CN105826525A - Copper oxide and activated carbon composite material and preparation method and application thereof - Google Patents

Copper oxide and activated carbon composite material and preparation method and application thereof Download PDF

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Publication number
CN105826525A
CN105826525A CN201610163308.7A CN201610163308A CN105826525A CN 105826525 A CN105826525 A CN 105826525A CN 201610163308 A CN201610163308 A CN 201610163308A CN 105826525 A CN105826525 A CN 105826525A
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China
Prior art keywords
oxide
composite material
activated carbon
absorbent charcoal
lithium ion
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Inventor
赵翰庆
张鼎
李忠
徐守冬
王利芹
刘世斌
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a copper oxide and activated carbon composite material and a preparation method and application thereof and belongs to the field of nano material preparation and lithium ion batteries.Activated carbon subjected to acid treatment is added into a copper nitrate aqueous solution according to a certain proportion, the obtained mixture is subjected to low-temperature treatment under the protective atmosphere after severe stirring and drying, and finally the copper oxide and activated carbon composite material is synthesized.The prepared nano-scale copper oxide particles are evenly loaded in the surface and channels of the activated carbon and serve as the cathode material of the lithium ion batteries, good electrochemical performance is shown, the method is simple in synthesis process, and large-scale production is easy.

Description

A kind of Cu oxide/absorbent charcoal composite material and its preparation method and application
Technical field
The present invention relates to a kind of Cu oxide/absorbent charcoal composite material and its preparation method and application, belong to nano material preparation and field of lithium ion battery.
Background technology
In order to meet the lithium ion battery application demand in the extensive energy storage such as electric automobile, intelligent grid, exploitation specific capacity is high, have extended cycle life, lithium ion battery that safety is good, and research new electrode materials is most important.Industrial, anode material for lithium-ion batteries develops into LiFePO4 from cobalt acid lithium, nickle cobalt lithium manganate, and negative material is still based on various graphite type material at present, and its theoretical capacity only has 372mAh g-1.Additionally, due to the current potential of carbon material negative pole current potential and lithium metal very close to, easily separate out generation dendrite lithium during charging, pierce through barrier film and cause short circuit to explode, cause the biggest potential safety hazard.But being as the research of negative material, other is proved to have higher storage lithium performance such as tinbase, silica-based, metal-oxide negative material.Wherein, transition metal oxide material is due to the physical and chemical performance of its uniqueness, and has possessed higher theoretical specific capacity (500 ~ 1000mAh g-1).France Tarascon et al. (Nature, 2000,407,496) first finds and has carried out the storage characteristic research of transition metal oxide, has caused worldwide research boom (Chem.Soc.Rev., 2010,39,3115-3141).
In transition metal oxide, copper oxide causes the concern of researcher due to its high theoretical capacity, low cost, the advantage such as nontoxic.Large-sized copper oxide particle is owing to occurring bigger volumetric expansion efflorescence occur in charging and discharging lithium battery cyclic process, and then has a strong impact on battery capacity and cyclical stability.Material nano and Surface coating are the effective ways improving the problems referred to above.In the past few years, the method such as chemical reduction method, hydro-thermal method can successfully synthesize the nanoscale copper product that pattern is special, is applied to cathode of lithium battery and shows preferable cyclical stability (ScriptaMater.2007,57,337-340).The method that Feng et al. combines high-temperature process by electronation, has synthesized the micro-nano octahedra granule of CuO, and wherein, the CuO granule of hollow-core construction, in the range of electric current density 0.2C and voltage 0.01-3V, can keep 440mAh g after circulating 50 weeks-1Capacity (J.AlloysCompd.2014,600,162-167).The foliaceous CuO composite graphite alkene nanometer sheet material of zhou et al. synthesis, in the voltage range of 0.005-3V, circulates the capacity (Electrochim.Acta2014,125,615-621) that still can keep 600mAh/g for 50 weeks under the electric current density of 100mA/g.Wu et al. uses metal organic frame to be raw material, has gone out hollow CuO octahedron material with water heat transfer, under the electric current density of 100mA/g, in the voltage range of 0.01-3V, still can keep 470100mAh g after 100 circle circulations-1Capacity (J.Mater.Chem.A, 2013,1,11126-11129).Additionally, the material with carbon element of different structure is also used to be coated with nano oxidized copper product, in order to alleviate the volumetric expansion of circulating battery process in which materials, and the electric conductivity of material can be improved, show cyclical stability and the high rate performance of excellence.But, the materials synthesis complex process that these patterns are special, product small scale, it is more difficult to realize industrialization.
Summary of the invention
It is desirable to provide a kind of synthesis technique is simple, reversible capacity is big, Cu oxide/absorbent charcoal composite material of good cycling stability and preparation method thereof.Present invention also offers the application in lithium ion battery negative material of the Cu oxide/absorbent charcoal composite material.
The invention provides a kind of Cu oxide/absorbent charcoal composite material, be made up of the raw material of following weight proportion:
Copper source: 10-30%
Activated carbon: 70-90%；
Copper source is the one in nitrate trihydrate copper, copper chloride, copper sulphate pentahydrate.
The invention provides the preparation method of above-mentioned Cu oxide/absorbent charcoal composite material, comprise the following steps:
(1), during Jiang Tongyuan is dissolved in deionized water, quickly stirring is allowed to form clear solution；
(2) add activated carbon and stir dipping, being subsequently placed in forced air drying in baking oven；Drying time is 10 ~ 24 hours, and oven temperature is 80 ~ 120 DEG C；
(3) being finally transferred in tube furnace, in protective atmosphere, roasting 2 ~ 10 hours under the conditions of 300 DEG C ~ 500 DEG C, are then cooled to room temperature, and prepare Cu oxide/absorbent charcoal composite material.
The invention provides the application in lithium ion battery negative material of the above-mentioned Cu oxide/absorbent charcoal composite material.
The application in lithium ion battery negative material of the described Cu oxide/absorbent charcoal composite material, comprises the following steps:
(1) Cu oxide/activated carbon of preparation is made electrode slice with acetylene black and binding agent according to proportioning 8:1:1, mix homogeneously；Described binding agent is: any one in Kynoar, polyvinyl alcohol, sodium carboxymethyl cellulose or polyurethane；
(2) electrode slice is formed in glove box button cell, at room temperature measure its charge/discharge cycle characteristics and high rate performance, to check Cu oxide/activated carbon nano composite material as the chemical property of lithium ion battery negative material.
Beneficial effects of the present invention:
1) nanosized copper oxide is uniformly dispersed on activated carbon；
2) negative material prepared by the method has the advantage that excellent performance, and technique is simple, can accomplish scale production, and with short production cycle.
Accompanying drawing explanation
Fig. 1 is the HR-TEM figure of sample prepared under conditions of embodiment 1.
The sample that Fig. 2 is prepared under conditions of embodiment 1,2 is prepared as button cell at 100mA g-1Cycle performance figure under electric current density, in 0.01-3V voltage range.
The sample that Fig. 3 is prepared under conditions of embodiment 1 is prepared as button cell at 100mA g-1Charge-discharge performance figure under electric current density, in 0.01-3V voltage range.
Detailed description of the invention
Further illustrate the present invention below by embodiment, but be not limited to following example.
Embodiment 1:
Preparation molar concentration is the copper nitrate solution 200mL of 0.1mol/L, adds the activated carbon of 5g and stirs dipping, being subsequently placed in forced air drying 12 hours in 100 DEG C of baking ovens.Finally being transferred in tube furnace, in nitrogen atmosphere, roasting 4 hours under the conditions of 350 DEG C, are then cooled to room temperature, and prepare Cu oxide/absorbent charcoal composite material.Its pattern is as shown in Figure 1.
Then Cu oxide/activated carbon and the acetylene black of preparation and binding agent (Kynoar) are mixed homogeneously according to mass ratio 8:1:1 and make electrode slice；Electrode slice is formed in glove box button cell, at room temperature measures its charge/discharge cycle characteristics (voltage 0.01 ~ 3V, electric current density 100mA g-1), to check Cu oxide/activated carbon nano composite material as the chemical property of lithium ion battery negative material.As shown in Figure 2.Illustrating that this embodiment obtains the first discharge specific capacity of sample is 1598.7mAh/g, and charge specific capacity is 699.9mAh/g.When charging cycle to 25 circle, specific discharge capacity is 512.4mAh/g, and charge specific capacity is 506.4mAh/g, and coulombic efficiency reaches 98.8%.Hereafter, the specific capacity of charge and discharge cycles is always stable, and when being recycled to 100 circle, specific discharge capacity is 501.8mAh/g, and charge specific capacity is 495.6mAh/g.Fig. 3 is charge and discharge cycles curve chart, from the 1st circle to the 100th circle, the curve of reduction reaction, has three discharge platforms between 2.0-2.3V, 1.3-1.75V and 0.5-1.0V；The curve of oxidation reaction, only one of which charging platform between 2.0-2.5V.Such electrochemical characteristic further illustrates the material that we are done and has the advantage that Reversible Cycle is good.
Embodiment 2:
Preparation molar concentration is the copper nitrate solution 100mL of 0.2mol/L, adds the activated carbon of 5g and stirs dipping, being subsequently placed in forced air drying 24 hours in 80 DEG C of baking ovens.Finally being transferred in tube furnace, in nitrogen atmosphere, roasting 2 hours under the conditions of 500 DEG C, are then cooled to room temperature, and prepare Cu oxide/absorbent charcoal composite material.
Then Cu oxide/activated carbon and the acetylene black of preparation and binding agent (Kynoar) are mixed homogeneously according to mass ratio 8:1:1 and make electrode slice；Electrode slice is formed in glove box button cell, at room temperature measures its charge/discharge cycle characteristics (voltage 0.01 ~ 3V, electric current density 100mA g-1), to check Cu oxide/activated carbon nano composite material as the chemical property of lithium ion battery negative material, see Fig. 2.The sample obtained for embodiment 2, first discharge specific capacity is 1535.9mAh/g, and charge specific capacity is 661.1mAh/g.When charging cycle to 30 circle, specific discharge capacity is 371mAh/g, and charge specific capacity is 362.2mAh/g, and coulombic efficiency reaches 97.6%.Hereafter, the specific capacity of charge and discharge cycles is always stable, and when being recycled to 100 circle, specific discharge capacity is 350.3mAh/g, and charge specific capacity is 344.4mAh/g.Illustrative material has the advantage that Reversible Cycle is good.
Embodiment 3:
Preparation molar concentration is the copper-bath 200mL of 0.1mol/L, adds the activated carbon of 10g and stirs dipping, being subsequently placed in forced air drying 10 hours in 120 DEG C of baking ovens.Finally being transferred in tube furnace, in nitrogen atmosphere, roasting 4 hours under the conditions of 450 DEG C, are then cooled to room temperature, and prepare Cu oxide/absorbent charcoal composite material.
Then Cu oxide/activated carbon and the acetylene black of preparation and binding agent (polyvinyl alcohol) are mixed homogeneously according to mass ratio 8:1:1 and make electrode slice；Electrode slice is formed in glove box button cell.
Embodiment 4:
Preparation molar concentration is the copper chloride solution 200mL of 0.2mol/L, adds the activated carbon of 3g and stirs dipping, being subsequently placed in forced air drying 24 hours in 100 DEG C of baking ovens.Finally being transferred in tube furnace, in nitrogen atmosphere, roasting 10 hours under the conditions of 300 DEG C, are then cooled to room temperature, and prepare Cu oxide/absorbent charcoal composite material.
Then Cu oxide/activated carbon and the acetylene black of preparation and binding agent (polyvinyl alcohol) are mixed homogeneously according to mass ratio 8:1:1 and make electrode slice；Electrode slice is formed in glove box button cell.

Claims (5)

1. Cu oxide/absorbent charcoal composite material, it is characterised in that: it is made up of the raw material of following weight proportion:
Copper source: 10-30%
Activated carbon: 70-90%；
Copper source is the one in nitrate trihydrate copper, copper chloride, copper sulphate pentahydrate.
2. the preparation method of the Cu oxide/absorbent charcoal composite material described in a claim 1, it is characterised in that: comprise the following steps:
(1), during Jiang Tongyuan is dissolved in deionized water, quickly stirring is allowed to form clear solution；
(2) add activated carbon and stir dipping, being subsequently placed in forced air drying in baking oven；Drying time is 10 ~ 24 hours, and oven temperature is 80 ~ 120 DEG C；
(3) being finally transferred in tube furnace, in protective atmosphere, roasting 2 ~ 10 hours under the conditions of 300 DEG C ~ 500 DEG C, are then cooled to room temperature, and prepare Cu oxide/absorbent charcoal composite material.
3. the application in lithium ion battery negative material of the Cu oxide/absorbent charcoal composite material described in a claim 1.
Cu oxide/the absorbent charcoal composite material the most according to claim 3 application in lithium ion battery negative material, it is characterised in that: comprise the following steps:
(1) Cu oxide/activated carbon of preparation is made electrode slice with acetylene black and binding agent according to proportioning 8:1:1, mix homogeneously；(2) electrode slice is formed in glove box button cell, at room temperature measure its charge/discharge cycle characteristics and high rate performance, to check Cu oxide/activated carbon nano composite material as the chemical property of lithium ion battery negative material.
Cu oxide/the absorbent charcoal composite material the most according to claim 4 application in lithium ion battery negative material, it is characterised in that: described binding agent is: any one in Kynoar, polyvinyl alcohol, sodium carboxymethyl cellulose or polyurethane.
CN201610163308.7A 2016-03-22 2016-03-22 Copper oxide and activated carbon composite material and preparation method and application thereof Pending CN105826525A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106450421A (en) * 2016-08-31 2017-02-22 襄阳艾克特电池科技股份有限公司 Preparation method of lithium copper oxide battery
CN107413329A (en) * 2017-05-12 2017-12-01 中国第汽车股份有限公司 A kind of metal oxide-loaded method for preparation of active carbon

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580525A (en) * 2012-03-21 2012-07-18 河北工业大学 Method for using activated carbon load copper oxide composite catalyst to absorb nitrogenous oxide
CN103227328A (en) * 2012-11-26 2013-07-31 北京理工大学 Cuprous oxide/porous carbon composite material as lithium ion battery cathode material and preparation method thereof
CN104512878A (en) * 2013-09-30 2015-04-15 上海交通大学 Method for generating cubic nano cuprous oxide particles on surface of moulded porous carbon

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580525A (en) * 2012-03-21 2012-07-18 河北工业大学 Method for using activated carbon load copper oxide composite catalyst to absorb nitrogenous oxide
CN103227328A (en) * 2012-11-26 2013-07-31 北京理工大学 Cuprous oxide/porous carbon composite material as lithium ion battery cathode material and preparation method thereof
CN104512878A (en) * 2013-09-30 2015-04-15 上海交通大学 Method for generating cubic nano cuprous oxide particles on surface of moulded porous carbon

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GUOHUA SUN ET AL.: "Physical and electrochemical characterization of CuO-doped activated carbon in ionic liquid", 《ELECTROCHIMICA ACTA》 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106450421A (en) * 2016-08-31 2017-02-22 襄阳艾克特电池科技股份有限公司 Preparation method of lithium copper oxide battery
CN107413329A (en) * 2017-05-12 2017-12-01 中国第汽车股份有限公司 A kind of metal oxide-loaded method for preparation of active carbon

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