CN107170963A - A kind of mechanical metallurgy method preparation method of ternary cathode material of lithium ion battery NCM or NCA - Google Patents
A kind of mechanical metallurgy method preparation method of ternary cathode material of lithium ion battery NCM or NCA Download PDFInfo
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- CN107170963A CN107170963A CN201710249224.XA CN201710249224A CN107170963A CN 107170963 A CN107170963 A CN 107170963A CN 201710249224 A CN201710249224 A CN 201710249224A CN 107170963 A CN107170963 A CN 107170963A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/40—Alloys based on alkali metals
- H01M4/405—Alloys based on lithium
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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 provides a kind of ternary cathode material of lithium ion battery NCM or NCA mechanical metallurgy method preparation method, including following steps：Step（1）:The preparation of presoma：Prepare high-purity nickel powder, high-purity cobalt powder, high-purity manganese powder or high purity aluminum powder, proportionally nickel powder, cobalt powder, manganese powder or aluminium powder are mixed by wet ball grinding, the mixed powder of ball milling to certain particle size is sanded by sand mill, the alloyed powder after sand milling is obtained into spherical alloy powder by spray drying；The pre-oxidation of gained spherical alloy powder is obtained into precursor;Step（2）:The preparation of tertiary cathode material：The precursor of gained is sufficiently mixed with lithium source, sintered under atmospheric condition, the material after sintering is through broken, classification, except NCM the or NCA tertiary cathode materials needed for being obtained after magnetic.The present invention prepares NCM using mechanical alloying drying process with atomizing, and NCA spherical alloy powders, resulting materials Elemental redistribution is uniform, and good product quality is adapted to scale, industrialized production high-tap density tertiary cathode material.
Description
Technical field
The invention belongs to energy storage material and electrochemical field, it is related to a kind of ternary cathode material of lithium ion battery NCM and NCA
Preparation method
Background technology
Lithium ion battery has high energy density, excellent cycle life, memory-less effect, low self-discharge rate because of it
And the advantages of low stain, have become the first choice of electrokinetic cell.In the evolution of lithium ion battery, positive pole material is all the time
Key factor.In recent years, tertiary cathode material NCM, NCA are widely used as the positive electrode of lithium ion battery.NCM, NCA make
It is for the major advantage of anode material for lithium-ion batteries：Discharge platform is more steady, and lithium storage content is high.With technological progress, ternary
Material is increasingly becoming the main product of positive electrode.
Body before current ternary material manufacturer is generally prepared during tertiary cathode material is prepared using coprecipitation technology
Body, often to be used in production ammoniacal liquor do often produced in complexing agent, and production process one ton of tertiary cathode material need generation
35 tons of waste water, the processing of waste water is cumbersome, and cost is higher and there is ammonia nitrogen disclosure risk, and ammonia nitrogen removing device fixes input
Larger, production technology is not environmentally friendly enough, and resulting materials tap density is relatively low.
The content of the invention
In order to overcome the shortcoming of existing technology of preparing, the present invention provide a kind of ternary cathode material of lithium ion battery NCM or
NCA mechanical metallurgy method preparation method, including following steps：
Step（1）:The preparation of presoma：High-purity nickel powder, high-purity cobalt powder, high-purity manganese powder or high purity aluminum powder are prepared, proportionally will
Nickel powder, cobalt powder, manganese powder or aluminium powder are mixed by wet ball grinding, and the mixed powder of ball milling to certain particle size is sanded by sand mill,
Alloyed powder after sand milling is obtained into spherical alloy powder by spray drying；The pre-oxidation of gained spherical alloy powder is obtained into precursor;
Step（2）:The preparation of tertiary cathode material：The precursor of gained is sufficiently mixed with lithium source, burnt under atmospheric condition
Material after knot, sintering is through crushing, being classified, except the subsequent treatment process such as magnetic obtains required NCM or NCA tertiary cathode materials.
Wherein, the purity of high-purity nickel powder, high-purity cobalt powder, high-purity manganese powder or high purity aluminum powder is more than 99.99%.
It is preferred that, the step（1）Middle nickel powder, cobalt powder, manganese powder or aluminium powder are as obtained by Mechanical Method or as obtained by atomization.
It is preferred that, the step（1）Middle nickel powder, cobalt powder, manganese powder or aluminium powder mol ratio are（1-8）：（1-2）:(0.04-3).
It is preferred that, the step（1）In mixed by wet ball grinding, ratio of grinding media to material 4-40：1,200-600 turns of ball milling speed/
Minute, Ball-milling Time 1-60 hours.
It is preferred that, the step（1）Middle use sand mill is ground, and the solid content of slurry is 10%-60%, is sanded and uses
Abrading-ball be a diameter of 0.1-0.5mm zirconiums ball, be sanded time 1-8 hour, the sanding media used for water, dispersant use it is organic
Thing ammonium salt or organic matter titanate esters.
It is preferred that, the step（1）In pass through drying process with atomizing prepare spherical alloy powder, the air intake of spray drying chamber
Temperature is 200-550 DEG C, 80-100 DEG C of air outlet temperature, material solid content 10-60%, and spray disk rotating speed 18000-30000 turns every
Minute.
It is preferred that, the step（1）In NCM or NCA tertiary cathode materials are obtained as the pre- oxygen of spherical alloy powder by obtained by
Precursor, Pre oxidation is 200-800 DEG C, preoxidation time 2-8 hours, 1-5 DEG C/min of programming rate.
It is preferred that, the step（2）In lithium source used be lithium carbonate, lithium hydroxide, lithium nitrate, lithium oxalate, lithium acetate
It is a kind of or several.
It is preferred that, the step（2）In presoma used and lithium source proportioning for calculation in the molar ratio, match as 1：1.02-
1.1。
It is preferred that, the step（2）Middle sintering atmosphere is air or oxygen, and sintering temperature is 400-1050 DEG C, heating
1-5 DEG C of speed/min, sintering time is 10-20 hours, the material natural cooling after sintering, by crushing, classification, except magnetic is obtained
Final products.
The present invention prepares NCM using mechanical alloying-drying process with atomizing, NCA spherical alloy powders, by appropriate pre-
Oxidation processes obtain presoma and then with lithium, and high density tertiary cathode material is prepared by rational sintering process, and traditional
Learn coprecipitation technology to compare, it is not necessary to use ammoniacal liquor, it is not necessary to use substantial amounts of pure water, it is not necessary to strictly control course of reaction,
Technological operation is simpler, environmentally friendly, and resulting materials Elemental redistribution is uniform, and product quality more preferably, and is more suitable for scale, work
Industry metaplasia produces high-tap density tertiary cathode material.
Brief description of the drawings
Fig. 1 be the present invention be embodiment 4 presoma SEM figure；
Fig. 2 be the present invention be embodiment 4 prepare tertiary cathode material NCM811 SEM figure;
Fig. 3 be the present invention be embodiment 4 prepare tertiary cathode material NCM811 product distribution diagram of element;
Fig. 4 be the present invention be embodiment 4 prepare tertiary cathode material NCM811 charging and discharging curve figure;
Fig. 5 be the present invention be embodiment 4 prepare tertiary cathode material NCM811 cycle performance figure;
Fig. 6 be the present invention be embodiment 5 NCA presomas SEM figure;
Fig. 7 be the present invention be embodiment 5 prepare tertiary cathode material NCA SEM figure;
Fig. 8 be the present invention be embodiment 5 prepare tertiary cathode material NCA product distribution diagram of element;
Fig. 9 be the present invention be embodiment 5 prepare tertiary cathode material NCA multiplying power property figure.
Embodiment
Below in conjunction with the accompanying drawings, the preferably embodiment to the present invention is described in further detail：
Embodiment 1
High-purity nickel powder 58.7g, high-purity cobalt powder 58.9g, high-purity manganese powder 54.9g are weighed respectively, proportionally by nickel powder, cobalt powder, manganese
Powder is mixed by wet ball grinding, ratio of grinding media to material 4：1,200 revs/min of ball milling speed, Ball-milling Time 1 hour, by ball milling to certain grain
The mixed powder of degree is sanded by sand mill, and solid content control is 10%, and the abrading-ball used is sanded for a diameter of 0.1mm zirconiums ball, is sanded
1 hour time, the sanding media of use is water, and dispersant is organic matter ammonium salt, and the slurry after sand milling is carried out into spray drying makes
Ball, the EAT of spray drying chamber is 200 DEG C, 80 DEG C of air outlet temperature, material solid content 10%, 18000 turns of spray disk rotating speed
It is per minute, gained spherical alloy powder is pre-oxidized after drying process with atomizing, Pre oxidation is 200 DEG C, and preoxidation time 8 is small
When, 1 DEG C/min of programming rate obtains tertiary cathode material precursor after pre-oxidation.
By gained tertiary cathode material precursor with lithium carbonate in molar ratio 1：0.51 is sufficiently mixed, under the atmosphere of air
Sinter, sintering temperature is 1050 DEG C, 5 DEG C/min of programming rate, sintering time is 10 hours, the material after sintering is through crushing, dividing
Level, except obtaining required tertiary cathode material NCM111 after magnetic.
Embodiment 2
High-purity nickel powder 58.7g, high-purity cobalt powder 23.6g, high-purity manganese powder 32.9g are weighed respectively, proportionally by nickel powder, cobalt powder, manganese
Powder is mixed by wet ball grinding, ratio of grinding media to material 40：1,600 revs/min of ball milling speed, Ball-milling Time 60 hours, by ball milling to necessarily
The mixed powder of granularity is sanded by sand mill, and solid content control is 60%, and the abrading-ball used is sanded for a diameter of 0.5mm zirconiums ball, sand
Time consuming 8 hours, the sanding media of use is water, and dispersant is organic matter titanate esters, and it is dry that the slurry after sand milling is carried out into spraying
Dry pelletizing, the EAT of spray drying chamber is 550 DEG C, 100 DEG C of air outlet temperature, material solid content 60%, spray disk rotating speed
30000 rpms, gained spherical alloy powder is pre-oxidized after drying process with atomizing, Pre oxidation is 800 DEG C, during pre-oxidation
Between 2 hours, 5 DEG C/min of programming rate obtains tertiary cathode material precursor after pre-oxidation；
By gained tertiary cathode material precursor with lithium hydroxide in molar ratio 1：1.1 are sufficiently mixed, and are burnt under the atmosphere of oxygen
Knot, sintering temperature is 400 DEG C, 1 DEG C/min of programming rate, and sintering time is 20 hours, material after sintering through broken, classification,
Except obtaining required tertiary cathode material NCM523 after magnetic.
Embodiment 3
High-purity nickel powder 52.7g, high-purity cobalt powder 17.7g, high-purity manganese powder 16.5g are weighed respectively, proportionally by nickel powder, cobalt powder, manganese
Powder is mixed by wet ball grinding, ratio of grinding media to material 20：1,400 revs/min of ball milling speed, Ball-milling Time 30 hours, by ball milling to necessarily
The mixed powder of granularity is sanded by sand mill, and solid content control is 40%, and the abrading-ball used is sanded for a diameter of 0.2mm zirconiums ball, sand
Time consuming 4 hours, the sanding media of use is water, and dispersant is organic matter titanate esters, and it is dry that the slurry after sand milling is carried out into spraying
Dry pelletizing, the EAT of spray drying chamber is 300 DEG C, 90 DEG C of air outlet temperature, material solid content 40%, spray disk rotating speed
25000 rpms, gained spherical alloy powder is pre-oxidized after drying process with atomizing, Pre oxidation is 500 DEG C, during pre-oxidation
Between 5 hours, 2 DEG C/min of programming rate obtains tertiary cathode material precursor after pre-oxidation；
By gained tertiary cathode material precursor with lithium carbonate in molar ratio 1：0.53 is sufficiently mixed, and is burnt under the atmosphere of air
Knot, sintering temperature is 900 DEG C, 3 DEG C/min of programming rate, and sintering time is 15 hours, material after sintering through broken, classification,
Except obtaining required tertiary cathode material NCM622 after magnetic.
Embodiment 4
High-purity nickel powder 234.4g, high-purity cobalt powder 29.5g, high-purity manganese powder 27.5 are weighed respectively, proportionally by nickel powder, cobalt powder, manganese
Powder is mixed by wet ball grinding, ratio of grinding media to material 10：1,300 revs/min of ball milling speed, Ball-milling Time 20 hours, by ball milling to necessarily
The mixed powder of granularity is sanded by sand mill, and solid content control is 30%, and the abrading-ball used is sanded for a diameter of 0.3mm zirconiums ball, sand
Time consuming 5 hours, the sanding media of use is water, and dispersant is organic matter ammonium salt, and the slurry after sand milling is spray-dried
Pelletizing, the EAT of spray drying chamber is 350 DEG C, 85 DEG C of air outlet temperature, material solid content 30%, spray disk rotating speed 20000
Rpm, gained spherical alloy powder is pre-oxidized after drying process with atomizing, Pre oxidation is 600 DEG C, and preoxidation time 4 is small
When, 4 DEG C/min of programming rate obtains tertiary cathode material precursor after pre-oxidation；
By gained tertiary cathode material precursor with lithium oxalate in molar ratio 1：0.54 is sufficiently mixed, and is burnt under the atmosphere of air
Knot, sintering temperature is 800 DEG C, 2 DEG C/min of programming rate, and sintering time is 18 hours, material after sintering through broken, classification,
Except obtaining required tertiary cathode material NCM811 after magnetic.
Embodiment 5
1mol/L nickel oxalate, 1mol/L cobalt oxalate, 0.3mol/L each 1L of liquor alumini chloridi is prepared respectively, and height is weighed respectively
Pure nickel powder 58.6g, high-purity cobalt powder 58.9g, high-purity manganese powder 8.1g, are proportionally mixed nickel powder, cobalt powder, manganese powder by wet ball grinding
Close, ratio of grinding media to material 25：1,500 revs/min of ball milling speed, Ball-milling Time 50 hours passes through the mixed powder of ball milling to certain particle size
Sand mill is sanded, and solid content control is 50%, and the abrading-ball used is sanded for a diameter of 0.4mm zirconiums ball, 6 hours time is sanded, uses
Sanding media be water, dispersant is organic matter titanate esters, and the slurry after sand milling is carried out into spray drying pelletizing, spray drying chamber
EAT be 400 DEG C, 95 DEG C of air outlet temperature, material solid content 50%, 27000 rpms of spray disk rotating speed, spraying is dry
Gained spherical alloy powder is pre-oxidized after drying process, Pre oxidation is 700 DEG C, preoxidation time 3 hours, 3 DEG C of programming rate/
Minute, tertiary cathode material precursor is obtained after pre-oxidation；
By gained tertiary cathode material precursor with lithium acetate in molar ratio 1：0.54 is sufficiently mixed, and is burnt under the atmosphere of air
Knot, sintering temperature is 950 DEG C, 4 DEG C/min of programming rate, and sintering time is 17 hours, material after sintering through broken, classification,
Except obtaining required tertiary cathode material NCA after magnetic.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (10)
1. the mechanical metallurgy method preparation method of ternary cathode material of lithium ion battery NCM or NCA a kind of, it is characterised in that including
Following steps：
Step（1）:The preparation of presoma：High-purity nickel powder, high-purity cobalt powder, high-purity manganese powder or high purity aluminum powder are prepared, proportionally will
Nickel powder, cobalt powder, manganese powder or aluminium powder are mixed by wet ball grinding, and the mixed powder of ball milling to certain particle size is sanded by sand mill,
Alloyed powder after sand milling is obtained into spherical alloy powder by spray drying；The pre-oxidation of gained spherical alloy powder is obtained into precursor;
Step（2）:The preparation of tertiary cathode material：The precursor of gained is sufficiently mixed with lithium source, burnt under atmospheric condition
Knot, material after sintering is through broken, classification, except NCM the or NCA tertiary cathode materials needed for being obtained after magnetic.
2. preparation method as claimed in claim 1, it is characterised in that the step（1）Middle nickel powder, cobalt powder, manganese powder or aluminium powder
As obtained by Mechanical Method or as obtained by atomization.
3. preparation method as claimed in claim 1, it is characterised in that the step（1）Middle nickel powder, cobalt powder, manganese powder or aluminium powder
Mol ratio is（1-8）：（1-2）:(0.04-3).
4. preparation method as claimed in claim 1, it is characterised in that the step（1）In mixed by wet ball grinding, ball material
Compare 4-40：1,200-600 revs/min of ball milling speed, Ball-milling Time 1-60 hours.
5. preparation method as claimed in claim 1, it is characterised in that the step（1）Middle use sand mill is ground, slurry
The solid content of material is 10%-60%, and the abrading-ball used is sanded for a diameter of 0.1-0.5mm zirconiums ball, time 1-8 hour is sanded, uses
Sanding media be water, dispersant use organic matter ammonium salt or organic matter titanate esters.
6. preparation method as claimed in claim 1, it is characterised in that the step（1）In prepared by drying process with atomizing
Spherical alloy powder, the EAT of spray drying chamber is 200-550 DEG C, 80-100 DEG C of air outlet temperature, material solid content 10-
60%, 18000-30000 rpms of spray disk rotating speed.
7. preparation method as claimed in claim 1, it is characterised in that the step（1）In pass through the spherical alloy powder by obtained by
Pre- oxygen obtains NCM or NCA tertiary cathode material precursors, and Pre oxidation is 200-800 DEG C, and preoxidation time 2-8 hours rises
Warm 1-5 DEG C/min of speed.
8. preparation method as claimed in claim 1, it is characterised in that the step（2）In lithium source used be lithium carbonate, hydrogen
Lithia, lithium nitrate, lithium oxalate, lithium acetate it is a kind of or several.
9. preparation method as claimed in claim 1, it is characterised in that the step（2）In presoma used and lithium source match somebody with somebody
Than for calculation in the molar ratio, matching as 1：1.02-1.1.
10. preparation method as claimed in claim 1, it is characterised in that the step（2）Middle sintering atmosphere is air or oxygen
Gas, sintering temperature is 400-1050 DEG C, 1-5 DEG C of programming rate/min, and sintering time is 10-20 hours, and the material after sintering is certainly
So cooling, by crushing, classification, except magnetic obtains final products.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109786672A (en) * | 2018-12-25 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Preparation method of micron-sized single crystal ternary cathode material |
| CN109817945A (en) * | 2019-02-20 | 2019-05-28 | 惠州亿纬锂能股份有限公司 | A kind of nickelic positive electrode and preparation method thereof |
| CN112960704A (en) * | 2021-02-01 | 2021-06-15 | 福建金山锂科新材料有限公司 | Preparation method of high-voltage lithium nickel manganese oxide positive electrode material |
| CN114464789A (en) * | 2022-01-19 | 2022-05-10 | 华中科技大学 | Energy storage secondary battery layered positive electrode material and preparation method thereof |
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| CN103633308A (en) * | 2013-11-28 | 2014-03-12 | 宁波金和新材料股份有限公司 | Lithium, nickel, cobalt, aluminum and oxygen-rich cathode material and preparation method thereof |
| CN104425814A (en) * | 2013-09-09 | 2015-03-18 | 北京国能电池科技有限公司 | Lithium manganate material and preparation method thereof and lithium ion battery cathode material |
| CN103972495B (en) * | 2014-05-16 | 2016-03-23 | 盐城市新能源化学储能与动力电源研究中心 | A kind of preparation method of lithium ion battery anode material nickel LiMn2O4 |
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| CN104425814A (en) * | 2013-09-09 | 2015-03-18 | 北京国能电池科技有限公司 | Lithium manganate material and preparation method thereof and lithium ion battery cathode material |
| CN103633308A (en) * | 2013-11-28 | 2014-03-12 | 宁波金和新材料股份有限公司 | Lithium, nickel, cobalt, aluminum and oxygen-rich cathode material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109786672A (en) * | 2018-12-25 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Preparation method of micron-sized single crystal ternary cathode material |
| CN109786672B (en) * | 2018-12-25 | 2022-03-04 | 中国电子科技集团公司第十八研究所 | Preparation method of micron-sized single crystal ternary cathode material |
| CN109817945A (en) * | 2019-02-20 | 2019-05-28 | 惠州亿纬锂能股份有限公司 | A kind of nickelic positive electrode and preparation method thereof |
| CN112960704A (en) * | 2021-02-01 | 2021-06-15 | 福建金山锂科新材料有限公司 | Preparation method of high-voltage lithium nickel manganese oxide positive electrode material |
| CN114464789A (en) * | 2022-01-19 | 2022-05-10 | 华中科技大学 | Energy storage secondary battery layered positive electrode material and preparation method thereof |
| CN114464789B (en) * | 2022-01-19 | 2023-03-10 | 华中科技大学 | Energy storage secondary battery layered positive electrode material and preparation method thereof |
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Inventor after: Fang Wanli Inventor after: Yu Wei Inventor after: Xie Haijun Inventor before: Zhang Baoping Inventor before: Fang Wanli Inventor before: Yu Wei Inventor before: Xie Haijun |
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Effective date of registration: 20170922 Address after: Longgang District of Shenzhen City, Guangdong province 518000 Ping Street Fu Tai Road No. 6 Applicant after: Fang Wanli Applicant after: Yu Wei Applicant after: Xie Haijun Address before: Longgang District of Shenzhen City, Guangdong province 518000 Ping Street Fu Tai Road No. 6 Applicant before: Zhang Baoping Applicant before: Fang Wanli Applicant before: Yu Wei Applicant before: Xie Haijun |
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Application publication date: 20170915 |
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