CN108091852A - A kind of molybdenum trioxide coated lithium ion battery positive electrode and preparation method thereof - Google Patents
A kind of molybdenum trioxide coated lithium ion battery positive electrode and preparation method thereof Download PDFInfo
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- CN108091852A CN108091852A CN201711321616.9A CN201711321616A CN108091852A CN 108091852 A CN108091852 A CN 108091852A CN 201711321616 A CN201711321616 A CN 201711321616A CN 108091852 A CN108091852 A CN 108091852A
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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
- H01M4/366—Composites as layered products
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 relates to a kind of molybdenum trioxide coated lithium ion battery positive electrode and preparation method thereof, anode material for lithium-ion batteries of the invention includes composite oxides kernel and clad two parts.Kernel is ternary materials, LiMn2O4, the LiFePO4s such as single or doping vario-property cobalt acid lithium, nickle cobalt lithium manganate or nickel cobalt lithium aluminate etc., and clad is molybdenum trioxide.The process of preparing of anode material for compound lithium ion battery disclosed in this invention is simple, process control, convenient for industrialized production.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical fields, and in particular to a kind of molybdenum trioxide coated lithium ion electricity
Pond positive electrode and preparation method thereof.
Background technology
With greatly developing for new-energy automobile, lithium ion battery industry comes into Rapid development stage.Influence lithium from
The critical material of sub- battery performance mainly has positive electrode, negative material, electrolyte etc..Wherein, positive electrode is to limit at present
The principal element of battery performance, while be also to account for the higher principal element of lithium ion battery cost, close to 40%.
Positive electrode current material mainly has cobalt acid lithium, nickle cobalt lithium manganate or nickel cobalt lithium aluminate ternary material, LiMn2O4, ferric phosphate
Lithium etc., but these types of material has the defects of respective, if cobalt acid lithium is expensive, overcharge resistance performance is poor, the capacity under low-voltage
It plays limited;Nickle cobalt lithium manganate or nickel cobalt lithium aluminate ternary material there are compacted density it is low, with electrolyte poor compatibility and flatulence
The problems such as;The high temperature circulation and high-temperature storage performance of LiMn2O4 are bad;LiFePO4 then there are cryogenic property it is poor the problems such as.For
Solve the problems, such as these, surface coating technology is the most commonly used and effective improvement means, can improve the surface of positive electrode
Structural stability improves the cycle performance under battery high voltage.Have many documents and patent report both at home and abroad on coating modification
Road, but the mode coated and the selection of coating there are still some problems, influence the uniformity coefficient, gram volume and electric discharge of material
Voltage platform etc..
Therefore, design cladding mode evenly, select suitable coating, can obtain the more excellent lithium of performance from
Sub- cell positive material.
The content of the invention
In view of problems of the prior art, it is an object of the invention to provide a kind of molybdenum trioxide coated lithium ion electricity
Pond positive electrode and preparation method thereof, anode material for lithium-ion batteries include composite oxides kernel and clad two parts.It is interior
Core is ternary materials, LiMn2O4, the LiFePO4s such as single or doping vario-property cobalt acid lithium, nickle cobalt lithium manganate or nickel cobalt lithium aluminate
Deng clad is molybdenum trioxide.
Composite oxide particle kernel including at least one or more of lithium and nickel, cobalt, manganese, has following chemistry
The average composition of formula expression:LixNiaCobMncM1-a-b-cO2Or LixFedM1-dPO4;Wherein, M represent selected from Mn, Cr, Co, Ni, V,
At least one of Ti, Al, Ga, Nb and Mg element, and 0≤a≤1,0≤b≤1,0≤c≤1,0≤d≤1,0.4≤x≤
1.5.Clad is molybdenum trioxide, is coated on at least a portion on the surface of above-mentioned composite oxide particle.
For this purpose, the present invention uses following technical scheme:
The present invention provides a kind of preparation method of molybdenum trioxide coated lithium ion battery positive electrode, the described method includes with
Lower step:
(1) composite oxide particle is placed in tube furnace end, close to gas outlet position;
(2) a certain amount of molybdenum trioxide is placed in tube furnace flat-temperature zone, heat treatment 600- is carried out under protective atmosphere
1200 DEG C, keep the temperature 0.5-48h;
(3) position of throughput and composite oxide particle is controlled, molybdenum trioxide is made to be coated on surface, is finally produced
Object.
The ingenious high temperature sublimation characteristics using molybdenum trioxide of the invention, make it be deposited on the composite oxide particle of low-temperature space
Surface is evenly coated, process control, obtains the anode material for lithium-ion batteries of molybdenum trioxide cladding, improves the electrochemistry of material
Performance.
According to the present invention, the molybdenum trioxide described in step (2) can be molybdenum trioxide particles or molybdenum trioxide is molten
The liquid or material through thermally decomposing to generate molybdenum trioxide, such as ammonium molybdate, sodium molybdate, the present invention are not specifically limited.
According to the present invention, the protective atmosphere described in step (2) for nitrogen, argon gas or helium any one or at least two
The combination of kind, such as can be any one in nitrogen, argon gas or helium;Typical but non-limiting is combined as:Nitrogen and
Argon gas;Argon gas and helium;Nitrogen and helium;Nitrogen, argon gas and helium etc., as space is limited and for it is concise the considerations of, the present invention
No longer exclusive list.
According to the present invention, the heat treatment temperature described in step (2) is 600-1200 DEG C, for example, can be 600 DEG C, 700 DEG C,
Specific point value between 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C or 1200 DEG C and above-mentioned numerical value, as space is limited and for letter
The considerations of bright, the present invention no longer exclusive list.
Heat treatment temperature in the present invention described in step (2) is preferably 700-1000 DEG C
According to the present invention, the heat treatment time described in step (2) be 0.5-48h, such as can be 0.5h, 1h, 2h, 3h,
4h、5h、6h、7h、8h、9h、10h、11h、12h、3h、14h、15h、16h、17h、18h、19h、20h、21h、22h、23h、24h、
25h、26h、27h、28h、29h、30h、31h、32h、33h、34h、35h、36h、37h、38h、39h、40h、41h、42h、43h、
Specific point value between 44h, 45h, 46h, 47h or 48h and above-mentioned numerical value, as space is limited and for it is concise the considerations of, this hair
Bright no longer exclusive list.
Heat treatment time in the present invention described in step (2) is preferably for 2-10h.
According to the present invention, the heat treatment heating rate described in step (2) be 1-30 DEG C/min, such as can be 1 DEG C/min,
3℃/min、6℃/min、10℃/min、12℃/min、15℃/min、18℃/min、20℃/min、23℃/min、26℃/
Specific point value between min or 30 DEG C/min and above-mentioned numerical value, as space is limited and for it is concise the considerations of, the present invention no longer
Exclusive list.
According to the present invention, the mass ratio of the clad molybdenum trioxide and composite oxide particle kernel is (0.0001-
0.5):1, such as can be 0.0001:1、0.0003:1、0.0005:1、0.0007:1、0.001:1、0.003:1、0.005:1、
0.007:1、0.01:1、0.03:1、0.05:1、0.07:1、0.1:1、0.3:1 or 0.5:It is specific between 1 and above-mentioned numerical value
Point value, as space is limited and for it is concise the considerations of, the present invention no longer exclusive list.
According to the present invention, the composite oxides kernel is the ternarys materials such as cobalt acid lithium, nickle cobalt lithium manganate or nickel cobalt lithium aluminate
Material, LiMn2O4, the doping vario-property object of LiFePO4 or above-mentioned substance, grain size is preferably 1-20 μm.
According to the present invention, because the length and diameter of tube furnace are different, not to the position of throughput and composite oxide particle
Make concrete restriction, to be less than the sublimation temperature of molybdenum trioxide, molybdenum trioxide is enable to be deposited on composite oxide particle surface be
Preferably.
Compared with prior art, the present invention at least has the advantages that:
(1) present invention coats molybdenum trioxide by the way of deposition on composite oxide particle surface, and coating thickness is equal
It is even and continuous.
(2) molybdenum trioxide has good chemical stability, can generate one layer of uniform guarantor in complex oxide surface
Cuticula can completely cut off electrolyte and active material, reduce the generation of side reaction, avoid the decomposition of electrolyte at higher voltages.
Therefore, gained positive electrode remains to keep preferable cyclical stability and capacity retention ratio at higher voltages, while has excellent
Different high temperature storage and cryogenic property.
Specific embodiment
The present invention is described in more detail below.But following examples is only the simple example of the present invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
The typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
(1) 20g lithium nickelate particles are placed in tube furnace end, close to gas outlet position;
(2) a certain amount of molybdenum trioxide is placed in tube furnace flat-temperature zone, carries out 1200 DEG C of heat treatment in a nitrogen atmosphere, protected
Warm 4h;;
(3) position of throughput and lithium nickelate particle is controlled, molybdenum trioxide is made to be coated on surface, obtains final product,
The mass ratio of middle molybdenum trioxide and lithium nickelate particle kernel is 0.2:1.
Electrochemical property test is carried out using gained composite material as anode material for lithium-ion batteries, pole piece proportioning is compound
Material:Acetylene black:PVDF=90:5:5.Using lithium piece as reference electrode, CR2025 type button cells are prepared.In 2.5-4.2V voltages
Window, under 0.1C current densities, it is 205mAh/g to cycle specific discharge capacity for the first time, 200 circle capacity retention ratios 90% of cycle.
Embodiment 2
(1) 3g lithium iron phosphate particles are placed in tube furnace end, close to gas outlet position;
(2) a certain amount of molybdenum trioxide is placed in tube furnace flat-temperature zone, carries out 800 DEG C of heat treatment under an argon atmosphere, protected
Warm 48h;
(3) position of throughput and lithium iron phosphate particles is controlled, molybdenum trioxide is made to be coated on surface, obtains final product,
The mass ratio of wherein molybdenum trioxide and lithium iron phosphate particles kernel is 0.0001:1.
Electrochemical property test is carried out using gained composite material as anode material for lithium-ion batteries, pole piece proportioning is compound
Material:Acetylene black:PVDF=90:5:5.Using lithium piece as reference electrode, CR2025 type button cells are prepared.In 2.5-3.9V voltages
Window, under 0.1C current densities, it is 152mAh/g to cycle specific discharge capacity for the first time, 200 circle capacity retention ratios 93% of cycle..
Embodiment 3
(1) 0.5g nickel cobalt lithium aluminate particles are placed in tube furnace end, close to gas outlet position;
(2) a certain amount of molybdenum trioxide is placed in tube furnace flat-temperature zone, 600 DEG C of heat treatment is carried out under helium atmosphere, protected
The mass ratio of warm 0.5h, wherein molybdenum trioxide and nickel cobalt lithium aluminate particle kernel is 0.5:1;
(3) position of throughput and nickel cobalt lithium aluminate particle is controlled, molybdenum trioxide is made to be coated on surface, is finally produced
Object.
Electrochemical property test is carried out using gained composite material as anode material for lithium-ion batteries, pole piece proportioning is compound
Material:Acetylene black:PVDF=90:5:5.Using lithium piece as reference electrode, CR2025 type button cells are prepared.In 2.5-4.2V voltages
Window, under 0.1C current densities, it is 185mAh/g to cycle specific discharge capacity for the first time, 200 circle capacity retention ratios 92% of cycle.
Embodiment 4
(1) 10g nickle cobalt lithium manganate particles are placed in tube furnace end, close to gas outlet position;
(2) a certain amount of molybdenum trioxide is placed in tube furnace flat-temperature zone, hot place is carried out under nitrogen and argon gas mixed atmosphere
700 DEG C of reason keeps the temperature 5h;
(3) position of throughput and nickle cobalt lithium manganate particle is controlled, molybdenum trioxide is made to be coated on surface, is finally produced
The mass ratio of object, wherein molybdenum trioxide and nickle cobalt lithium manganate particle kernel is 0.5:1.
Electrochemical property test is carried out using gained composite material as anode material for lithium-ion batteries, pole piece proportioning is compound
Material:Acetylene black:PVDF=90:5:5.Using lithium piece as reference electrode, CR2025 type button cells are prepared.In 2.5-4.2V voltages
Window, under 0.1C current densities, it is 175mAh/g to cycle specific discharge capacity for the first time, 200 circle capacity retention ratios 91% of cycle.
Applicant states that the present invention illustrates the detailed process equipment of the present invention and technological process by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, selection of concrete mode etc. all fall within the present invention's
Within protection domain and the open scope.
Claims (6)
- A kind of 1. molybdenum trioxide coated lithium ion battery positive electrode and preparation method thereof, which is characterized in that the positive electrode Including:Composite oxide particle kernel and clad.(1) composite oxide particle kernel including at least one or more of lithium and nickel, cobalt, manganese, has following chemical formula The average composition of expression:LixNiaCobMncM1-a-b-cO2Or LixFedM1-dPO4;Wherein, M represent selected from Mn, Cr, Co, Ni, V, At least one of Ti, Al, Ga, Nb and Mg element, and 0≤a≤1,0≤b≤1,0≤c≤1,0≤d≤1,0.4≤x≤ 1.5。(2) clad is molybdenum trioxide, is coated on at least a portion on the surface of above-mentioned composite oxide particle.
- 2. the preparation method comprises the following steps:(1) composite oxide particle is placed in tube furnace end, close to gas outlet position;(2) a certain amount of molybdenum trioxide is placed in tube furnace flat-temperature zone, 600-1200 DEG C of heat treatment is carried out under protective atmosphere, Keep the temperature 0.5-48h;(3) position of throughput and composite oxide particle is controlled, molybdenum trioxide is made to be coated on surface, obtains final product.
- 3. method as claimed in claim 1 or 2, which is characterized in that the protective atmosphere described in step (2) is nitrogen, argon gas Helium any one or at least two combination.
- 4. the method as described in claim 1-3, which is characterized in that the clad molybdenum trioxide and composite oxide particle The mass ratio of kernel is (0.0001-0.5):1.
- 5. the method as described in claim 1-4, which is characterized in that the composite oxides kernel is cobalt acid lithium, nickel cobalt mangaic acid The ternary materials such as lithium or nickel cobalt lithium aluminate, LiMn2O4, the doping vario-property object of LiFePO4 or above-mentioned substance, grain size is preferably 1-20 μm。
- 6. the molybdenum trioxide coated lithium ion battery anode being prepared according to claim 1-5 any one of them preparation methods Material.
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CN108682839A (en) * | 2018-06-05 | 2018-10-19 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery positive electrode and preparation method thereof |
CN110120513A (en) * | 2019-05-24 | 2019-08-13 | 哈尔滨理工大学 | A method of nickle cobalt lithium manganate/molybdenum oxide spheric electrode material is prepared using atomic vapor deposition technology |
CN110783538A (en) * | 2019-09-22 | 2020-02-11 | 英德市科恒新能源科技有限公司 | Ternary positive electrode material of lithium battery with metal oxide coated in gas phase and preparation method thereof |
CN112701261A (en) * | 2020-12-25 | 2021-04-23 | 清远道动新材料科技有限公司 | MoO (MoO)3Coated high-nickel ternary positive electrode material and preparation method thereof |
CN113054168A (en) * | 2019-12-28 | 2021-06-29 | 湖南杉杉能源科技股份有限公司 | Tungsten-molybdenum composite coated ternary cathode material and preparation method thereof |
CN113571693A (en) * | 2021-07-30 | 2021-10-29 | 浙江帕瓦新能源股份有限公司 | Modified ternary positive electrode material precursor of lithium ion battery and preparation method thereof |
CN114361441A (en) * | 2022-01-07 | 2022-04-15 | 江苏大学 | Preparation method of in-situ coated single crystal high-nickel ternary cathode material |
US20220310990A1 (en) * | 2021-03-24 | 2022-09-29 | Hyundai Motor Company | Positive electrode material for lithium secondary battery and lithium secondary battery including same |
CN115304108A (en) * | 2022-07-13 | 2022-11-08 | 合肥国轩电池材料有限公司 | Preparation method and device of tungsten-coated ternary cathode material |
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CN108682839A (en) * | 2018-06-05 | 2018-10-19 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery positive electrode and preparation method thereof |
CN110120513A (en) * | 2019-05-24 | 2019-08-13 | 哈尔滨理工大学 | A method of nickle cobalt lithium manganate/molybdenum oxide spheric electrode material is prepared using atomic vapor deposition technology |
CN110783538A (en) * | 2019-09-22 | 2020-02-11 | 英德市科恒新能源科技有限公司 | Ternary positive electrode material of lithium battery with metal oxide coated in gas phase and preparation method thereof |
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CN113054168A (en) * | 2019-12-28 | 2021-06-29 | 湖南杉杉能源科技股份有限公司 | Tungsten-molybdenum composite coated ternary cathode material and preparation method thereof |
CN112701261A (en) * | 2020-12-25 | 2021-04-23 | 清远道动新材料科技有限公司 | MoO (MoO)3Coated high-nickel ternary positive electrode material and preparation method thereof |
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US11962001B2 (en) * | 2021-03-24 | 2024-04-16 | Hyundai Motor Company | Positive electrode material for lithium secondary battery and lithium secondary battery including same |
CN113571693A (en) * | 2021-07-30 | 2021-10-29 | 浙江帕瓦新能源股份有限公司 | Modified ternary positive electrode material precursor of lithium ion battery and preparation method thereof |
CN114361441A (en) * | 2022-01-07 | 2022-04-15 | 江苏大学 | Preparation method of in-situ coated single crystal high-nickel ternary cathode material |
CN115304108A (en) * | 2022-07-13 | 2022-11-08 | 合肥国轩电池材料有限公司 | Preparation method and device of tungsten-coated ternary cathode material |
CN115304108B (en) * | 2022-07-13 | 2023-10-27 | 合肥国轩电池材料有限公司 | Preparation method and device of tungsten-coated ternary cathode material |
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Effective date of registration: 20230309 Address after: 100190 north two street, Zhongguancun, Haidian District, Beijing, 1 Patentee after: Institute of Process Engineering, Chinese Academy of Sciences Address before: 100190 No. two, No. 1, North Haidian District, Beijing, Zhongguancun Patentee before: Institute of Process Engineering, Chinese Academy of Sciences Patentee before: HEBEI AIPUAI TECHNOLOGY DEVELOPMENT CO.,LTD. |