CN107162054B - A kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal - Google Patents

A kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal Download PDF

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CN107162054B
CN107162054B CN201710345139.3A CN201710345139A CN107162054B CN 107162054 B CN107162054 B CN 107162054B CN 201710345139 A CN201710345139 A CN 201710345139A CN 107162054 B CN107162054 B CN 107162054B
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nanocrystal
dimensional netted
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CN107162054A (en
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曹丽云
寇领江
黄剑锋
杨军
李嘉胤
吴建鹏
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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
    • C01G31/00—Compounds of vanadium
    • 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
    • C01P2004/30—Particle morphology extending in three dimensions
    • 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
    • C01P2006/80—Compositional purity

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Abstract

The invention discloses a kind of preparation methods of three-dimensional netted ammonium vanadate nanocrystal, comprising the following steps: by NH4VO3It solves homogeneously in ethylene glycol, obtainsConcentration is the NH of 0.01-0.1mol/L4VO3Solution；Using HCl solution by NH4VO3The pH of solution is adjusted to 1-3.5, then reacts 0.5-2h under ultrasound environments, obtains solution A；Solution A is placed in the reaction kettle that liner is politef, and reaction kettle is arranged in homogeneous hydro-thermal reaction, 4-8h is reacted at 160-200 DEG C, obtains suspension in reaction kettle；Suspension is centrifugally separating to obtain powder product, powder product is alternately cleaned using deionized water and dehydrated alcohol, then the product after cleaning is dried, obtains three-dimensional netted NH4V3O8Nanocrystal.The three-dimensional netted NH of this method preparation4V3O8Positive electrode of the nanocrystal as lithium battery has chemical property good, the excellent feature of big high rate performance, and this method simple process, and product chemistry composition is uniform.

Description

A kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, it is related to a kind of three-dimensional netted ammonium vanadate nanocrystal Preparation method.
Background technique
Since human civilization, exploitation, utilization and the storage of energy are just ceased with the life style of the mankind and quality of life breath It is related.The fossil fuel of long-time service increases the greenhouse effects of the earth, exacerbates the deterioration of environment, to the existence ring of the mankind Border constitutes great threat.In order to make full use of natural energy, such as wind energy, tide energy, solar energy, it is desirable to suitable Energy storage device, so secondary cell can be recycled, the medium of the energy can be effectively stored as one kind, is realized Chemical energy and electric energy mutually convert.With the development of secondary cell, lithium ion battery is increasingly becoming now state-of-the-art secondary Battery, have the characteristics that discharge voltage is high, specific energy is big, have extended cycle life, have a safety feature with it is environmentally protective, therefore also claimed For green battery.
China's vanadium resource is abundant, and barium oxide, vanadate and derivative are as a kind of important energy storage material by scientific research Staff widely researches and develops.The NH of layer structure4V3O8Material have be easy to ion insertion and abjection, good conductivity, The advantages that electrochemically stable, while also there is photocatalysis characteristic, electrical conduction performance, Chu Li, the performance for storing up sodium.With LiV3O8Material It compares, due toAnd H+Presence, the NH of layer structure4V3O8The interlamellar spacing of material is expanded, while being also formed point Hydrogen bond in son effectively raises the stability of material, NH4V3O8Material relies on unique structure and electron transport characteristic, may be used also To be applied to super capacitor material, sensor material and nano electron device, there are very extensive application and Research Prospects.
Preparation pure phase NH at present4V3O8Mainly there are the precipitation method, hydro-thermal method, solvent-thermal method and sol-gal process, prepared shape As long as looks have one-dimensional nanometer rods, nanobelt, nano wire and two-dimensional sheet-like morphology, these are effectively mentioned with unique texture material High NH4V3O8Chemical property, but NH4V3O8The three-dimensional netted pattern relevant report of nano material is fewer, three-dimensional netted Pattern compared to low-dimensional materials, the contact area with electrolyte can be promoted, accelerate the transmission speed and electronics of lithium ion Transmission rate.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of three-dimensional netted ammonium vanadate nanocrystal；This method preparation Positive electrode of the three-dimensional netted ammonium vanadate nanocrystal as lithium battery has chemical property good, the excellent spy of big high rate performance Point, and this method simple process, product chemistry composition are uniform.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of this three-dimensional netted ammonium vanadate nanocrystal, comprising the following steps:
Step 1, by NH4VO3It solves homogeneously in ethylene glycol, obtainsConcentration is the NH of 0.01-0.1mol/L4VO3It is molten Liquid；
Step 2, using HCl solution by NH4VO3The pH of solution is adjusted to 1-3.5, then reacts 0.5- under ultrasound environments 2h obtains solution A；
Step 3, solution A is placed in the reaction kettle that liner is politef, and reaction kettle is arranged homogeneous In hydro-thermal reaction, 4-8h is reacted at 160-200 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product the product after cleaning is dried, obtain three-dimensional netted NH4V3O8Nanocrystal.
Further, the features of the present invention also characterized in that:
Wherein the concentration of the ethylene glycol in step 1 is 100%, and is heated to 30-50 DEG C.
Wherein the concentration of HCl solution is 0.1-0.2mol/L in step 2.
Wherein the ultrasonic power under step 2 ultrasound environments is 200-300W.
Wherein the packing ratio of solution A in a kettle is 30-60% in step 3.
Wherein detailed process dry in step 4 is to be dried the product after cleaning under vacuum conditions, dry temperature Degree is 50-80 DEG C, a length of 5-10h when dry.
Wherein drying process is to be dried using electric vacunm drying case.
The beneficial effects of the present invention are: compared with the existing technology, the present invention is using Vltrasonic device auxiliary, ethylene glycol solvent Solvent-thermal method prepares three-dimensional netted NH4V3O8Nanocrystal；Energy can be provided for subsequent chemical reaction in ultrasonic procedure, made Solution rapidly and uniformly mixes；Use 100% ethylene glycol as solvent, in high-pressure sealed reaction kettle, NH4VO3Solution compares Vivaciously, product formation rate is slow, therefore products therefrom NH4V3O8Particle size, pattern be easy to control, while product point It is preferable to dissipate property.
Detailed description of the invention
Fig. 1 is the XRD spectrum of three-dimensional netted ammonium vanadate nanocrystal of the invention；
Fig. 2 is the SEM photograph of three-dimensional netted ammonium vanadate nanocrystal of the invention.
Specific embodiment
The invention will be described in further detail with reference to the accompanying drawing:
The present invention provides a kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal, detailed processes are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 30-50 DEG C, obtain Concentration is the NH of 0.01-0.1mol/L4VO3Solution；
Step 2, using the HCl solution of 0.1-0.2mol/L by NH4VO3The pH of solution is adjusted to 1-3.5, then in 200- 0.5-2h is reacted under the ultrasound environments of 300W, obtains solution A；
Step 3, solution A is placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 30- 60%, and reaction kettle is arranged in homogeneous hydro-thermal reaction, 4-8h is reacted at 160-200 DEG C, is suspended in reaction kettle Liquid；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 5-10h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8Nanometer Crystal, interior electric vacunm drying case is vacuum environment, and temperature is 50-80 DEG C.
From XRD spectrum shown in FIG. 1 it is found that three-dimensional netted NH produced by the present invention4V3O8The good crystallinity of nanocrystal, Purity is high；From SEM photograph shown in Fig. 2 it is found that three-dimensional netted NH produced by the present invention4V3O8Nanocrystal has three-dimensional netted Structure, and structure is more loose.
Specific embodiments of the present invention include:
Embodiment 1
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 30 DEG C, obtainIt is dense Degree is the NH of 0.05mol/L4VO3Solution；
Step 2, using the HCl solution of 0.1mol/L by NH4VO3The pH of solution is adjusted to 3, then in the ultrasonic ring of 300W 2h is reacted under border, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 50%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 6h is reacted at 180 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 8h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 60 DEG C.
Embodiment 2
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 50 DEG C, obtainIt is dense Degree is the NH of 0.03mol/L4VO3Solution；
Step 2, using the HCl solution of 0.1mol/L by NH4VO3The pH of solution is adjusted to 3, then in the ultrasonic ring of 300W 1h is reacted under border, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 60%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 8h is reacted at 160 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 8h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 60 DEG C.
Embodiment 3
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 35 DEG C, obtainIt is dense Degree is the NH of 0.08mol/L4VO3Solution；
Step 2, using the HCl solution of 0.2mol/L by NH4VO3The pH of solution is adjusted to 1, then in the ultrasonic ring of 200W 2h is reacted under border, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 40%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 7h is reacted at 170 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 5h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 50 DEG C.
Embodiment 4
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 40 DEG C, obtainIt is dense Degree is the NH of 0.05mol/L4VO3Solution；
Step 2, using the HCl solution of 0.2mol/L by NH4VO3The pH of solution is adjusted to 2, then in the ultrasonic ring of 200W 1h is reacted under border, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 30%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 4h is reacted at 180 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 10h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 70 DEG C.
Embodiment 5
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 45 DEG C, obtainIt is dense Degree is the NH of 0.01mol/L4VO3Solution；
Step 2, using the HCl solution of 0.2mol/L by NH4VO3The pH of solution is adjusted to 3.5, then in the ultrasound of 300W 1h is reacted under environment, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 50%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 5h is reacted at 200 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 8h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 80 DEG C.
Embodiment 6
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 45 DEG C, obtainIt is dense Degree is the NH of 0.08mol/L4VO3Solution；
Step 2, using the HCl solution of 0.15mol/L by NH4VO3The pH of solution is adjusted to 2.5, then in the ultrasound of 260W 1.5h is reacted under environment, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 45%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 5h is reacted at 170 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 6h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 75 DEG C.
Embodiment 2
Prepare three-dimensional netted ammonium vanadate nanocrystal, detailed process are as follows:
Step 1, by NH4VO3It solves homogeneously in 100% ethylene glycol solvent, and is heated to 35 DEG C, obtainIt is dense Degree is the NH of 0.09mol/L4VO3Solution；
Step 2, using the HCl solution of 0.13mol/L by NH4VO3The pH of solution is adjusted to 2, then in the ultrasonic ring of 230W 0.8h is reacted under border, obtains solution A；
Step 3, solution A being placed in the reaction kettle that liner is politef, the packing ratio in reaction kettle is 55%, And reaction kettle is arranged in homogeneous hydro-thermal reaction, 7.5h is reacted at 190 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleans powder using deionized water and dehydrated alcohol Then product after cleaning is dried 6h in electric vacunm drying case, obtains three-dimensional netted NH by product4V3O8It is nanocrystalline Body, interior electric vacunm drying case is vacuum environment, and temperature is 70 DEG C.

Claims (6)

1. a kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal, which comprises the following steps:
Step 1, by NH4VO3It solves homogeneously in ethylene glycol, obtainsConcentration is the NH of 0.01-0.1mol/L4VO3Solution；Its The concentration of middle ethylene glycol is 100%, and is heated to 30-50 DEG C；
Step 2, using HCl solution by NH4VO3The pH of solution is adjusted to 1-3.5, then reacts 0.5-2h under ultrasound environments, obtains To solution A；
Step 3, solution A is placed in the reaction kettle that liner is politef, and reaction kettle is arranged in homogeneous hydro-thermal In reaction, 4-8h is reacted at 160-200 DEG C, obtains suspension in reaction kettle；
Step 4, suspension is centrifugally separating to obtain powder product, alternately cleaning powder produces using deionized water and dehydrated alcohol Then object the product after cleaning is dried, obtain three-dimensional netted NH4V3O8Nanocrystal.
2. the preparation method of three-dimensional netted ammonium vanadate nanocrystal according to claim 1, which is characterized in that the step The concentration of HCl solution is 0.1-0.2mol/L in 2.
3. the preparation method of three-dimensional netted ammonium vanadate nanocrystal according to any one of claims 1 or 2, feature exist In the ultrasonic power under step 2 ultrasound environments is 200-300W.
4. the preparation method of three-dimensional netted ammonium vanadate nanocrystal according to claim 1, which is characterized in that the step The packing ratio of solution A in a kettle is 30-60% in 3.
5. the preparation method of three-dimensional netted ammonium vanadate nanocrystal according to claim 1, which is characterized in that the step Dry detailed process is to be dried the product after cleaning under vacuum conditions in 4, and drying temperature is 50-80 DEG C, dry Shi Changwei 5-10h.
6. according to claim 1 or the preparation method of three-dimensional netted ammonium vanadate nanocrystal described in 5 any one, feature exist In the drying process is to be dried using electric vacunm drying case.
CN201710345139.3A 2017-05-16 2017-05-16 A kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal Active CN107162054B (en)

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Publication number Priority date Publication date Assignee Title
CN107720822B (en) * 2017-09-15 2019-08-09 陕西科技大学 A kind of preparation method of sea urchin shape anode material for lithium-ion batteries
CN113839020B (en) * 2021-09-16 2024-06-21 陕西理工大学 Sheet (NH)4)2V4O9Preparation method of flexible zinc ion battery electrode material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103700824A (en) * 2013-12-18 2014-04-02 陕西科技大学 Preparation method of sandwiched-layer-shaped NH4V3O8 nanocrystalline
CN103715407A (en) * 2013-12-18 2014-04-09 陕西科技大学 Preparation method of porous structure ammonium vanadate material
CN105932278A (en) * 2016-04-29 2016-09-07 陕西科技大学 Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103700824A (en) * 2013-12-18 2014-04-02 陕西科技大学 Preparation method of sandwiched-layer-shaped NH4V3O8 nanocrystalline
CN103715407A (en) * 2013-12-18 2014-04-09 陕西科技大学 Preparation method of porous structure ammonium vanadate material
CN105932278A (en) * 2016-04-29 2016-09-07 陕西科技大学 Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8

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