CN110071325A - A kind of preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material - Google Patents
A kind of preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material Download PDFInfo
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- CN110071325A CN110071325A CN201910255929.1A CN201910255929A CN110071325A CN 110071325 A CN110071325 A CN 110071325A CN 201910255929 A CN201910255929 A CN 201910255929A CN 110071325 A CN110071325 A CN 110071325A
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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
- H01M10/052—Li-accumulators
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
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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
The present invention proposes a kind of preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material, metallic boron hydrides is placed in the environment of free from admixture reaction to heat and decompose by this method, it realizes the part hydrogen release of metallic boron hydrides, obtains multiphase composition metal-boron-hydrogen compound solid electrolyte material after cooling.The synergistic effect that the In-situ reaction of the remaining metallic boron hydrides of the material use and newly generated metallic boron hydrides generates, makes material integrally have preferably conductivity performance；The solid electrolyte material of this method preparation has wide electrochemical window and preferable electrode compatibility, the stability to cathode is improved using the favorable compatibility of remaining metallic boron hydrides and metal negative electrode, the compatibility to anode is improved using electrochemical stability possessed by newly generated metallic boron hydrides simultaneously, finally substantially enhances the stability and compatibility of electrolyte.
Description
Technical field
The present invention relates to novel energy resource material technology field more particularly to a kind of multiphase composition metal-boron-hydrogen compound solid-states
The preparation method of electrolyte.
Background technique
With a wide range of foundation of the widely available and smart grid of electric car, develops safer and there is more high energy
The secondary cell of metric density is the new challenge of energy storage device.Solid state battery be it is current it is universally recognized, existing cell body can be promoted
It is the technology path of safety and energy density.Solid state battery is high with security performance compared with conventional liquid battery, energy density is big,
The advantages that operating temperature section is wide.And it is typically free of inflammable volatile ingredient, there is no leakage situation, high mechanical strength, resist
The features such as temperature performance is good；Meanwhile composed battery can be well using the metal for being difficult to apply in conventional liquid battery
Cathode, to make battery that there is higher specific energy.
For lithium battery, although such as lithium-germanium-phosphorus-sulphur solid electrolyte possesses preferable ionic conductivity performance, electrification
It is [Adv.Energ.Mater., 6 (8) 1501590] to be improved to learn window；Though and lithium-lanthanum-zirconium-oxygen solid electrolyte have compared with
Good electrochemical window, but it is unstable to lithium anode.These all limit their practical application [Nature, 16 (5)
572]。
It can reach 10 under metallic boron hydrides such as 120 degree of lithium borohydride high temperature-3S cm-1Ionic conductivity, and as solid
State electrolyte is fine to lithium an- ode phasic property, and anti-Li dendrite ability is strong, and the lithium battery assembled is not susceptible to short circuit, to be
One kind having potential solid electrolyte material very much.But since it only has 10 at room temperature-7S cm-1Conductivity limit always
Its application.The method to improve its conductivity is modified to it, such as addition lithium chloride, lithium bromide or lithium iodide lithium halide reduce
Its phase transition temperature is to promote room-temperature conductivity [J.Am.Chem.Soc., 131 (2009) 894.]；By being reacted with decaborane
It further generates new two boron of boron hydride lithium, ten dihydro 12 and promotes conductivity [Chem.Mater, 30 (2) to change structure
386-391].But the conductivity that these methods are formed by solid electrolyte material is respectively less than 10-4S cm-1, it is insufficient for electricity
The requirement in pond.It still needs to find new method to promote its conductivity at room temperature.
For other types secondary cell (such as sode cell, potassium battery, magnesium cell), corresponding metallic boron hydrides
(such as sodium borohydride, potassium borohydride, magnesium borohydride) also all has that ionic conductivity is low, equally urgently finds and promotes it
The method of conductivity at room temperature.
Summary of the invention
It is an object of the invention to propose a kind of preparation of multiphase composition metal-boron-hydrogen compound solid electrolyte material
Multiphase composition metal-boron-hydrogen compound the solid electrolyte material of method, preparation has excellent ionic conductivity and electrification
Learn stability.
In order to achieve the above objectives, the present invention proposes a kind of multiphase composition metal-boron-hydrogen compound solid electrolyte material
Metallic boron hydrides is placed in the environment of free from admixture reaction and heats by preparation method, so that the metallic boron hydrides point
Solution will obtain multinomial composition metal-boron-hydrogen after the metallic boron hydrides cooling after release hydrogen to discharge hydrogen partial
Compounds solid state electrolyte.
Preferably, it is described by the metallic boron hydrides grind into powder be placed in the environment of free from admixture reaction into
Row heating.
Preferably, the environment of the free from admixture reaction is vacuum, hydrogen atmosphere or inert atmosphere.
Preferably, the inert atmosphere includes hydrogen, it is a kind of in argon gas and nitrogen or at least two mixed atmosphere.
Preferably, the metallic boron hydrides includes lithium borohydride, sodium borohydride, potassium borohydride, magnesium borohydride or boron
Calcium hydride.
Preferably, the air pressure of the environment of the free from admixture reaction is less than or equal to 10 megapascal.
Preferably, the metallic boron hydrides is placed in the temperature heated in the environment of the free from admixture reaction is
350℃-550℃。
Preferably, the amount that the metallic boron hydrides decomposes to discharge hydrogen partial is to account for the metal hydroboration
The 30%-70% of total hydrogen content of object.
Compared with prior art, of the invention to be advantageous in that: the solid electrolyte material of this method preparation have compared with
High ionic conductivity and electrochemical stability.Metallic boron hydrides is placed in the environment of free from admixture reaction at heating by this method
Reason is decomposed, and is realized the part hydrogen release of metallic boron hydrides, is obtained multiphase composition metal-boron-hydrogen compound solid-state after cooling
What the In-situ reaction of electrolyte, the remaining metallic boron hydrides of the material use and newly generated metallic boron hydrides generated
Synergistic effect, makes material integrally have preferably conductivity performance；
The solid electrolyte material of this method preparation has wide electrochemical window and preferable electrode compatibility, using surplus
The favorable compatibility of remaining metallic boron hydrides and metal negative electrode improves the stability to cathode, while utilizing newly generated gold
Belong to electrochemical stability possessed by boron hydride to improve the compatibility to anode, finally substantially enhances electrolyte
Stability and compatibility；As material can bear 1mAcm for a long time under 35 degree-2Current density, while can be with a variety of positive electrodes
It forms battery and carries out loop test.
At the same time, this method preparation process is simple, and repeatability is strong, is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is the multiphase of lithium borohydride and different hydrogen release ratios complex lithium-boron-hydrogen compound solid state electrolysis in embodiment 1
Compound sodium-boron-hydrogen compound the solid electrolyte material of the multiphase of sodium borohydride and different hydrogen release ratios in material and embodiment 2
Conductivity vary with temperature the contrast schematic diagram of curve；
Fig. 2 is that lithium borohydride, the Fourier of multiphase complex lithium-boron-hydrogen compound solid electrolyte material are red in embodiment 2
(a), 11B solid state nmr (b) Comparative result schematic diagram outside；
Fig. 3 is that the scanning electron microscope of multiphase composite magnesium-boron-hydrogen compound solid electrolyte material in embodiment 3 is seen
Examine schematic diagram；
Fig. 4 is the electrochemical stability test of the compound potassium-boron-hydrogen compound solid electrolyte material of multiphase in embodiment 4
Result schematic diagram；
Fig. 5 is that the compound sodium-boron-hydrogen compound solid electrolyte material of multiphase is used for sodium symmetrical cycle performance in embodiment 5
Performance, current density 1mAcm-1。
Fig. 6 is that a figure lithium titanate, b figure elemental sulfur, c figure titanium disulfide are respectively positive electrode in embodiment 6, and lithium metal is
The battery charging and discharging curve of negative electrode material.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be made below into
Illustrate to one step.
The present invention proposes a kind of preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material, by metal
Boron hydride is placed in the environment of free from admixture reaction and is heated, so that metallic boron hydrides decomposes to discharge hydrogen partial,
Multinomial composition metal-boron-hydrogen compound solid electrolyte material will be obtained after metallic boron hydrides cooling after release hydrogen.
In the present embodiment, metallic boron hydrides grind into powder is placed in the environment of free from admixture reaction and is added
Heat.
In the present embodiment, the environment of free from admixture reaction is vacuum, hydrogen atmosphere or inert atmosphere.
In the present embodiment, inert atmosphere includes hydrogen, it is a kind of in argon gas and nitrogen or at least two mixed atmosphere.
In the present embodiment, metallic boron hydrides include lithium borohydride, sodium borohydride, potassium borohydride, magnesium borohydride or
Calcium borohydride.
In the present embodiment, the air pressure of the environment of free from admixture reaction is less than or equal to 10 megapascal.
In the present embodiment, it is 350 that metallic boron hydrides is placed in the temperature heated in the environment of free from admixture reaction
℃-550℃。
In the present embodiment, the amount that metallic boron hydrides decomposes to discharge hydrogen partial is account for metallic boron hydrides total
The 30%-70% of hydrogen content.
Further explanation explanation will be made to the present invention by specific embodiment below:
Embodiment 1
It uses mortar grinder at powder in glove box 0.8 gram of lithium borohydride (purity > 95%), is placed in closed container
In.Then closed container is evacuated to vacuum, 450 degree of heat preservations is warming up to 5 degree of heating rate per minute, drug is made to discharge hydrogen
Gas.Monitoring hydrogen burst size reach drug always hydrogeneous quality 38%, begin to cool container.After being cooled to room temperature, by material from
It is taken out in closed container and obtains electrolyte sample at powder with mortar grinder.Above step is repeated, drug hydrogen desorption capacity is reached
To the 43% of lithium borohydride gross mass, two kinds of multiphase complex lithium-boron-hydrogen compound solid electrolyte materials are obtained.
Embodiment 2
It uses mortar grinder at powder in glove box 0.8 gram of sodium borohydride (purity > 95%), is placed in closed container
In.Then closed container is evacuated to vacuum, 520 degree of heat preservations is warming up to 5 degree of heating rate per minute, drug is made to discharge hydrogen
Gas.Monitoring hydrogen burst size reach drug always hydrogeneous quality 40%, begin to cool container.After being cooled to room temperature, by material from
It is taken out in closed container and obtains electrolyte sample at powder with mortar grinder.Above step is repeated, drug hydrogen desorption capacity is reached
To the 45% of lithium borohydride gross mass, the compound sodium-boron-hydrogen compound solid electrolyte material of two kinds of multiphases is obtained.
As shown in Figure 1, being carried out not to a series of obtained multiphase composition metal-boron-hydrogen compound solid electrolyte materials
Ionic conductivity test under synthermal.It can be seen that a series of same isothermal of conductivity performance ratio of prepared electrolytes
Raw material conductivity under degree is higher by three orders of magnitude, and multiphase composition metal-boron-hydrogen compound solid electrolyte material is 35
Degree can reach 10-4S cm-1The order of magnitude.
Embodiment 3
It uses mortar grinder at powder in glove box 0.8 gram of lithium borohydride (purity > 95%), is placed in closed container
In.Then closed container is filled with to the hydrogen of 2 megapascal, 450 degree of heat preservations are warming up to 5 degree of heating rate per minute, make drug
Discharge hydrogen.Monitoring hydrogen burst size reach drug always hydrogeneous quality 40% after, begin to cool container.After being cooled to room temperature,
Material is taken out from closed container and obtains electrolyte sample at powder with mortar grinder.
To the lithium of obtained multiphase complex lithium-boron-hydrogen compound solid electrolyte material, raw material lithium borohydride and synthesis
Two boron, ten dihydro 12 carries out Fourier's infrared test and the test of 11 boron solid state nmrs, and test results are shown in figure 2；
Can see after hydrogen release from Fourier's infrared test result in Fig. 2 has two boron of lithium, ten dihydro in lithium borohydride drug
12 and remaining lithium borohydride.It can see two boron of lithium, ten dihydro generated from 11 boron solid state nmr test results
12 is different with two boron of lithium, ten dihydro 12 of standard, occurs due to its decomposed and with remaining lithium borohydride compound
Effect, makes its 11 boron peak position shift.The above result shows that the lithium borohydride drug after hydrogen release be containing lithium borohydride and
Compound lithium-boron-the hydrogen compound of lithium two boron, ten dihydros, 12 multiphases.
Embodiment 4
It uses mortar grinder at powder in glove box 1 gram of magnesium borohydride (purity > 95%), is placed in closed container.
Then closed container is filled with to the hydrogen of 5 megapascal, 400 degree of heat preservations are warming up to 5 degree of heating rate per minute, discharge drug
Hydrogen.Monitoring hydrogen burst size reach drug always hydrogeneous quality 50% after, start natural cooling container.After being cooled to room temperature,
Material is taken out from closed container and obtains electrolyte sample at powder with mortar grinder.
Observation test is carried out with scanning electron microscope to prepared electrolyte, observation obtains prepared multiphase
Compound metal-boron-micron-sized the resolution image of hydrogen compound solid electrolyte, test results are shown in figure 3；
It can be seen that the compound magnesium-boron-hydrogen compound of prepared multiphase from the scanning electron microscope image in Fig. 3
Solid electrolyte porosity and looseness, it is easy to form, it is convenient to be come into full contact with positive and negative pole material, interface impedance is reduced, meets and is used as magnesium
The requirement of cell electrolyte.
Embodiment 5
It uses mortar grinder at powder in glove box 0.5 gram of potassium borohydride (purity > 95%), is placed in closed container
In.Then closed container is filled with to the hydrogen of 7 megapascal, 500 degree of heat preservations are warming up to 3 degree of heating rate per minute, make drug
Discharge hydrogen.Monitoring hydrogen burst size reach drug always hydrogeneous quality 60% after, start natural cooling container.It is cooled to room temperature
Afterwards, material is taken out from closed container and obtains electrolyte sample at powder with mortar grinder.
Cyclic voltammetric electro-chemical test is carried out to prepared electrolyte, obtains corresponding cyclic curve.Scanning electricity
Electrode potential range is -0.05V to 4V, and sweep speed is 0.5mV s-1, test results are shown in figure 4；
It can be seen that the compound potassium-boron of prepared multiphase-hydrogen compound solid-state electricity from the cyclic voltammetry curve in Fig. 4
Solution matter electrochemical window can reach 4V, this explanation within this range this solid electrolyte in actual battery applications not
Electrochemical decomposition can occur, meet the requirement as potassium cell electrolyte.
Embodiment 6
It uses mortar grinder at powder in glove box 1.5 grams of sodium borohydrides (purity > 95%), is placed in closed container
In.Then closed container is evacuated to vacuum, 500 degree of heat preservations is warming up to 5 degree of heating rate per minute, drug is made to discharge hydrogen
Gas.Monitoring hydrogen burst size reach drug always hydrogeneous quality 32% after, begin to cool container.After being cooled to room temperature, by material
It is taken out from closed container and obtains electrolyte sample at powder with mortar grinder.
The test of anti-sodium dendrite ability is carried out to the prepared compound sodium-boron-hydrogen compound solid electrolyte material of multiphase,
Using metallic sodium as both sides electrode, the Symmetrical cells of sodium are assembled under 35 degree with 1mA cm-2Electric current carry out charge-discharge test, obtain
To circulation time-voltage pattern, test results are shown in figure 5.
It can be seen that prepared solid electrolyte material in 1mA cm from the anti-sodium dendrite test result of Fig. 5-2Electric current
Under test condition, charge and discharge cycles can be carried out well.Circulation remained to normal charge and discharge after 1000 hours, illustrated prepared
Electrolyte applies to that normal charge and discharge can be carried out in sode cell under high current, largely avoided the hair of battery short circuit situation
It is raw.
Embodiment 7
It uses mortar grinder at powder in glove box 1.2 grams of lithium borohydrides (purity > 95%), is placed in closed container
In.Then it is filled with the hydrogen of 8 megapascal into closed container, 500 degree of heat preservations are warming up to 4 degree of heating rate per minute, make medicine
Product discharge hydrogen.After monitoring hydrogen burst size reaches the 50% of the total hydrogeneous quality of drug, container is begun to cool.It is cooled to room temperature
Afterwards, material is taken out from closed container and obtains electrolyte sample at powder with mortar grinder.
The test of battery performance is carried out, to prepared electrolyte to detect electrolyte to the simultaneous of electrode material
Capacitive is assembled into battery 35 by negative electrode material of lithium metal respectively using lithium titanate, elemental sulfur, titanium disulfide as positive electrode
Degree is lower to carry out charge-discharge test, and test results are shown in figure 5.
It can be seen that from the cell testing results of Fig. 6 when electrolyte is matched from different electrode materials, it can be just
Often work, and battery performance is good, the compatibility for illustrating electrolyte preferably, can be very good in the utilization of practical lithium battery
It plays a role.
Method of the invention has the advantage that compared with current material and technology
The solid electrolyte material ionic conductivity with higher and electrochemical stability of this method preparation.This method will
Metallic boron hydrides is placed in heat treatment under inert atmosphere and carries out decomposing part hydrogen release, obtains multiphase composition metal-boron-after cooling
Hydrogen compound solid electrolyte material.The original of the material use remaining metallic boron hydrides and newly generated metallic boron hydrides
The synergistic effect of the compound generation in position, makes material integrally have preferably conductivity performance；
The solid electrolyte material of this method preparation has wide electrochemical window and preferable electrode compatibility.Using surplus
The favorable compatibility of remaining metallic boron hydrides and metal negative electrode improves the stability to cathode, while utilizing newly generated gold
Belong to electrochemical stability possessed by boron hydride to improve the compatibility to anode, finally substantially enhances electrolyte
Stability and compatibility；As material can bear the current density of 1mAcm-2 for a long time under 35 degree, while can be with a variety of positive electrodes
It forms battery and carries out loop test.
This method preparation process is simple, and repeatability is strong, is suitble to large-scale production.
The above is only a preferred embodiment of the present invention, does not play the role of any restrictions to the present invention.Belonging to any
Those skilled in the art, in the range of not departing from technical solution of the present invention, to the invention discloses technical solution and
Technology contents make the variation such as any type of equivalent replacement or modification, belong to the content without departing from technical solution of the present invention, still
Within belonging to the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material, which is characterized in that by metal
Boron hydride is placed in the environment of free from admixture reaction and is heated, so that the metallic boron hydrides decomposes to discharge part hydrogen
Gas will obtain multinomial composition metal-boron-hydrogen compound solid electrolyte after the metallic boron hydrides cooling after release hydrogen
Material.
2. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 1,
It is characterized in that, is added in the environment that the metallic boron hydrides grind into powder is placed on to the free from admixture reaction
Heat.
3. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 1,
It is characterized in that, the environment of the free from admixture reaction is vacuum, hydrogen atmosphere or inert atmosphere.
4. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 3,
Be characterized in that, the inert atmosphere includes hydrogen, it is a kind of in argon gas and nitrogen or at least two mixed atmosphere.
5. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 1,
It is characterized in that, the metallic boron hydrides includes lithium borohydride, sodium borohydride, potassium borohydride, magnesium borohydride or calcium borohydride.
6. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 1,
It is characterized in that, the air pressure of the environment of the free from admixture reaction is less than or equal to 10 megapascal.
7. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 1,
Be characterized in that, the metallic boron hydrides is placed in the temperature heated in the environment of free from admixture reaction be 350 DEG C-
550℃。
8. the preparation method of multiphase composition metal-boron-hydrogen compound solid electrolyte material according to claim 1,
It is characterized in that, the amount that the metallic boron hydrides decomposes to discharge hydrogen partial is account for the metallic boron hydrides total
The 30%-70% of hydrogen content.
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