CN107381638A - A kind of electric field regulation and control selective freezing synthesis perovskite MgNbO3Magnesium ion battery negative material and preparation method thereof - Google Patents
A kind of electric field regulation and control selective freezing synthesis perovskite MgNbO3Magnesium ion battery negative material and preparation method thereof Download PDFInfo
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- CN107381638A CN107381638A CN201710550876.7A CN201710550876A CN107381638A CN 107381638 A CN107381638 A CN 107381638A CN 201710550876 A CN201710550876 A CN 201710550876A CN 107381638 A CN107381638 A CN 107381638A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/58—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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- 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
- C01P2006/40—Electric properties
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- 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
Abstract
A kind of electric field regulation and control selective freezing synthesis perovskite MgNbO3Magnesium ion battery negative material and preparation method thereof, it is characterized in that：Change the crystallization property with lattice defect crystal using the electric field for applying specific direction in high temperature solid state reaction, grow to form cylindrical shape particle along direction of an electric field；The non-homogeneous crystallization of cylindrical shape particle surface simultaneously and unevenly adhere to sintering aid at the big position of surface curvature radius and part adhesive turns into continuous poriferous pattern；Such pattern advantageously reduces crystal boundary resistance and electromigration resistance；Accelerate the speed of the magnesium ion transfer ability in electrolyte and lattice and redox reaction and there is certain structural rigidity, be that the material volume in charge and discharge process changes to form buffering so as to form high performance Magnesium ion battery negative material.
Description
Technical field
The present invention relates to a kind of high performance calcium titanium ore composite magnesium ion battery cathode material manufacture method technical field.
Background technology
Lithium rechargeable battery have volume, weight energy than it is high, voltage is high, self-discharge rate is low, memory-less effect, circulation
The absolute advantages such as long lifespan, power density height, had more than at present in global portable power source market 30,000,000,000 dollar/year shares and with
Speed more than 10% gradually increases.Particularly in recent years, petering out with fossil energy, solar energy, wind energy, biomass
The new energy such as energy are increasingly becoming the alternative of traditional energy, and wherein wind energy, solar energy has intermittence, to meet lasting electricity
Power supply needs to use substantial amounts of energy-storage battery simultaneously；The urban air-quality problem getting worse that vehicle exhaust is brought, it is electronic
Very urgent stage has been arrived in vigorously advocating and developing for car (EV) or hybrid electric vehicle (HEV)；These demands provide
Lithium ion battery explosive growth point, while higher requirement also is proposed to the performance of lithium ion battery.
The raising of the capacity of lithium ion battery plus-negative plate material be scientific and technical personnel research primary goal, high power capacity both positive and negative polarity
It is high-leveled and difficult to meet high power consumption and high power that the research and development of material can alleviate current Li-ion batteries piles volume big, heavy weight, price
The situation that equipment needs.But since lithium ion battery in 1991 is commercialized, the actual specific capacity of positive electrode is hesitated all the time
Wander between 100-180mAh/g, positive electrode specific capacity is low to have become bottleneck of the lifting lithium ion battery than energy.Compare
In positive pole, the room for promotion of negative material capacity is also very big, such as tin and tin alloy material, silicon and silicon alloy material, all kinds of transition
Metal oxide [Md.Arafat Rahman, Guangsheng Song, Anand I.Bhatt, Yat Choy Wong, and
Cuie Wen, Nanostructured Silicon Anodes for High-Performance Lithium-Ion
Batteries, Adv.Funct.Mater.2016,26,647-678] etc..But high rate performance, circulation such as to take into account material
Capacity retention can be still extremely difficult.Wherein main cause has：1st, electrode material simultaneously will when redox reaction occurs
Conducted with quick Lithium-ion embeding deintercalation and electronics, i.e., there is good electron conduction and ionic conductivity simultaneously, no
Few negative material has higher lithium ion diffusion coefficient, but is electronic body, and the negative material also having is good
Electronic conductor, but lithium ion diffusivity is weak, so that the polarization of battery increases considerably；2nd, many electrode materials are in lithium
Ion has larger Volume Changes during being embedded in deintercalation, so as to cause the broken and active electrode material of electrode material granules
Expect the loss in cyclic process, big Volume Changes also bring material lattice transformation in charge and discharge process to produce the second phase simultaneously
And have a strong impact on the performance of battery.3rd, the lithium cell negative pole material of conversion reaction mechanism, the electronic isolation of reaction product lithium compound
Property has had a strong impact on the invertibity of material.
Because multielectron transfer be present in the lithium cell negative pole material of alloy mechanism and the lithium cell negative pole material of conversion reaction mechanism
Process often shows higher specific capacity, and metal oxide, sulfide, phosphide, carbonate, chloride are as allusion quotation in recent years
The conversion alloy reaction mechanism lithium cell negative pole material of type is gradually of concern.With the work of conventional lithium ion battery electrode material
Principle is different, and traditional lithium ion cell positive and negative pole, which all have lithium ion, can be embedded in or the space of deintercalation, and electric
Solve lithium ion in matter embedded back and forth and deintercalation and " rocking chair " proposed as Armand etc. that discharge between a positive electrode and a negative electrode
Battery.And material is changed by taking+divalent metal oxide as an example, it may occur that similar following change：
2Li++MeO+2e-→Li2O+Me0
And after conversion reaction, it is also possible to the alloy process of diversified forms can occur, such as：
Lim+Me0 n→LimMe0 n
It can be discharged more than 1000mAh.g during the two-1Specific capacity, thus obtain investigation of materials personnel height
The attention of degree.But as it was previously stated, to take into account the high rate performance of material, circulation volume retention property still extremely difficult.Metal oxygen
These conversion negative materials of compound, sulfide, phosphide, carbonate, chloride obtain more research, these conversion alloys
Type negative material is all often single metallization compound.In addition, reserves of the elemental lithium in the earth's crust are very low, rare lithium resource causes
Following lithium ion battery cost constantly rises.Seeking a kind of alternative inexpensive electrochemical energy storing device turns into urgently to be resolved hurrily
The problem of.The electrochemical properties of magnesium are similar with lithium, and earth rich reserves, are to be expected in future substitute most having for lithium ion battery uncommon
The selection of prestige.
As lithium ion transition material, the Magnesium ion battery negative material of alloy mechanism is it can also happen that following electrification
Learn reaction：
Mg2++MeO+2e-→MgO+Me0
Mgm+Me0 n→MgmMe0 n
And larger specific capacity can be discharged, but generally because magnesium ion ionic radius is larger, electrode potential is low,
Migration velocity in electrode material is slow, and the battery performance such as energy density, power density still has very big compared with lithium ion battery
Gap.And the negative pole candidate material of Magnesium ion battery is few, it is studied at present also very inadequate.
Perovskite structure ABO3Type oxide obtains important application in solar cells recently.Its structure is that A positions are
The larger cation of radius, in 12 coordination structures, in the hole being made up of octahedron；B positions are transition metal class
Compared with small cation, octahedral coordination is formed with six oxonium ions.Change A, the element species of B location, A, the element of B location by it
His same valence state or the atomic component of aliovalent state are substituted all there may be different types of lattice defect, so as to as with
The functional material of different functionalities.ABO3Type oxide can carry out alloy reaction when carrying out alloy reaction with two kinds of metals, its
There may be the Alloy solid solution of a variety of phases, due to bimetallic interaction, it is also possible to produce completely different with monometallic
Electrochemical properties, therefore ABO3Type oxide is likely to become a kind of high-performance Magnesium ion battery negative material, and it may be carried
For near or above 300mAh.g-1Specific capacity, magnesium ion enter or abjection material volume change it is also smaller；But the material
Research and development in Magnesium ion battery is substantially at blank.And its subject matter is：1st, ionic conductivity and electronic conductance
Rate is relatively low；2nd, the product magnesia after conversion reaction is electronic body and its magnesium ion Diffusion Activation Energy is also higher, cause compared with
Big activation polarization；3rd, synthesis temperature is higher, easily causes growing up and reuniting for crystal grain.
For these problems, these problems, such as by material can be extenuated to a certain extent by changing the pattern of material
Particle size reduction can reduce the approach of magnesium ion diffusion to the yardstick of nanometer, shorten diffusion time of magnesium ion so as to improve material
Dynamic performance；Too small granularity also easily causes the difficulty of electronic conduction between particle；Reunion between same particle or
Excessive particle easily causes the problems such as infiltration of electrolyte between particles is difficult, and magnesium ion migration velocity is slow.
Therefore it is that perovskite structure oxide is made to develop a kind of perovskite structure oxide with excellent electrochemical performance
For the key of secondary Magnesium ion battery negative material application.
The content of the invention
The present invention proposes a kind of electric field regulation and control selective freezing synthesis perovskite MgNbO for existing background technology3Magnesium from
Sub- cell negative electrode material and preparation method thereof, it is characterized in that：Changed using the electric field for applying specific direction in high temperature solid state reaction
Become the crystallization property with lattice defect crystal, grow to form cylindrical shape particle along direction of an electric field；Cylindrical shape particle simultaneously
The non-homogeneous crystallization on surface unevenly adheres to sintering aid at the big position of surface curvature radius and part adhesive turns into continuous more
Hole pattern；Such pattern advantageously reduces crystal boundary resistance, improves locomitivity of the magnesium ion in lattice；Form continuous electricity
Son migration network, reduces electromigration resistance；Increase and the contact area of electrolyte, accelerate electrolyte and the magnesium ion in lattice
The speed of transfer ability and redox reaction；Such structure also has certain structural rigidity, is in charge and discharge process
Material volume changes to form buffering so as to form high performance Magnesium ion battery negative material.
This electric field regulation and control selective freezing synthesis perovskite MgNbO3Magnesium ion battery negative material, its preparation method are：
Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, the mass ratio of ball milling and material is
20: 1, with 200-400 revs/min of speed ball milling 10-20 hours.By the material after ball milling in tube furnace with 2-10 DEG C/minute
The speed of clock is warming up to after 800-900 DEG C applies a DC voltage, voltage 600-900V, in this temperature at the both ends of tube furnace
30 DEG C are cooled to the furnace after being incubated 3-6 hours under lower and electric field；Material after cooling is ground into 5-15 minutes in mortar, poly-
Tetrafluoroethene agitating paddle is persistently stirred in lower immersion 30 DEG C of lithium metaborate saturated solutions of constant temperature with 900-1200rpm speed, partially
The mass ratio of the quality of lithium borate saturated solution and the material after the cooling immersed is 10: 1, will after persistently stirring 5-10 minutes
Thermostat temperature is reduced to 18-22 DEG C and continues to stir 5-15 minutes, filters thereafter, 5- is dried in 120-160 DEG C of drying box
10 hours.Then dried material is warming up to 450-550 DEG C and herein temperature in tube furnace with 2-10 DEG C/min of speed
Electric field regulation and control selective freezing synthesis perovskite MgNbO is made in degree lower insulation 3-5 hours3Magnesium ion battery negative material.
Compared with prior art, the advantage of the invention is that：Utilize the electricity for applying specific direction in high temperature solid state reaction
Field changes the crystallization property with lattice defect crystal, grows to form cylindrical shape particle along direction of an electric field；Cylindrical shape simultaneously
The non-homogeneous crystallization of particle surface and unevenly adhere to sintering aid at the big position of surface curvature radius and part adhesive turns into
Continuous poriferous pattern；Such pattern advantageously reduces crystal boundary resistance, improves locomitivity of the magnesium ion in lattice；The company of being formed
Continuous electron transfer network, reduce electromigration resistance；Increase and the contact area of electrolyte, accelerate in electrolyte and lattice
The speed of magnesium ion transfer ability and redox reaction；Such structure also has certain structural rigidity, is discharge and recharge
Material volume in journey changes to form buffering so as to form high performance Magnesium ion battery negative material.
Brief description of the drawings
Charging capacity, discharge capacity and the efficiency for charge-discharge figure of preceding 10 circulations of Fig. 1 materials, voltage range 0.1V-
3.0V, charging and discharging currents 0.5C.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1：Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, ball milling
It is 20: 1 with the mass ratio of material, with 400 revs/min of speed ball milling 20 hours.By the material after ball milling in tube furnace with
10 DEG C/min of speed is warming up to after 900 DEG C applies a DC voltage, voltage 900V, in this temperature at the both ends of tube furnace
30 DEG C are cooled to the furnace after being incubated 5 hours under lower and electric field；Material after cooling is ground 12 minutes in mortar, in polytetrafluoro
Ethene agitating paddle is persistently stirred in lower immersion 30 DEG C of lithium metaborate saturated solutions of constant temperature with 1200rpm speed, and lithium metaborate is satisfied
It is 10: 1 with the quality of solution and the mass ratio of the material after the cooling of immersion, after persistently stirring 9 minutes, thermostat temperature is reduced to
22 DEG C and continue stirring 15 minutes, filter thereafter, in 160 DEG C of drying box dry 10 hours.Then by dried material
550 DEG C being warming up to 10 DEG C/min of speed in tube furnace and be incubated 5 hours at this temperature, electric field regulation and control selection is made
Crystallization synthesis perovskite MgNbO3Magnesium ion battery negative material.
Embodiment 2：Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, ball milling
It is 20: 1 with the mass ratio of material, with 400 revs/min of speed ball milling 15 hours.By the material after ball milling in tube furnace with 8
DEG C/min speed be warming up to after 900 DEG C tube furnace both ends apply a DC voltage, voltage 900V, at this temperature
And cool to 30 DEG C with the furnace after under electric field being incubated 5 hours；Material after cooling is ground 12 minutes in mortar, in polytetrafluoroethyl-ne
Alkene agitating paddle is persistently stirred in lower immersion 30 DEG C of lithium metaborate saturated solutions of constant temperature with 1000rpm speed, lithium metaborate saturation
The mass ratio of the quality of solution and the material after the cooling immersed is 10: 1, and after persistently stirring 7 minutes, thermostat temperature is reduced to 20
DEG C and continue stirring 10 minutes, filter thereafter, in 140 DEG C of drying box dry 8 hours.Then by dried material in pipe
500 DEG C being warming up to 8 DEG C/min of speed in formula stove and be incubated 4 hours at this temperature, electric field regulation and control selective freezing is made
Synthesize perovskite MgNbO3Magnesium ion battery negative material.
Embodiment 3：Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, ball milling
It is 20: 1 with the mass ratio of material, with 200 revs/min of speed ball milling 10 hours.By the material after ball milling in tube furnace with 2
DEG C/min speed be warming up to after 800 DEG C tube furnace both ends apply a DC voltage, voltage 600V, at this temperature
And cool to 30 DEG C with the furnace after under electric field being incubated 3 hours；Material after cooling is ground 6 minutes in mortar, in polytetrafluoroethyl-ne
Alkene agitating paddle is persistently stirred in lower immersion 30 DEG C of lithium metaborate saturated solutions of constant temperature with 900rpm speed, and lithium metaborate saturation is molten
The mass ratio of the quality of liquid and the material after the cooling immersed is 10: 1, and after persistently stirring 5 minutes, thermostat temperature is reduced to 18 DEG C
And continue stirring 5 minutes, filter thereafter, dried 5 hours in 120 DEG C of drying box.Then by dried material in tubular type
450 DEG C being warming up to 3 DEG C/min of speed in stove and be incubated 3 hours at this temperature, electric field regulation and control selective freezing conjunction is made
Into perovskite MgNbO3Magnesium ion battery negative material.
Embodiment 4：Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, ball milling
It is 20: 1 with the mass ratio of material, with 300 revs/min of speed ball milling 15 hours.By the material after ball milling in tube furnace with 8
DEG C/min speed be warming up to after 850 DEG C tube furnace both ends apply a DC voltage, voltage 900V, at this temperature
And cool to 30 DEG C with the furnace after under electric field being incubated 6 hours；Material after cooling is ground 15 minutes in mortar, in polytetrafluoroethyl-ne
Alkene agitating paddle is persistently stirred in lower immersion 30 DEG C of lithium metaborate saturated solutions of constant temperature with 1000rpm speed, lithium metaborate saturation
The mass ratio of the quality of solution and the material after the cooling immersed is 10: 1, and after persistently stirring 7 minutes, thermostat temperature is reduced to 18
DEG C and continue stirring 5 minutes, filter thereafter, in 120 DEG C of drying box dry 5 hours.Then by dried material in pipe
520 DEG C being warming up to 8 DEG C/min of speed in formula stove and be incubated 5 hours at this temperature, electric field regulation and control selective freezing is made
Synthesize perovskite MgNbO3Magnesium ion battery negative material.
Embodiment 5：Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, ball milling
It is 20: 1 with the mass ratio of material, with 400 revs/min of speed ball milling 20 hours.By the material after ball milling in tube furnace with 6
DEG C/min speed be warming up to after 850 DEG C tube furnace both ends apply a DC voltage, voltage 800V, at this temperature
And cool to 30 DEG C with the furnace after under electric field being incubated 5 hours；Material after cooling is ground 12 minutes in mortar, in polytetrafluoroethyl-ne
Alkene agitating paddle is persistently stirred in lower immersion 30 DEG C of lithium metaborate saturated solutions of constant temperature with 1100rpm speed, lithium metaborate saturation
The mass ratio of the quality of solution and the material after the cooling immersed is 10: 1, and after persistently stirring 7 minutes, thermostat temperature is reduced to 20
DEG C and continue stirring 12 minutes, filter thereafter, in 150 DEG C of drying box dry 7 hours.Then by dried material in pipe
500 DEG C being warming up to 8 DEG C/min of speed in formula stove and be incubated 5 hours at this temperature, electric field regulation and control selective freezing is made
Synthesize perovskite MgNbO3Magnesium ion battery negative material.
Claims (1)
- A kind of 1. electric field regulation and control selective freezing synthesis perovskite MgNbO3The preparation method of Magnesium ion battery negative material, its feature For：Magnesium nitrate hexahydrate, niobium hydroxide are put into ball mill with the ratio of the amount 1: 1 of material, the quality of ball milling and material Than for 20: 1, with 200-400 revs/min of speed ball milling 10-20 hours；By the material after ball milling in tube furnace with 2-10 DEG C/min speed be warming up to after 800-900 DEG C tube furnace both ends apply a DC voltage, voltage 600-900V, 30 DEG C are cooled to the furnace after being incubated 3-6 hours at a temperature of this and under electric field；Material after cooling is ground to 5-15 points in mortar Clock, it is molten that 30 DEG C of lithium metaborate saturations of constant temperature are immersed in the case where Teflon stir oar is persistently stirred with 900-1200rpm speed In liquid, the mass ratio of the quality of lithium metaborate saturated solution and the material after the cooling immersed is 10: 1, persistently stirs 5-10 points Zhong Hou, thermostat temperature are reduced to 18-22 DEG C and continue to stir 5-15 minutes, filter thereafter, done in 120-160 DEG C of drying box Dry 5-10 hours；Then by dried material in tube furnace with 2-10 DEG C/min of speed be warming up to 450-550 DEG C and Electric field regulation and control selective freezing synthesis perovskite MgNbO is made in insulation 3-5 hours at a temperature of this3Magnesium ion battery negative material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116581234A (en) * | 2023-04-17 | 2023-08-11 | 大连亚泰科技新材料股份有限公司 | Preparation method of magnesium ion battery anode material |
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| CN116581234B (en) * | 2023-04-17 | 2024-02-02 | 大连亚泰科技新材料股份有限公司 | Preparation method of magnesium ion battery anode material |
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