CN102530905B - Preparation method of nano FePO4 with controllable particle size - Google Patents
Preparation method of nano FePO4 with controllable particle size Download PDFInfo
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- CN102530905B CN102530905B CN201110445797.2A CN201110445797A CN102530905B CN 102530905 B CN102530905 B CN 102530905B CN 201110445797 A CN201110445797 A CN 201110445797A CN 102530905 B CN102530905 B CN 102530905B
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Abstract
The method provides a method for preparing nano FePO4. The method comprises the steps of: a. dissolving soluble phosphorus source and soluble ferric iron salt in deionized water, and adjusting the pH value with an acid until the solution is clear and transparent; b. adding an organic solvent and a surfactant to the solution obtained in the step a, and stirring until the solution is in a homogeneous, clear and stable state; c. adjusting the solution obtained in the step b to a certain temperature, placing the solution in an ultrasonic field, slowly adding an alkaline solution under vigorously stirring, and adjusting the solution to a certain pH value to obtain FePO4 colloidal particle sol; and d. centrifugally cleaning the FePO4 colloidal particle sol with deionized water three times, ultrasonically dispersing in an organic solvent, and drying in a vacuum drying oven at a certain drying temperature for a certain drying time to obtain nano FePO4. The method for preparing FePO4 provided by the invention has the characteristics of simple production process and low cost; and the product obtained by the method has low impurity content, excellent appearance and controllable particle size.
Description
Technical field
The present invention relates to Material Field, particularly, the present invention relates to nanometer Fe PO
4preparation method.
Background technology
Before lithium ion secondary battery anode material ferric lithium phosphate invention, tertiary iron phosphate is mainly used in the fields such as ceramic foodstuff additive, is also used as in recent years support of the catalyst.Flourish along with lithium ion battery anode material lithium iron phosphate, tertiary iron phosphate is also widely used in the presoma of preparing high-performance lithium iron phosphate cathode material.
In recent years, day by day serious along with the progressively exhausted and vehicle exhaust environmental pollution of whole world petroleum resources, power truck (EV) or hybrid electric vehicle (HEV) and corresponding electrical source of power are developed rapidly.The plurality of advantages such as lithium ion battery volume is little, operating voltage is high, memory-less effect, pollution are little, have extended cycle life, thereby be subject to extensive welcome.Anode material for lithium-ion batteries is a key factor that determines battery performance, and business-like positive electrode material has LiCoO at present
2, LiNiO
2, LiMn
2o
4deng, but other positive electrode material of comparing, LiFePO
4there are two significant advantages: excellent safety performance and cycle performance, this is because its inner unique scaffolding structure makes its molecular structure in working cycle highly stable, therefore generally believes in the world in recent years LiFePO
4it is the best novel anode material of high-energy power battery.
Although LiFePO
4have many merits, but also have some shortcomings part, particularly current LiFePO
4main application fields is power lithium-ion rechargeable battery, so make these shortcomings seem more outstanding during heavy-current discharge: first, its specific conductivity is low, pure LiFePO
4specific conductivity generally at this order of magnitude of 10-10S/m, this problem is seriously restricting it as the practical application of high-power battery; Secondly, because of LiFePO
4structure is limited for the passage that lithium ion diffusion provides, and lithium ion is in the embedding of crystal grain inside and to deviate from speed slow, and this causes working as LiFePO
4the embedding of lithium ion and deviate from speed and be less than interfacial chemistry pace of change when the high-multiplying power discharge, while showing as high-multiplying power discharge, gram volume is lower and polarization is severe; Finally, the low energy density of battery that causes of its tap density and compacted density is low; Granule-morphology is difficult to control and causes its processing characteristics poor.These problems cause it in commercial applications, to have a lot of obstacles, so must solve LiFePO from material preparation
4these difficulties that face.At many raising LiFePO
4in the method for performance, obtain the LiFePO of nanometer
4thereby reduce the diffusion length of Li+ in crystal grain, contribute to greatly to improve LiFePO
4high magnification impulse electricity performance.
Synthetic LiFePO
4scheme a lot, in many synthetic schemess, with FePO
4for precursor synthesis LiFePO
4there is salient feature: FePO
4with LiFePO
4there is similar crystalline structure, and Li+ at high temperature has fabulous diffusion, so can be by controlling FePO
4granule-morphology, size and size-grade distribution synthesize desirable nanometer LiFePO
4, be also FePO
4hereditary property.Accordingly, we can relatively easily utilize various soft chemical methods to prepare nanometer Fe PO
4, by controlling pH value, temperature, concentration, tensio-active agent and other condition, synthesize the controllable nano FePO of particle diameter, pattern, size-grade distribution
4, and synthesize LiFePO by high temperature solid state reaction
4, simultaneously by FePO
4particle size, pattern etc. entail LiFePO
4.And the LiFePO of suitable particles pattern, size, size-grade distribution
4to there is excellent electrochemical character lithium ion battery essential condition.
Therefore, by controlling pH value, temperature, concentration, tensio-active agent and other condition, synthesize the controllable nano FePO of particle diameter, pattern, size-grade distribution
4thereby, utilize this controllable nano FePO
4for precursor synthesis LiFePO
4method be very significant.
Summary of the invention
The invention provides synthesis of nano FePO
4method.
According to an aspect of the present invention, provide a kind of nanometer Fe PO for preparing
4method, comprise the following steps:
A. soluble sources and solubility trivalent iron salt are dissolved in deionized water, utilize acid to regulate its pH value to make solution in clear;
B. to add organic solvent, tensio-active agent in a step gained solution and be stirred to solution evenly, clarification, steady state;
C. regulate b step gained solution to certain temperature, then solution is inserted in ultrasonic field, and slowly add basic solution under vigorous stirring, regulator solution to certain pH value obtains FePO
4micelle colloidal sol;
D. with deionized water to described FePO
4micelle colloidal sol carries out eccentric cleaning three times, and ultrasonic being scattered in organic solvent put into vacuum drying oven dry, and under certain drying temperature, dry certain hour obtains having the greyish white or light yellow ball shaped nano FePO of better dispersiveness
4.
In aforesaid method, wherein said method is included in and in step b, adds pattern adjusting control agent.
In aforesaid method, wherein said soluble sources is selected from phosphoric acid, sodium phosphate, potassiumphosphate, ammonium phosphate, disodium-hydrogen, potassium phosphate,monobasic, ammonium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate or primary ammonium phosphate.
In aforesaid method, wherein said trivalent iron salt is iron nitrate, iron(ic) chloride or ferric sulfate.
In aforesaid method, the concentration of wherein said soluble sources or molysite is all in 0.05mol/L to 4mol/L scope.
In aforesaid method, wherein said acid is sulfuric acid, nitric acid or hydrochloric acid.
In aforesaid method, wherein the organic solvent in step b is selected from ethanol, ethylene glycol, Virahol, glycerol, lauryl alcohol, glycol ether, triglycol, Tetraglycol 99, poly(oxyethylene glycol) 400, one or more in trihydroxybutane.
In aforesaid method, wherein in step b the volume of organic solvent in 0% to 30% scope.
In aforesaid method, wherein said tensio-active agent is selected from one or more in sodium lauryl sulphate, cetyl trimethylammonium bromide, polyoxyethylene glycol, polyvinyl alcohol, polyoxyethylene octyl phenolic ether, octyl phenyl Soxylat A 25-7.
In aforesaid method, wherein said pattern adjusting control agent is selected from one or more in Isopropylamine, diethylamine, hexanediamine, triethylamine, quadrol, Diisopropylamine, diethanolamine, diethylenetriamine, triethylene tetramine.
In aforesaid method, the 0-2% that the add-on of wherein said pattern adjusting control agent is liquor capacity.
In aforesaid method, the 0-3% that the add-on of wherein said tensio-active agent is solution quality.
In aforesaid method, wherein said basic solution is selected from one or more of soluble carbonate salt, ammoniacal liquor or organic amine.
In aforesaid method, wherein said soluble carbonate salt is selected from sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus, volatile salt or bicarbonate of ammonia.
In aforesaid method, the concentration of wherein said basic solution is in the scope of 0.1mol/L to 6mol/L.
In aforesaid method, wherein the temperature in step c is between-5 to 20 ℃.
In aforesaid method, the frequency of wherein said ultrasonic field is between 10K to 100KHz, and power is between 0 to 3000W.
In aforesaid method, wherein the pH value in step c is between 1.0 to 4.5.
In aforesaid method, wherein the organic solvent in steps d is selected from one or more in propyl alcohol, butanols, ethylene glycol, acetone, Virahol, glycerol, methyl-sulphoxide, DMF, N-Methyl pyrrolidone.
In aforesaid method, wherein the organic solvent in steps d is one or more and the mixed solvent of ethanol in propyl alcohol, butanols, ethylene glycol, acetone, Virahol, glycerol, methyl-sulphoxide, DMF, N-Methyl pyrrolidone.
In aforesaid method, wherein said drying temperature is between 100 to 120 ℃.
In aforesaid method, wherein said time of drying is between 0.5 to 10 hour.
Use the prepared nano ferric phosphate of method of the present invention to have the following advantages:
Production technique is simple, cost is low;
With with the strong base solution such as NaOH, regulate pH value to compare, with carbonate adjusting pH value, reacting phase is to Fe (OH) in gentleness and product
3, Fe
2o
3impurity is few;
With organism such as polyvalent alcohol and organic amines, regulate the pattern of controlling product, products obtained therefrom has good pattern;
This reaction is reacted at relatively low temperature, and considers soltion viscosity, ultrasonic field effect, the reaction many factors such as bubble that generate, and by various reaction conditionss, controls grain diameter;
The pattern of nano ferric phosphate and particle size have the advantages that arbitrarily to regulate and control, and particle diameter can change between 10nm～300nm.
Accompanying drawing explanation
Fig. 1 illustrates the X-ray diffractogram (XRD figure) of the nano ferric phosphate of embodiment 6 preparations.
Fig. 2 illustrates the transmission electron microscope picture (TEM figure) that embodiment 6 prepares nano ferric phosphate.
Fig. 3 illustrates the scanning electron microscope diagram (SEM figure) that embodiment 6 prepares nano ferric phosphate.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but these embodiment are not used in restriction the present invention.
Embodiment 1
The phosphoric acid and being dissolved in 100ml deionized water of each 0.01mol of iron nitrate that meet stoichiometric ratio are made into settled solution, to solution, add each 1g surface active agent polyvinyl alcohol and PEG1000, and add organic solvent ethylene glycol 10ml and pattern adjusting control agent quadrol 1ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is adjusted to 0 ℃, afterwards solution is inserted in certain ultrasonic field (10KHz, 1000W), under vigorous stirring, the sodium carbonate solution of 2mol/L is slowly joined in above-mentioned settled solution simultaneously, pH is adjusted to 1.5, necessarily obtains FePO
4micelle colloidal sol.Gained colloidal sol is carried out to centrifugation, and use deionized water ultrasonic cleaning, repeatedly be scattered in n-propyl alcohol gained tertiary iron phosphate is ultrasonic after three times, after put into vacuum drying oven and be dried under certain vacuum degree, dry after 5 hours at certain 105 ℃, obtain having the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO of better dispersiveness
4h
2o).(gained FePO
4.H
2the XRD of O, TEM, SEM are shown in respectively accompanying drawing 1, accompanying drawing 2, accompanying drawing 3)
Embodiment 2
0.4mol primary ammonium phosphate and 0.4mol iron(ic) chloride are dissolved in 100ml deionized water and are made into settled solution, to solution, add each 3g surface active agent polyvinyl alcohol, and add organic solvent 20ml glycerol and pattern adjusting control agent diethylenetriamine 1ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is adjusted to 15 ℃, afterwards solution is inserted in certain ultrasonic field (80KHz, 2000W), under vigorous stirring, the sodium carbonate solution of 6mol/L is slowly joined in above-mentioned settled solution simultaneously, pH is adjusted to 4.0, necessarily obtains FePO
4micelle colloidal sol.Gained colloidal sol is carried out to centrifugation, and use deionized water ultrasonic cleaning, repeatedly be scattered in propyl carbinol gained tertiary iron phosphate is ultrasonic after three times, after put into vacuum drying oven and be dried under certain vacuum degree, dry after 8 hours at certain 110 ℃, obtain having the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO of better dispersiveness
4h
2o).
Embodiment 3
0.05mol sodium phosphate and 0.05mol iron nitrate are dissolved in 100ml deionized water, utilize nitric acid to regulate its pH value, be made into the settled solution of 0.5mol/L, to solution, add each 3% surfactant emulsifiers OP-10 and Macrogol 4000, and add organic solvent triglycol (30%) and pattern adjusting control agent diethanolamine 1%, and be stirred to solution evenly, clarification, steady state.Under vigorous stirring, the sodium carbonate solution of 6mol/L is slowly joined in above-mentioned settled solution, pH is adjusted to 4.5, obtain FePO
4micelle colloidal sol.Gained colloidal sol is carried out to centrifugation, and use deionized water ultrasonic cleaning, repeatedly after three times by the ultrasonic the solvent mixture that is scattered in ethanol and ethylene glycol of gained tertiary iron phosphate, after put into vacuum drying oven and be dried under certain vacuum degree, dry after 10 hours at certain 120 ℃, obtain having the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO of better dispersiveness
4h
2o).
Embodiment 4
0.1mol SODIUM PHOSPHATE, MONOBASIC and 0.1mol iron nitrate are dissolved in 100ml deionized water, are made into settled solution, and add organic solvent 10ml glycerol and 15ml glycol ether and pattern adjusting control agent hexanediamine 0.5ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is adjusted to 20 ℃, afterwards solution is inserted in certain ultrasonic field (50KHz, 500W), under vigorous stirring, the saleratus of 1mol/L and the mixed basic solution of ammoniacal liquor are slowly joined in above-mentioned settled solution simultaneously, pH is adjusted to 1.0, obtains FePO
4micelle colloidal sol.Gained colloidal sol is carried out to centrifugation, and use deionized water ultrasonic cleaning, repeatedly after three times by the ultrasonic the solvent mixture that is scattered in ethanol and ethylene glycol of gained tertiary iron phosphate, after put into vacuum drying oven and be dried under certain vacuum degree, dry after 3 hours at certain 100 ℃, obtain having the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO of better dispersiveness
4h
2o).
Embodiment 5
0.005mol sodium phosphate and 0.005mol iron nitrate are dissolved in 100ml deionized water, utilize nitric acid to regulate its pH value, be made into the settled solution of 0.05mol/L, to solution add each 0.5g Surfactant SDS and and PEG20000, and add pattern adjusting control agent diethanolamine 1ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is adjusted to-5 ℃, afterwards solution is inserted in certain ultrasonic field (10KHz, 3000W), under vigorous stirring, the sodium carbonate solution of 2mol/L is slowly joined in above-mentioned settled solution simultaneously, pH is adjusted to 2.5, necessarily obtains FePO
4micelle colloidal sol.Gained colloidal sol is carried out to centrifugation, and use deionized water ultrasonic cleaning, repeatedly after three times by the ultrasonic the solvent mixture that is scattered in ethanol and ethylene glycol of gained tertiary iron phosphate, after put into vacuum drying oven and be dried under certain vacuum degree, dry after 10 hours at certain 100 ℃, obtain having the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO of better dispersiveness
4h
2o).
Embodiment 6
The potassium primary phosphate of 0.0.01mol and 0.0.01mol iron nitrate are dissolved in 100ml ionized water, be made into settled solution, to solution, add each 1g surfactant emulsifiers OP-10 and Macrogol 4000, and add 15ml triglycol, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is adjusted to 10 ℃, afterwards solution is inserted in certain ultrasonic field (100KHz, 1000W), under vigorous stirring, the ammonium bicarbonate soln of 3mol/L is slowly joined in above-mentioned settled solution simultaneously, pH is adjusted to 2.5, necessarily obtains FePO
4micelle colloidal sol.Gained colloidal sol is carried out to centrifugation, and use deionized water ultrasonic cleaning, repeatedly be scattered in glycerol solvent gained tertiary iron phosphate is ultrasonic after three times, after put into vacuum drying oven and be dried under certain vacuum degree, dry after 0.5 hour at certain 120 ℃, obtain having the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO of better dispersiveness
4h
2o).
Although described the present invention with reference to specific embodiment of the invention scheme, those skilled in the art is to be understood that and in the situation that not departing from true spirit of the present invention and scope, can carries out various changes and can replace equivalents.In addition, many modifications can be carried out so that particular case, material, material composition, method, method steps adapt to the spirit and scope of the present invention.All these change in the scope of the claims subsidiary.
Claims (21)
1. prepare nanometer Fe PO for one kind
4method, comprising:
A. soluble sources and solubility trivalent iron salt are dissolved in deionized water, utilize acid to regulate its pH value to make solution in clear;
B. to add organic solvent, tensio-active agent in a step gained solution and be stirred to solution evenly, clarification, steady state;
C. regulate b step gained solution to certain temperature, then solution is inserted in ultrasonic field, and slowly add soluble carbonate salt under vigorous stirring, regulator solution to certain pH value obtains FePO
4micelle colloidal sol;
D. with deionized water to described FePO
4micelle colloidal sol carries out eccentric cleaning three times, and ultrasonic being scattered in organic solvent put into vacuum drying oven dry, and under certain drying temperature, dry certain hour obtains nanometer Fe PO
4.
2. method according to claim 1, wherein said method is included in and in step b, adds pattern adjusting control agent.
3. method according to claim 1, wherein said soluble sources is selected from phosphoric acid, sodium phosphate, potassiumphosphate, ammonium phosphate, disodium-hydrogen, potassium phosphate,monobasic, ammonium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate or primary ammonium phosphate.
4. method according to claim 1, wherein said trivalent iron salt is iron nitrate, iron(ic) chloride or ferric sulfate.
5. method according to claim 1, the concentration of wherein said soluble sources or molysite is all in 0.0.1mol/L to 4mol/L scope.
6. method according to claim 1, wherein said acid is sulfuric acid, nitric acid or hydrochloric acid.
7. method according to claim 1, wherein the organic solvent in step b is selected from ethanol, ethylene glycol, Virahol, glycerol, lauryl alcohol, glycol ether, triglycol, Tetraglycol 99, poly(oxyethylene glycol) 400, one or more in trihydroxybutane.
8. method according to claim 1, wherein in step b the volume of organic solvent in 0% to 30% scope.
9. method according to claim 1, wherein said tensio-active agent is selected from one or more in sodium lauryl sulphate, cetyl trimethylammonium bromide, polyoxyethylene glycol, polyvinyl alcohol, polyoxyethylene octyl phenolic ether, octyl phenyl Soxylat A 25-7.
10. method according to claim 1, wherein said pattern adjusting control agent is selected from one or more in Isopropylamine, diethylamine, hexanediamine, triethylamine, quadrol, Diisopropylamine, diethanolamine, diethylenetriamine, triethylene tetramine.
11. methods according to claim 1, the 0-2% that the add-on of wherein said pattern adjusting control agent is liquor capacity.
12. methods according to claim 1, the 0-3% that the add-on of wherein said tensio-active agent is solution quality.
13. methods according to claim 1, wherein said soluble carbonate salt is selected from sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus, volatile salt or bicarbonate of ammonia.
14. methods according to claim 1, the concentration of wherein said soluble carbonate salt is in the scope of 0.1mol/L to 6mol/L.
15. methods according to claim 1, wherein the temperature in step c is between-5 to 20 ℃.
16. methods according to claim 1, the frequency of wherein said ultrasonic field is between 10K to 100KHz, and power is between 0 to 3000W.
17. methods according to claim 1, wherein the pH value in step c is between 1.0 to 4.5.
18. methods according to claim 1, wherein the organic solvent in steps d is selected from one or more in propyl alcohol, butanols, ethylene glycol, acetone, Virahol, glycerol, methyl-sulphoxide, DMF, N-Methyl pyrrolidone.
19. methods according to claim 1, wherein the organic solvent in steps d is one or more and the mixed solvent of ethanol in propyl alcohol, butanols, ethylene glycol, acetone, Virahol, glycerol, methyl-sulphoxide, DMF, N-Methyl pyrrolidone.
20. methods according to claim 1, wherein said drying temperature is between 100 to 120 ℃.
21. methods according to claim 1, wherein said time of drying is between 0.5 to 10 hour.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20140021843A (en) * | 2012-08-10 | 2014-02-21 | 삼성정밀화학 주식회사 | A process for making nano-sized iron phosphate particle |
| CN103832991B (en) * | 2014-03-03 | 2015-11-25 | 湖南雅城新材料发展有限公司 | A kind of preparation method of iron phosphate nano material |
| CN104505495A (en) * | 2014-12-09 | 2015-04-08 | 山东精工电子科技有限公司 | Method for ultrasonic preparation of nano iron phosphate of lithium iron phosphate |
| CN105118995A (en) * | 2015-10-14 | 2015-12-02 | 湖南省正源储能材料与器件研究所 | Production method of battery-grade iron phosphate |
| CN105645371B (en) * | 2016-01-08 | 2017-10-03 | 西南大学 | The phosphatic one step preparation method of nano transition metal and its application |
| CN108793116B (en) * | 2018-06-27 | 2020-09-15 | 内江师范学院 | Preparation method and application of micron iron phosphate with different morphologies |
| CN108840317B (en) * | 2018-09-28 | 2020-03-24 | 广东光华科技股份有限公司 | Preparation method of high-purity high-compaction battery-grade iron phosphate |
| CN110010890A (en) * | 2018-12-26 | 2019-07-12 | 广西大学 | A kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
| CN111653846B (en) * | 2020-07-27 | 2021-10-29 | 中南大学 | Treatment method of waste lithium iron phosphate battery |
| CN112436132B (en) * | 2020-12-10 | 2021-07-02 | 桂林理工大学 | Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus |
| CN112978696B (en) * | 2021-02-23 | 2021-10-01 | 长沙学院 | Iron phosphate and preparation method and application thereof |
| CN116143099B (en) * | 2023-02-24 | 2024-03-19 | 南京理工大学 | Method for cooperatively synthesizing lithium iron phosphate electrode material by using ethylene glycol and sodium dodecyl sulfate |
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Address after: 313100 No. 18, Qiao Qiao Road, pheasant Industrial Park, Zhejiang, Changxin Patentee after: Zhejiang energy energy Polytron Technologies Inc Patentee after: China Jiliang University Patentee after: Tianneng Battery Group Co., Ltd. Address before: 313100 No. 18, Qiao Qiao Road, pheasant Industrial Park, Zhejiang, Changxin Patentee before: Zhejiang Tianneng Energy Technology Co., Ltd. Patentee before: China Jiliang University Patentee before: Tianneng Battery Group Co., Ltd. |
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| CP01 | Change in the name or title of a patent holder | ||
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Address after: 313100 No. 18 Baoqiao Road, Zhejiang Changxing Pheasant City Industrial Park Co-patentee after: China Jiliang University Patentee after: Zhejiang energy energy Polytron Technologies Inc Co-patentee after: Tianneng Battery Group Co., Ltd. Address before: 313100 No. 18 Baoqiao Road, Zhejiang Changxing Pheasant City Industrial Park Co-patentee before: China Jiliang University Patentee before: Zhejiang energy energy Polytron Technologies Inc Co-patentee before: Tianneng Battery Group Co., Ltd. |
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Address after: 313100 No. 18, Qiao Qiao Road, pheasant Industrial Park, Zhejiang, Changxin Co-patentee after: China Institute of Metrology Patentee after: Tianneng Shuai Fude Energy Co., Ltd Co-patentee after: Tianneng Battery Group Co., Ltd. Address before: 313100 No. 18, Qiao Qiao Road, pheasant Industrial Park, Zhejiang, Changxin Co-patentee before: China Institute of Metrology Patentee before: Zhejiang energy energy Polytron Technologies Inc Co-patentee before: Tianneng Battery Group Co., Ltd. |