CN105552433A - Preparation method for amorphous state sulfide solid electrolyte - Google Patents
Preparation method for amorphous state sulfide solid electrolyte Download PDFInfo
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- CN105552433A CN105552433A CN201510976514.5A CN201510976514A CN105552433A CN 105552433 A CN105552433 A CN 105552433A CN 201510976514 A CN201510976514 A CN 201510976514A CN 105552433 A CN105552433 A CN 105552433A
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- solid electrolyte
- sulfide solid
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/002—Inorganic electrolyte
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- H—ELECTRICITY
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- H01M2300/00—Electrolytes
- H01M2300/0085—Immobilising or gelification of electrolyte
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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
- H01M2300/0088—Composites
- H01M2300/0091—Composites in the form of mixtures
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to the field of a lithium ion battery and specifically to a preparation method for an amorphous state sulfide solid electrolyte. The preparation method for the amorphous state sulfide solid electrolyte is characterized by comprising the following steps of (1) putting metal lithium, elemental sulfur and phosphorus pentasulfide into an anhydrous and oxygen-free sealed container for mixing; and (2) performing mechanical grinding on the mixed raw materials obtained in the step (1) to obtain the amorphous state sulfide solid electrolyte. According to the preparation method, the proportion of lithium to sulfur to phosphorus can be accurately controlled; the problem of a relatively low purity of the product caused by raw material volatilization existing in a high-temperature solid state method is solved; and meanwhile, the preparation method is rich in raw material sources and simple in process; and the high-purity amorphous state sulfide solid electrolyte can be obtained in one step by a ball milling method.
Description
Technical field
The present invention relates to field of lithium ion battery, particularly a kind of preparation method of amorphous state sulfide solid electrolyte.
Background technology
Low energy consumption, eco-friendly new-energy automobile are the directions of future automobile development, and electrokinetic cell is the key factor affecting new-energy automobile performance.The electrokinetic cell of existing new-energy automobile selects liquid organic electrolyte usually, but the easily on fire or blast when improper use, there is larger potential safety hazard.All-solid-state battery uses solid electrolyte, and there is not incendive liquid electrolyte, fail safe significantly improves, and the charge capacity of all-solid-state battery is more simultaneously, power output is also larger.But the ionic conductivity that solid electrolyte is low at present hinders the practicality of all-solid-state battery.
With solid oxide electrolyte, in sulfide solid electrolyte, sulphion radius is comparatively large, less to the constraint of lithium ion, and lithium ion mobility is easy, and conductivity is higher.Document " Alithiumsuperionicconductor, Nat.Mater., 2011,10,682-686. " reports the sulfide solid electrolyte Li prepared for raw material with lithium sulfide, germanium sulfide and phosphorus pentasulfide
10geP
2s
12conductivity at room temperature, up to 1.2 × 10-2S/cm, reaches business level of electrolyte and particularly attracts people's attention.But synthetic method Raw common at present generally adopts lithium sulfide, and lithium sulfide is expensive, easy moisture absorption hydrolysis, have impact on Industrialization Progress.Publication number is that the Chinese patent of CN1937301A discloses " a kind of can be used as sulfide material of lithium ion battery solid electrolyte and preparation method thereof ", multiple lithium source high temperature method is adopted to prepare sulfide solid electrolyte, although can sulfide solid electrolyte be prepared, but high-temperature process causes material crystallization, ionic conductivity lower and increase energy consumption, material volatilization cause product proportioning to be difficult to accurate control.
Summary of the invention
The present invention is in order to make up the defect of prior art, and providing a kind of lithium metal adopting low price to be easy to get is lithium source, is prepared the method for amorphous state sulfide solid electrolyte material by simple mechanical milling method.
The present invention is achieved through the following technical solutions:
The preparation method of amorphous state sulfide solid electrolyte, is characterized in that: mainly comprise the following steps:
(1) a certain proportion of lithium metal, elemental sulfur, phosphorus pentasulfide are dropped in the closed container of anhydrous and oxygen-free and mix;
(2) raw material of mixing in step (1) is carried out mechanical lapping, prepare amorphous state sulfide solid electrolyte.
In step (1), the mol ratio of lithium metal and elemental sulfur is 1.8:1 ~ 3:1.
Preferably, according to the ratio-dependent of end product, in step (1), the mol ratio of lithium metal and elemental sulfur is 2:1.
In step (1), described lithium metal and the mol ratio of phosphorus pentasulfide are 3:1 ~ 8:1.
Preferably, according to Li
3pS
4the ratio-dependent of compound, in step (1), the mol ratio of lithium metal and phosphorus pentasulfide is 6:1.
Preferably, the closed container of step (1) described anhydrous and oxygen-free is the glove box being full of inert gas, described glove box has water scavenging system, because lithium metal chance water or oxygen can react, phosphorus pentasulfide is the easy moisture absorption also, so necessary exclusion of water and oxygen, therefore to operate in an inert atmosphere, commercially available nitrogen or the water content of argon gas own extremely low, simultaneously have water scavenging system in glove box, can ensure not change in Sample Preparation Procedure.
The method of the mechanical lapping described in step (2) comprises ball-milling method and polishing.
Preferably, the method for the mechanical lapping described in step (2) is ball-milling method, and ball-milling method by controlling the process of ratio of grinding media to material and time controling reaction, can be applicable to extensive and automation mechanized operation simultaneously.
In step (2), described ratio of grinding media to material 10:1 ~ 20:1, ratio of grinding media to material is too large, to increase between abrasive media and the idle work loss of impact friction between medium and ball grinder, not only make power consumption increase, output reduction, but also can aggravate the wearing and tearing of ball grinder; If ratio of grinding media to material is too little, the cushioning effect of material increases, and impact grinds effect and will weaken; Rotational speed of ball-mill is 150 ~ 250 revs/min, and rotating speed too low reaction is difficult to completely, and the problem of material sticks to ball grinder easily occurs, and rotating speed too Gao Zeyi aggravates the wearing and tearing of ball grinder, and temperature rise causes side reaction more greatly; Ball-milling Time is 10 ~ 48 hours, and the time is too short, and react insufficient, particle size distribution is uneven; Time is oversize, then affect efficiency, easily introduces impurity.
Preferably, ratio of grinding media to material 18:1 in described step (2), can give full play to the impact grinding effect of medium, improves the ability to work of ball mill; Rotational speed of ball-mill is 200 revs/min, and Ball-milling Time is 24 hours, can ensure that sufficient reacting is complete.
The invention has the beneficial effects as follows: the invention provides a kind of easy method preparing amorphous state sulfide solid electrolyte, accurately can control the ratio of lithium, sulphur, phosphorus, solve high temperature solid-state method Raw to volatilize the problem causing product purity lower, abundant raw material source simultaneously, technique is simple, just can obtain highly purified amorphous state sulfide solid electrolyte by ball-milling method one step.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Accompanying drawing 1 is Li prepared by the embodiment of the present invention 1
3pS
4aC impedance figure;
Accompanying drawing 2 is Li prepared by the embodiment of the present invention 2
8p
2s
9aC impedance figure.
Embodiment
Below by specific embodiments, the present invention is described in further detail, but these embodiments are only to illustrate, do not limit scope of the present invention.
Embodiment 1:
Lithium metal and elemental sulfur, phosphorus pentasulfide are according to the ratio of mol ratio 6:3:1, in the glove box being full of nitrogen, take 0.2333g lithium metal, 0.5333g elemental sulfur and 1.2334g phosphorus pentasulfide, above-mentioned raw materials and 36g zirconia ball are dropped in 100ml zirconia ball grinding jar, takes out from glove box after sealing completely.Then use planetary ball mill ball milling 24 hours under 200 revs/min of conditions, obtain amorphous state sulfide solid electrolyte Li
3pS
4.
Sample is pressed into diameter 15mm, the disk of thickness about 0.5mm, disk is clipped between stainless steel disk, spread upon by epoxide-resin glue on exposed solid electrolyte, standing 10 minutes to be solidified complete.Two ends stainless steel substrates is connected positive pole and negative pole respectively, electrochemical workstation tests AC impedance figure, the conductivity of sulfide solid electrolyte can be calculated according to the impedance of test.
Impedance test results with reference to the accompanying drawings shown in 1, the computing formula by conductivity:
Wherein, σ is electrolytical conductivity (S/cm);
L is the thickness (cm) of electrolyte compressing tablet;
S is the area (cm of electrolyte compressing tablet
2);
R is the resistance value (Ω) that AC impedance figure obtains.
Calculate, conductivityσ ≈ 0.7 × 10
-4s/cm
Embodiment 2:
Lithium metal and elemental sulfur, phosphorus pentasulfide are the ratio of 8:4:1 according to mol ratio, in the glove box being full of argon gas, take 0.2759g lithium metal, 0.6305g elemental sulfur and 1.0936g phosphorus pentasulfide, above-mentioned raw materials and 36g zirconia ball are dropped in 100ml zirconia ball grinding jar, takes out from glove box after sealing completely.Then use planetary ball mill ball milling 24 hours under 200 revs/min of conditions, obtain amorphous state sulfide solid electrolyte Li
8p
2s
9.
Sample is pressed into diameter 15mm, the disk of thickness about 0.5mm, disk is clipped between stainless steel disk, spread upon by epoxide-resin glue on exposed solid electrolyte, standing 10 minutes to be solidified complete.Two ends stainless steel substrates is connected positive pole and negative pole respectively, electrochemical workstation tests AC impedance figure, the conductivity of sulfide solid electrolyte can be calculated according to the impedance of test.
Impedance test results with reference to the accompanying drawings shown in 2, is calculated by the computing formula of conductivity, conductivityσ ≈ 0.7 × 10
-4s/cm.
Embodiment 3:
Lithium metal and elemental sulfur, phosphorus pentasulfide are the ratio of 8:4:1 according to mol ratio, in the glove box being full of nitrogen, take 0.2759g lithium metal, 0.6305g elemental sulfur and 1.0936g phosphorus pentasulfide, above-mentioned raw materials and 36g zirconia ball are dropped in 100ml zirconia ball grinding jar, takes out from glove box after sealing completely.Then use planetary ball mill ball milling 48 hours under 250 revs/min of conditions, obtain amorphous state sulfide solid electrolyte Li
8p
2s
9.
Sample is pressed into diameter 15mm, the disk of thickness about 0.5mm, disk is clipped between stainless steel disk, spread upon by epoxide-resin glue on exposed solid electrolyte, standing 10 minutes to be solidified complete.Two ends stainless steel substrates is connected positive pole and negative pole respectively, electrochemical workstation tests AC impedance figure, the conductivity of sulfide solid electrolyte can be calculated according to the impedance of test.
Experiment obtains impedance test results, is calculated, conductivityσ ≈ 0.6 × 10 by the computing formula of conductivity
-4s/cm.
Embodiment 4:
Lithium metal and elemental sulfur, phosphorus pentasulfide are the ratio of 14:7:3 according to mol ratio, in the glove box being full of argon gas, take 0.1984g lithium metal, 0.4534g elemental sulfur and 1.3482g phosphorus pentasulfide, above-mentioned raw materials and 28g zirconia ball are dropped in 100ml zirconia ball grinding jar, takes out from glove box after sealing completely.Then use planetary ball mill ball milling 24 hours under 250 revs/min of conditions, obtain amorphous state sulfide solid electrolyte Li
4 ~ 5p
2s
7.
Sample is pressed into diameter 15mm, the disk of thickness about 0.5mm, disk is clipped between stainless steel disk, spread upon by epoxide-resin glue on exposed solid electrolyte, standing 10 minutes to be solidified complete.Two ends stainless steel substrates is connected positive pole and negative pole respectively, electrochemical workstation tests AC impedance figure, the conductivity of sulfide solid electrolyte can be calculated according to the impedance of test.
Experiment obtains impedance test results, is calculated, conductivityσ ≈ 0.6 × 10 by the computing formula of conductivity
-4s/cm.
Embodiment 5:
Lithium metal and elemental sulfur, phosphorus pentasulfide are the ratio of 6:2:1 according to mol ratio, in the glove box being full of argon gas, take 0.2561g lithium metal, 0.3902g elemental sulfur and 1.3537g phosphorus pentasulfide, above-mentioned raw materials and 36g zirconia ball are dropped in 100ml zirconia ball grinding jar, takes out from glove box after sealing completely.Then use planetary ball mill ball milling 24 hours under 150 revs/min of conditions, obtain amorphous state sulfide solid electrolyte Li
6p
2s
7.
Sample is pressed into diameter 15mm, the disk of thickness about 0.5mm, disk is clipped between stainless steel disk, spread upon by epoxide-resin glue on exposed solid electrolyte, standing 10 minutes to be solidified complete.Two ends stainless steel substrates is connected positive pole and negative pole respectively, electrochemical workstation tests AC impedance figure, the conductivity of sulfide solid electrolyte can be calculated according to the impedance of test.
Experiment obtains impedance test results, is calculated, conductivityσ ≈ 0.6 × 10 by the computing formula of conductivity
-4s/cm.
Embodiment 6:
Lithium metal and elemental sulfur, phosphorus pentasulfide are the ratio of 6:2:1 according to mol ratio, in the glove box being full of argon gas, take 0.2561g lithium metal, 0.3902g elemental sulfur and 1.3537g phosphorus pentasulfide, above-mentioned raw materials and 25g zirconia ball are dropped in 100ml zirconia ball grinding jar, takes out from glove box after sealing completely.Then use planetary ball mill ball milling 48 hours under 150 revs/min of conditions, obtain amorphous state sulfide solid electrolyte Li
6p
2s
7.
Sample is pressed into diameter 15mm, the disk of thickness about 0.5mm, disk is clipped between stainless steel disk, spread upon by epoxide-resin glue on exposed solid electrolyte, standing 10 minutes to be solidified complete.Two ends stainless steel substrates is connected positive pole and negative pole respectively, electrochemical workstation tests AC impedance figure, the conductivity of sulfide solid electrolyte can be calculated according to the impedance of test.
Experiment obtains impedance test results, is calculated, conductivityσ ≈ 0.6 × 10 by the computing formula of conductivity
-4s/cm.
Claims (10)
1. the preparation method of amorphous state sulfide solid electrolyte, is characterized in that: mainly comprise the following steps:
(1) a certain proportion of lithium metal, elemental sulfur, phosphorus pentasulfide are dropped in the closed container of anhydrous and oxygen-free and mix;
(2) raw material of mixing in step (1) is carried out mechanical lapping, prepare amorphous state sulfide solid electrolyte.
2. the preparation method of amorphous state sulfide solid electrolyte according to claim 1, is characterized in that: in step (1), the mol ratio of lithium metal and elemental sulfur is 1.8:1 ~ 3:1.
3. the preparation method of amorphous state sulfide solid electrolyte according to claim 2, is characterized in that: in step (1), the mol ratio of lithium metal and elemental sulfur is 2:1.
4. the preparation method of amorphous state sulfide solid electrolyte according to claim 1, is characterized in that: in step (1), and described lithium metal and the mol ratio of phosphorus pentasulfide are 3:1 ~ 8:1.
5. the preparation method of amorphous state sulfide solid electrolyte according to claim 4, is characterized in that: in step (1), the mol ratio of lithium metal and phosphorus pentasulfide is 6:1.
6. the preparation method of amorphous state sulfide solid electrolyte according to claim 1, it is characterized in that: the closed container of step (1) described anhydrous and oxygen-free is the glove box being full of inert gas, described glove box has water scavenging system, and described inert atmosphere is nitrogen or argon gas.
7. the preparation method of amorphous state sulfide solid electrolyte according to claim 1, is characterized in that: the method for the mechanical lapping described in step (2) comprises ball-milling method and polishing.
8. the preparation method of the amorphous state sulfide solid electrolyte according to claim 1 or 7, is characterized in that: the method for the mechanical lapping described in step (2) is ball-milling method.
9. the preparation method of amorphous state sulfide solid electrolyte according to claim 1, is characterized in that: in step (2), described ratio of grinding media to material 10:1 ~ 20:1, and rotational speed of ball-mill is 150 ~ 250 revs/min, and Ball-milling Time is 10 ~ 48 hours.
10. the preparation method of the amorphous state sulfide solid electrolyte according to claim 1 or 9, is characterized in that: ratio of grinding media to material 18:1 in described step (2); Rotational speed of ball-mill is 200 revs/min, and Ball-milling Time is 24 hours.
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|---|---|---|---|
| CN201510976514.5A CN105552433A (en) | 2015-12-23 | 2015-12-23 | Preparation method for amorphous state sulfide solid electrolyte |
| PCT/CN2016/085324 WO2017107397A1 (en) | 2015-12-23 | 2016-06-08 | Preparation of amorphous sulfide solid electrolyte |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017107397A1 (en) * | 2015-12-23 | 2017-06-29 | 山东玉皇新能源科技有限公司 | Preparation of amorphous sulfide solid electrolyte |
| CN108336400A (en) * | 2018-05-15 | 2018-07-27 | 北京科技大学 | A kind of preparation method of sulfide solid electrolyte |
| CN110526278A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A method of red mercuric sulfide is synthesized using mechanical attrition method low temperature |
| CN113839086A (en) * | 2021-08-05 | 2021-12-24 | 恒大新能源技术(深圳)有限公司 | Sulfide solid electrolyte, preparation method thereof, solid electrolyte sheet and solid battery |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115838287B (en) * | 2023-02-10 | 2023-06-27 | 中国科学院宁波材料技术与工程研究所 | Method for preparing sulfide electrolyte by multi-step sintering and prepared sulfide electrolyte |
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|---|---|---|---|---|
| JPH11134937A (en) * | 1997-10-31 | 1999-05-21 | Osaka Prefecture | Manufacture of ion conductive sulfide glass, ion conductive sulfide glass, solid-type electrolyte and totally solid-type secondary battery |
| TW200501174A (en) * | 2003-04-24 | 2005-01-01 | Idemitsu Petrochemical Co | Lithium ion-conductive sulfide glass, process for producing glass ceramic, and wholly solid type cell made with the glass ceramic |
| CN103003890A (en) * | 2010-07-22 | 2013-03-27 | 丰田自动车株式会社 | Sulfide solid electrolyte glass, method for producing sulfide solid electrolyte glass, and lithium solid-state battery |
| WO2014176266A1 (en) * | 2013-04-23 | 2014-10-30 | Applied Materials, Inc. | Electrochemical cell with solid and liquid electrolytes |
| CN105098229A (en) * | 2014-05-15 | 2015-11-25 | 丰田自动车株式会社 | Sulfide solid electrolyte material, battery, and method for producing sulfide solid electrolyte material |
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| JP2003208919A (en) * | 2002-01-15 | 2003-07-25 | Idemitsu Petrochem Co Ltd | Manufacturing method of lithium ion conductive sulfide glass and glass ceramics as well as all solid-type battery using same glass ceramics |
| JP2004265685A (en) * | 2003-02-28 | 2004-09-24 | Idemitsu Petrochem Co Ltd | Manufacturing method of lithium ion conductive sulfide glass and glass ceramic and all solid type battery using the glass ceramic |
| JP5680288B2 (en) * | 2008-07-07 | 2015-03-04 | トヨタ自動車株式会社 | Method for producing sulfide solid electrolyte |
| CN105552433A (en) * | 2015-12-23 | 2016-05-04 | 山东玉皇新能源科技有限公司 | Preparation method for amorphous state sulfide solid electrolyte |
-
2015
- 2015-12-23 CN CN201510976514.5A patent/CN105552433A/en active Pending
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- 2016-06-08 WO PCT/CN2016/085324 patent/WO2017107397A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11134937A (en) * | 1997-10-31 | 1999-05-21 | Osaka Prefecture | Manufacture of ion conductive sulfide glass, ion conductive sulfide glass, solid-type electrolyte and totally solid-type secondary battery |
| TW200501174A (en) * | 2003-04-24 | 2005-01-01 | Idemitsu Petrochemical Co | Lithium ion-conductive sulfide glass, process for producing glass ceramic, and wholly solid type cell made with the glass ceramic |
| CN103003890A (en) * | 2010-07-22 | 2013-03-27 | 丰田自动车株式会社 | Sulfide solid electrolyte glass, method for producing sulfide solid electrolyte glass, and lithium solid-state battery |
| WO2014176266A1 (en) * | 2013-04-23 | 2014-10-30 | Applied Materials, Inc. | Electrochemical cell with solid and liquid electrolytes |
| CN105098229A (en) * | 2014-05-15 | 2015-11-25 | 丰田自动车株式会社 | Sulfide solid electrolyte material, battery, and method for producing sulfide solid electrolyte material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017107397A1 (en) * | 2015-12-23 | 2017-06-29 | 山东玉皇新能源科技有限公司 | Preparation of amorphous sulfide solid electrolyte |
| CN108336400A (en) * | 2018-05-15 | 2018-07-27 | 北京科技大学 | A kind of preparation method of sulfide solid electrolyte |
| CN110526278A (en) * | 2019-08-26 | 2019-12-03 | 浙江工业大学 | A method of red mercuric sulfide is synthesized using mechanical attrition method low temperature |
| CN113839086A (en) * | 2021-08-05 | 2021-12-24 | 恒大新能源技术(深圳)有限公司 | Sulfide solid electrolyte, preparation method thereof, solid electrolyte sheet and solid battery |
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| WO2017107397A1 (en) | 2017-06-29 |
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Application publication date: 20160504 |