CN110156079A - The preparation method and product of linear copper vanadate negative electrode material and application - Google Patents
The preparation method and product of linear copper vanadate negative electrode material and application Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of linear copper vanadate negative electrode material, and the copper vanadate of hydro-thermal method preparation nanometer threadiness is utilized using copper foil as copper source and substrate, which has biggish specific surface area and conductivity, is further conducive to the chemical property for improving material.First discharge specific capacity is 1500 mAh/g, and specific capacity is 302 mAh/g after 50 circulations.Compared with common composite oxides, cycle life is relatively stable.The preparation process is relatively easy, easy to operate.
Description
Technical field
Invention is related to a kind of preparation method of lithium cell cathode material, more particularly to a kind of linear copper vanadate negative electrode material
Preparation method and products thereof and application.
Background technique
With the development of society, lithium ion battery is concerned.Lithium ion battery be it is ideal in the world at present can
Rechargeable battery, it not only has many advantages, such as that energy density is big, has extended cycle life, memory-less effect and pollution are small.With technology
Progress, lithium ion battery will be widely used in the fields such as electric car, aerospace and biological medicine, therefore, research and development
Power is of great significance with lithium ion battery and associated materials.For power lithium ion battery, key is to mention
High power density and energy density, and what power density and energy density improved is electrode material at all, especially negative electrode material
Improvement.
From the beginning of the nineties in last century, Japanese scientific worker has developed the carbon material of layer structure, and carbon material is most
The early material being studied for people and being applied to lithium ion battery and be commercialized, be still so far everybody concern and the emphasis studied it
One, but there are some defects for carbon negative pole material: it when Battery formation, reacts to form SEI film with electrolyte, leads to disappearing for electrolyte
Consumption and lower coulombic efficiency for the first time；When over-charging of battery, it may form Li dendrite at carbon electrodes precipitating metal lithium and cause
Short circuit causes temperature to increase, battery explosion；In addition, diffusion coefficient of the lithium ion in carbon material is smaller, cause battery real
Existing high current charge-discharge, to limit the application range of lithium ion battery.
Copper vanadate (Cu3V2O8) be a kind of spinel structure composite oxides, it is negative to can also be used as lithium ion battery at present
Pole material passes through conversion and alloying reaction Li with higher+Storage volume.The material is considered a kind of promising
Lithium ion battery negative material.
The present invention provides a kind of preparation method of linear copper vanadate negative electrode material, utilizes hydro-thermal by copper source and substrate of copper foil
Method prepares the copper vanadate of nanometer threadiness, which has biggish specific surface area and conductivity, is further conducive to improve material
Chemical property.The preparation process is relatively easy, easy to operate.
Summary of the invention
To overcome the shortcomings of that copper vanadate chemical property is poor, it is an object of that present invention to provide a kind of linear copper vanadate cathode materials
The preparation method of material.
Another object of the present invention is: providing a kind of linear copper vanadate negative electrode material product that the above method obtains.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention is realized by following proposal: a kind of preparation method of threadiness copper vanadate negative electrode material, feature exist
In the copper vanadate using copper foil as copper source and substrate using hydro-thermal method preparation nanometer threadiness, the specific steps of this method are as follows:
(1) copper foil for shearing 0.1~0.2 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) metavanadate, urea, ammonium fluoride solution and hydrogen peroxide are mixed and is added in reaction kettle, wherein the copper foil reacted, inclined vanadium
The molar ratio of hydrochlorate, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, room temperature item
15~30 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under part, 130~150 DEG C of 3~5 h of reaction；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then use water and ethanol washing for several times, then vacuum drying oven 60~80
DEG C dry 10~15 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 500~700 DEG C of 3~5 h of temperature lower calcination.
The metavanadate is one of ammonium metavanadate and metavanadic acid copper or combinations thereof.
The hydrogen peroxide mass percent is 10%~30%.
The present invention provides a kind of linear copper vanadate negative electrode material, is prepared according to any of the above-described the method.
The present invention provides a kind of linear copper vanadate negative electrode material in lithium ion battery as the application of negative electrode material.
The utility model has the advantages that
The present invention provides a kind of preparation method of linear copper vanadate negative electrode material, utilizes hydro-thermal legal system by copper source and substrate of copper foil
The copper vanadate of standby nanometer threadiness, the material have biggish specific surface area and conductivity, are further conducive to the electricity for improving material
Chemical property.First discharge specific capacity is 1500 mAh/g, and specific capacity is 302 mAh/g after 50 circulations.With it is common
Composite oxides are compared, and cycle life is relatively stable.The preparation process is relatively easy, easy to operate.
Detailed description of the invention
Fig. 1 is embodiment 1Cu3V2O8SEM figure；
Fig. 2 is embodiment 2Cu3V2O8Cycle life figure；
Fig. 3 is embodiment 3Cu3V2O8High rate performance figure.
Specific embodiment
The present invention is described in detail by following specific example, but protection scope of the present invention is not only restricted to these
Examples of implementation.
Embodiment 1
A kind of threadiness copper vanadate negative electrode material, the copper vanadate of hydro-thermal method preparation nanometer threadiness is utilized using copper foil as copper source and substrate,
Specific steps are as follows:
(1) copper foil for shearing 0.1 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) by ammonium metavanadate, urea, ammonium fluoride solution and hydrogen peroxide mix be added reaction kettle in, wherein the copper foil reacted, partially
The molar ratio of ammonium vanadate, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, dioxygen
The mass percent of water is 10%, and 15 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under normal temperature condition, 130 DEG C of reactions 5
h；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then for several times with water and ethanol washing, then do for 80 DEG C of vacuum drying oven
Dry 10 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 500 DEG C of 5 h of temperature lower calcination.Fig. 1 is Cu3V2O8SEM
Figure, material are in the nano wire being made of nano particle, have biggish specific surface area, help to improve the electrochemistry of material
Energy.
Embodiment 2
A kind of threadiness copper vanadate negative electrode material, the specific steps of preparation are as follows:
(1) copper foil for shearing 0.1 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) metavanadic acid copper, urea, ammonium fluoride solution and hydrogen peroxide are mixed and is added in reaction kettle, wherein the copper foil reacted, inclined vanadium
The molar ratio of sour copper, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, hydrogen peroxide
Mass percent be 20%, 30 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under normal temperature condition, 150 DEG C reaction 3
h；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then for several times with water and ethanol washing, then do for 60 DEG C of vacuum drying oven
Dry 15 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 600 DEG C of 5 h of temperature lower calcination.
Fig. 2 is Cu3V2O8Cycle life figure；First discharge specific capacity is 1500 mAh/g, the specific volume after 50 circulations
Amount is 302 mAh/g.Compared with common composite oxides, cycle life is relatively stable.
Embodiment 3
A kind of threadiness copper vanadate negative electrode material, the specific steps of preparation are as follows:
(1) copper foil for shearing 0.2 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) metavanadic acid copper, urea, ammonium fluoride solution and hydrogen peroxide are mixed and is added in reaction kettle, wherein the copper foil reacted, inclined vanadium
The molar ratio of sour copper, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, hydrogen peroxide
Mass percent be 30%, 30 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under normal temperature condition, 150 DEG C reaction 3
h；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then for several times with water and ethanol washing, then do for 60 DEG C of vacuum drying oven
Dry 15 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 700 DEG C of 5 h of temperature lower calcination.
Fig. 3 is the present embodiment Cu3V2O8High rate performance figure, under 100 mA/g current density conditions, averaged discharge specific capacity
About 780 mAh/g, under 200 mA/g current density conditions, averaged discharge specific capacity is about 490 mAh/g, 400 mA/g electric currents
Under density conditions, averaged discharge specific capacity is about 390 mAh/g, under 800 mA/g current density conditions, averaged discharge specific capacity
About 300 mAh/g, under 1600 mA/g current density conditions, averaged discharge specific capacity is about 190 mAh/g, 2000 mA/g electricity
Under the conditions of current density, averaged discharge specific capacity is about 170 mAh/g.Under the conditions of high current density, there is relatively high ratio
Capacity.
Claims (8)
1. a kind of preparation method of threadiness copper vanadate negative electrode material, it is characterised in that utilize hydro-thermal method by copper source and substrate of copper foil
Prepare the copper vanadate of nanometer threadiness, the specific steps of this method are as follows:
(1) copper foil for shearing 0.1~0.2 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) metavanadate, urea, ammonium fluoride solution and hydrogen peroxide are mixed and is added in reaction kettle, wherein the copper foil reacted, inclined vanadium
The molar ratio of hydrochlorate, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, room temperature item
15~30 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under part, 130~150 DEG C of 3~5 h of reaction；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then use water and ethanol washing for several times, then vacuum drying oven 60~80
DEG C dry 10~15 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 500~700 DEG C of 3~5 h of temperature lower calcination.
2. the preparation method of linear copper vanadate negative electrode material according to claim 1, it is characterised in that the metavanadate
For one of ammonium metavanadate and metavanadic acid copper or combinations thereof.
3. a kind of preparation method of linear copper vanadate negative electrode material according to claim 1, it is characterised in that the dioxygen
Water quality percentage is 10%~30%.
4. the preparation method of linear copper vanadate negative electrode material according to any one of the claim 1 to 3, which is characterized in that specific
Step are as follows:
(1) copper foil for shearing 0.1 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) by ammonium metavanadate, urea, ammonium fluoride solution and hydrogen peroxide mix be added reaction kettle in, wherein the copper foil reacted, partially
The molar ratio of ammonium vanadate, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, dioxygen
The mass percent of water is 10%, and 15 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under normal temperature condition, 130 DEG C of reactions 5
h；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then for several times with water and ethanol washing, then do for 80 DEG C of vacuum drying oven
Dry 10 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 500 DEG C of 5 h of temperature lower calcination.
5. the preparation method of linear copper vanadate negative electrode material according to any one of the claim 1 to 3, which is characterized in that specific
Step are as follows:
(1) copper foil for shearing 0.1 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) metavanadic acid copper, urea, ammonium fluoride solution and hydrogen peroxide are mixed and is added in reaction kettle, wherein the copper foil reacted, inclined vanadium
The molar ratio of sour copper, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, hydrogen peroxide
Mass percent be 20%, 30 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under normal temperature condition, 150 DEG C reaction 3
h；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then for several times with water and ethanol washing, then do for 60 DEG C of vacuum drying oven
Dry 15 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 600 DEG C of 5 h of temperature lower calcination.
6. the preparation method of linear copper vanadate negative electrode material according to any one of the claim 1 to 3, which is characterized in that specific
Step are as follows:
(1) copper foil for shearing 0.2 mmol, 1 cm × 1 cm, is cleaned and dried the reactor bottom for being placed on 100 mL；
(2) metavanadic acid copper, urea, ammonium fluoride solution and hydrogen peroxide are mixed and is added in reaction kettle, wherein the copper foil reacted, inclined vanadium
The molar ratio of sour copper, urea and ammonium fluoride is 0.009 mmol:0.006 mmol:0.016 mmol:0.04 mmol, hydrogen peroxide
Mass percent be 30%, 30 min of magnetic agitation, is then transferred in hydrothermal reaction kettle under normal temperature condition, 150 DEG C reaction 3
h；
(3) it is cooled to room temperature, sediment is filtered by vacuum, then for several times with water and ethanol washing, then do for 60 DEG C of vacuum drying oven
Dry 15 h；
(4) above-mentioned sediment is obtained into linear vanadic acid copper product in 700 DEG C of 5 h of temperature lower calcination.
7. a kind of threadiness copper vanadate negative electrode material, it is characterised in that -6 any the methods are prepared according to claim 1.
8. a kind of copper vanadate negative electrode material answering as negative electrode material in lithium ion battery linear according to claim 7
With.
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