CN109326820A - A kind of production method of sulfide electrolyte and positive composite layer - Google Patents
A kind of production method of sulfide electrolyte and positive composite layer Download PDFInfo
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- CN109326820A CN109326820A CN201711243858.0A CN201711243858A CN109326820A CN 109326820 A CN109326820 A CN 109326820A CN 201711243858 A CN201711243858 A CN 201711243858A CN 109326820 A CN109326820 A CN 109326820A
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- composite layer
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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
- 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
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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
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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
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- 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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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention relates to technical field of lithium ion, and in particular to a kind of sulfide electrolyte and the production method of positive composite layer are specifically included: by red phosphorus, iris sulphur is dissolved in alcohol organic solvent, is accelerated reaction under microwave irradiation, is obtained liquid P2S5；Substrate is placed in reactor；Li2S is added in the resulting liquid P2S5 of step 1 and is dissolved in alcohol organic solvent formation source solution；Carrier gas is passed through in reactor, flow is controlled respectively in 300-1200sccm；Pressure is maintained at 10-100mbar；Source solution is sprayed by impulse jet nozzle to evaporation region, pulse frequency 1-10Hz, single pulse injecting time is 4-100ms, obtains lithium ion solid electrolyte P2S5-Li2S and positive composite layer on substrate.The present invention uses microwave irradiation, reacts p and s sufficiently and generates superfine powder, improves Li ionic conductivity, improve battery performance.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of system of sulfide electrolyte and positive composite layer
Make method.
Background technique
Judged according to the raw material nature of three kinds of batteries, monomer specific energy is more than 300Wh/Kg to LiFePO4
It is unable to reach with for lithium titanate battery, only ternary material can reach such requirement at present.It is three kinds of lithiums above
The comparison of battery material system, though ternary battery surmounts other batteries with energy density, its using liquid electrolyte,
There are biggish security risks.The view that lithium battery safety problem is consistent is able to solve for solid electrolyte in the industry.
But the organic electrolyte that traditional lithium battery uses is mainly carbonic ether and ethers, and the organic electrolyte is inflammable and explosive.
To solve safety issue, solid electrolyte is generally used.Sulfide solid electrolyte is the direction for studying solid electrolyte.?
In Japan Patent 2013-238522, using phosphorus, sulphur and Li2S directly react and obtain sulfide electrolyte, but its heating and ultrasound
Method catalytic efficiency it is not high, cause the conductibility of lithium ion not high, about 10-5S/cm.
The production method of existing sulfide electrolyte and positive composite layer has the disadvantage that 1) synthesizing sulfide electrolysis
The phosphorus pentasulfide of matter is severe toxicity；2) synthetic method is mechanical ball mill, can not industrialized production；3) the sulfide electrolyte synthesized
If being easy to produce interface problem using pressing process；4) battery that sulfide electrolyte is done is easy capacity attenuation.
Summary of the invention
In order to solve these problems, the present invention does not use the mechanical attrition method of solid phase, but phosphorus, sulphur and lithium sulfide are dissolved in
Organic solvent is formed a film in positive electrode surface by chemical deposition, greatly reduces interfacial effect in this way, improve battery capacity decaying.
The specific technical solution of the present invention is as follows:
A kind of production method of sulfide electrolyte and positive composite layer, comprising the following steps:
Step 1: by red phosphorus, iris sulphur is dissolved in alcohol organic solvent, under microwave irradiation accelerate reaction to get
To liquid P2S5；
Step 2: substrate is placed in reactor；The substrate is anode pole piece, aluminium flake, the copper to have completed
One of foil is a variety of.
Step 3: by the resulting liquid P of step 12S5Li is added2S is dissolved in alcohol organic solvent and forms source solution；
Carrier gas is passed through in reactor, flow is controlled respectively in 300-1200sccm；Pressure is maintained at 10-100mbar；
The substrate temperature of evaporation region, transportation zones and reactor is kept at 180-210 DEG C, 160-220 DEG C
With 280-850 DEG C；
Step 4: source solution is sprayed by impulse jet nozzle to evaporation region, pulse frequency 1-10Hz, single pulse spray
Penetrating the time is 4-100ms, obtains lithium ion solid electrolyte P on substrate2S5-Li2S and positive composite layer.
Further, in the step 1, the organic solvent includes but is not limited to n-butanol, sec-butyl alcohol, isobutanol, 1-
Amylalcohol, 2- amylalcohol, 3- amylalcohol, isoamyl alcohol, n-hexyl alcohol, n-heptanol, n-octyl alcohol, 2- ethyl -3- (2- ethyl)-hexanol.
Further, in the step 2, wave frequency used by the microwave irradiation is 2450 ± 50MHz.
Further, in the step 4, the pulse frequency of the impulse jet nozzle injection is 5-30Hz, single pulse injection
Time is 1-200ms, and there are three the impulse jet nozzles.
Further, in the step 4, the pulse frequency of impulse jet nozzle injection is 10Hz, and single pulse injecting time is
10-30ms。
Further, in the step 4, the carrier gas is nitrogen or argon gas.
Further, described to obtain lithium ion cell positive each component in step 4 are as follows: P:S=2:5 (w/w), Li2S:
P2S5=75:25 (n/n).
Beneficial effects of the present invention: microwave irradiation uses in the reaction of sulphur and phosphorus, improves reaction efficiency, improves lithium ion
Conductibility.PSE-CVD method is used for positive electrode surface, solves positive electrode and interface problem.Reduce space charge layer.PSE-
The form of the sulfide electrolyte material of CVD method preparation is film, is assembled into cell process without adding bonding agent and conduction
Agent greatly simplifies technique.The present invention does not use the mechanical attrition method of solid phase, but phosphorus, sulphur and lithium sulfide are dissolved in organic solvent,
It is formed a film by chemical deposition in positive electrode surface, greatly reduces interfacial effect in this way.It can simply be made in large quantities using PSE-CVD method
The lithium ion thin film anolyte material of standby each sulfide.Accelerate the reaction of p and s.The anode prepared using PSE-CVD method
Lower with sulfide electrolyte interface resistance, improves battery performance.The present invention uses microwave irradiation, and p and s is made sufficiently to react raw
At superfine powder, Li ionic conductivity is improved to 1.7~3.1 × 10-3S/cm
Detailed description of the invention
Fig. 1 is the flow chart of the embodiment of the present invention 1.
Fig. 2 is the electrode figure of the embodiment of the present invention 2.
Fig. 3 is the battery performance test result figure of the embodiment of the present invention 3.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
It should be understood that in the description of the present invention, the orientation or positional relationship of the instructions such as term "left", "right" is base
In orientation or positional relationship shown in the drawings, it is merely for convenience of the description present invention, rather than requires the present invention must be with specific
Orientation construction and operation, therefore be not considered as limiting the invention.
Embodiment 1:
A kind of production method of sulfide electrolyte and positive composite layer, comprising the following steps:
Step 1: it using n-butanol as solvent, configures P:S=2:5 (w/w), phosphorus (0.289g) and sulphur (0.722g) is incorporated
N-butanol 30ml will mix above and then stir, and be heated to 110 DEG C.Reaction obtains P2S5。
Step 2: placing substrate in reactor, and substrate is anode pole piece (ternary material pole piece)
Step 3: by the resulting liquid P of step 12S5Li is added2S (0.489g) incorporates n-butanol 10ml and is dissolved in alcohol
Class organic solvent forms source solution；
Carrier gas is passed through in reactor, flow is controlled respectively in 1100sccm；Pressure is maintained at 100mbar；
The substrate temperature of evaporation region, transportation zones and reactor is kept at 180-210 DEG C, 160-220 DEG C
With 280-850 DEG C；
Step 4: source solution is sprayed by impulse jet nozzle to evaporation region, pulse frequency 1-10Hz, single pulse spray
Penetrating the time is 4-100ms, obtains lithium ion solid electrolyte and positive composite layer on substrate.
Carrier gas is passed through in reactor, flow is controlled respectively in 1100sccm；Pressure is maintained at 100mbar；
Wherein, pulse frequency 1-10Hz, single pulse injecting time are 4-100ms；
Further, sulfide electrolyte is anode, and the negative electrode materials such as graphite or silicon-carbon are cathode, is assembled into such as Fig. 2
Battery.The pressure of 50-130Mpa (preferably 80-110Mpa) is applied to the two-stage of battery.Measure the performance of battery.
Embodiment 2:
A kind of production method of sulfide electrolyte and positive composite layer, comprising the following steps:
Step 1: it using n-butanol as solvent, configures P:S=2:5 (w/w), phosphorus (0.289g) and sulphur (0.722g) is incorporated
N-butanol 30ml will be mixed above and then be stirred, and be added microwave irradiation 5 minutes.Reaction obtains P2S5。
Other steps are identical as step described in embodiment 1.
Embodiment 3:
Step 1: it using n-butanol as solvent, configures P:S=2:5 (w/w), phosphorus (0.289g) and sulphur (0.722g) is incorporated
N-butanol 30ml will be mixed above and then be stirred, and be added microwave irradiation 10 minutes.Reaction obtains P2S5.
Other steps are identical as step described in embodiment 1.
Embodiment 4
A kind of production method of sulfide electrolyte and positive composite layer, comprising the following steps:
Step 1: it using n-butanol as solvent, configures P:S=2:5 (w/w), phosphorus (0.289g) and sulphur (0.722g) is incorporated
N-butanol 30ml will be mixed above and then be stirred, and be added microwave irradiation 10 minutes, and reaction obtains P2S5；
Step 2: substrate is placed in reactor；The substrate is anode pole piece, aluminium flake, the copper to have completed
One of foil is a variety of.
Step 3: by Li2S (0.489g) incorporates n-butanol 10ml, keeps P2S5:Li2S=25:75 (n/n), by step 1
Resulting liquid P2S5Li is added2S is dissolved in alcohol organic solvent and forms source solution；
Step 4: source solution is sprayed by impulse jet nozzle to evaporation region, pulse frequency 1-10Hz, single pulse spray
Penetrating the time is 4-100ms, obtains lithium ion solid electrolyte P on substrate2S5-Li2S and positive composite layer.
Carrier gas is passed through in reactor, flow is controlled respectively in 1100sccm；Pressure is maintained at 100mbar；
Wherein, pulse frequency 1-10Hz, single pulse injecting time are 4-100ms；
Obtained electrolyte composite layer with a thickness of 100 microns, under 100MPa pressure, compression moulding.Solid after pressurization
10~30 microns of electrolyte layer.
Compare the conduction of gained lithium: embodiment 1, the conduction of gained lithium is 2.0 × 10-5S/cm, embodiment 2, gained lithium
Conduction is 1.8 × 10-3S/cm, the conduction of lithium ion is 2.5 × 10 in embodiment 3-3The lithium ion conduction of S/cm, embodiment 4 is
2.6×10-4S/cm. the lithium-ion-conducting of embodiment 2 and 3 wants high.
Battery performance test carried out to 4 groups of embodiments, embodiment 1 as shown in Figure 3 due to there is no carry out microwave irradiation
Capacity attenuation is quickly.Embodiment 2 and 3 keeps having 90%. very well by 35 circulation volumes and embodiment 4 makes of conventional method
Battery capacity rapid decay.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, therefore, as long as with this
Any modifications, equivalent replacements, and improvements made by description of the invention and accompanying drawing content etc. should be included in protection model of the invention
Within enclosing.
Claims (7)
1. a kind of production method of sulfide electrolyte and positive composite layer, it is characterised in that: the following steps are included:
Step 1: by red phosphorus, iris sulphur is dissolved in alcohol organic solvent, accelerates reaction under microwave irradiation to get liquid is arrived
The P of body shape2S5；
Step 2: substrate is placed in reactor；The substrate is in the anode pole piece, aluminium flake, copper foil to have completed
It is one or more.
Step 3: by the resulting liquid P of step 12S5Li is added2S is dissolved in alcohol organic solvent and forms source solution；
Carrier gas is passed through in reactor, flow is controlled respectively in 300-1200sccm；Pressure is maintained at 10-100mbar；
By the substrate temperature of evaporation region, transportation zones and reactor be kept at 180-210 DEG C, 160-220 DEG C and
280-850℃；
Step 4: source solution is sprayed by impulse jet nozzle to evaporation region, pulse frequency 1-10Hz, when single pulse is sprayed
Between be 4-100ms, obtain lithium ion solid electrolyte P on substrate2S5-Li2S and positive composite layer.
2. the production method of sulfide electrolyte and positive composite layer according to claim 1, it is characterised in that: the step
In rapid one, the organic solvent includes but is not limited to n-butanol, sec-butyl alcohol, isobutanol, 1- amylalcohol, 2- amylalcohol, 3- amylalcohol, isoamyl
Alcohol, n-hexyl alcohol, n-heptanol, n-octyl alcohol, 2- ethyl -3- (2- ethyl)-hexanol.
3. the production method of sulfide electrolyte and positive composite layer according to claim 1, it is characterised in that: the step
In rapid two, wave frequency used by the microwave irradiation is 2450 ± 50MHz.
4. the production method of sulfide electrolyte and positive composite layer according to claim 1, it is characterised in that: the step
In rapid four, the pulse frequency of the impulse jet nozzle injection is 5-30Hz, and single pulse injecting time is 1-200ms, the arteries and veins
It rushes there are three nozzles.
5. the production method of sulfide electrolyte and positive composite layer according to claim 1, it is characterised in that: the step
In rapid four, the pulse frequency of impulse jet nozzle injection is 10Hz, and single pulse injecting time is 10-30ms.
6. the production method of sulfide electrolyte and positive composite layer according to claim 1, it is characterised in that: the step
In rapid four, the carrier gas is nitrogen or argon gas.
7. the production method of sulfide electrolyte and positive composite layer according to claim 1, it is characterised in that: step 4
In, it is described to obtain lithium ion battery solid electrolyte each component are as follows: P:S=2:5 (w/w), Li2S:P2S5=75:25 (n/n).
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| CN201711243858.0A CN109326820B (en) | 2017-11-30 | 2017-11-30 | Method for manufacturing sulfide electrolyte and positive electrode composite layer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212796A (en) * | 2011-05-18 | 2011-10-12 | 浙江大学 | Non-magnetic ions Zn<2+>, Mg<2+> and Al<3+> doped SnO2-based magnetic semiconductor film material and preparation method thereof |
| CN104143656A (en) * | 2014-07-04 | 2014-11-12 | 中南大学 | Method for preparing inorganic solid electrolyte membrane/electrode composite material |
| CN106450440A (en) * | 2016-09-13 | 2017-02-22 | 清华大学 | All-solid-state lithium-ion battery, solid electrolyte compound and preparation method |
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- 2017-11-30 CN CN201711243858.0A patent/CN109326820B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212796A (en) * | 2011-05-18 | 2011-10-12 | 浙江大学 | Non-magnetic ions Zn<2+>, Mg<2+> and Al<3+> doped SnO2-based magnetic semiconductor film material and preparation method thereof |
| CN104143656A (en) * | 2014-07-04 | 2014-11-12 | 中南大学 | Method for preparing inorganic solid electrolyte membrane/electrode composite material |
| CN106450440A (en) * | 2016-09-13 | 2017-02-22 | 清华大学 | All-solid-state lithium-ion battery, solid electrolyte compound and preparation method |
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