en) | 2020-01-17 | 2020-01-17 | Preparation method of lithium phosphide powder, lithium phosphide powder and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956020A (en) * | 2022-05-18 | 2022-08-30 | 武汉理工大学 | Li 3 Preparation method of P crystal powder and Li 3 P crystal powder and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950909A (en) * | 2014-04-25 | 2014-07-30 | 云南锡业集团有限责任公司研究设计院 | Preparation method of zinc phosphide |
| CN104627972A (en) * | 2015-01-30 | 2015-05-20 | 浙江工业大学 | Method for preparing lithium phosphate powder |
| JP5932691B2 (en) * | 2013-03-18 | 2016-06-08 | 三井造船株式会社 | Positive electrode material for lithium secondary battery and method for producing the same |
-
2020
- 2020-01-17 CN CN202010054988.5A patent/CN111039269A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5932691B2 (en) * | 2013-03-18 | 2016-06-08 | 三井造船株式会社 | Positive electrode material for lithium secondary battery and method for producing the same |
| CN103950909A (en) * | 2014-04-25 | 2014-07-30 | 云南锡业集团有限责任公司研究设计院 | Preparation method of zinc phosphide |
| CN104627972A (en) * | 2015-01-30 | 2015-05-20 | 浙江工业大学 | Method for preparing lithium phosphate powder |
Non-Patent Citations (1)
| Title |
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| G.BRAUER: "Konstitution von phosphiden,arseniden,antimoniden und wismutiden des lithiums,natriums und kaliums", 《ZEITSCHRIFT FÜR PHYSIKALISCHE CHEMIE》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956020A (en) * | 2022-05-18 | 2022-08-30 | 武汉理工大学 | Li 3 Preparation method of P crystal powder and Li 3 P crystal powder and application thereof |
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