CN103187564A - Preparation method for battery anode material LiNi0.5Mn1.5O4 - Google Patents

Preparation method for battery anode material LiNi0.5Mn1.5O4 Download PDF

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Publication number
CN103187564A
CN103187564A CN2011104445392A CN201110444539A CN103187564A CN 103187564 A CN103187564 A CN 103187564A CN 2011104445392 A CN2011104445392 A CN 2011104445392A CN 201110444539 A CN201110444539 A CN 201110444539A CN 103187564 A CN103187564 A CN 103187564A
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lini
manganese
nickel
source compound
cell positive
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罗英
顾海涛
冯毅
汤卫平
解晶莹
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Shanghai Institute of Space Power Sources
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Shanghai Institute of Space Power Sources
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a preparation method for a battery anode material LiNi0.5Mn1.5O4, which comprises the following steps of: weighing a nickel-source compound and a manganese-source compound according to a stoichiometric equation, and dissolving the nickel-source compound and the manganese-source compound in deionized water to obtain a mixed solution; adopting a dispersant solution in percentage of 0.1-0.8% by mass, adding a soluble precipitator having a stoichiometric dosage which is 1-1.2 times as much as the dosage of the dispersant solution, adequately and uniformly mixing the dispersant solution and the soluble precipitator to obtain a mixed solution; mixing the two mixed solutions, controlling the pH value to be 8-10, controlling the stirring speed to be 100-800 r/min, controlling the temperature to be 40-100 DEG C, and controlling the reaction time to be 5-24 hours, and then obtaining a precipitate containing nickel and manganese; calcining the precipitate containing nickel and manganese for 5-15 hours at 500-800 DEG C to obtain a manganese oxide containing nickel; and adequately and uniformly mixing the manganese oxide containing nickel with a lithium-source compound in proportion, and then calcining the mixture for 10-48 hours at 600-1000 DEG C to obtain the high-voltage LiNi0.5Mn1.5O4.

Description

Cell positive material LiNi 0.5Mn 1.5O 4The preparation method
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Technical field
The invention belongs to the lithium ion anode material technical field, relate in particular to a kind of cell positive material LiNi 0.5Mn 1.5O 4The preparation method.
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Background technology
Lithium ion battery is widely regarded as follow-on power ion battery owing to have characteristics such as high specific energy, high operating voltage, environmental friendliness.At present, power lithium-ion battery is more and more higher to the requirement of anodal material property, as higher energy density, cheap price, good cycle life etc.In the manganese cathode material of numerous spinel structures, LiM xMn 2-xO 4There is a high voltage platform in (M=Cr, Co, Fe, Ni etc.) more than 4.5V, have higher energy density, have therefore caused people's extensive concern.In this class 5V spinelle positive electrode, LiNi 0.5Mn 1.5O 4Voltage platform about 4.7V, theoretical specific capacity is 146.7mAh/g owing to have excellent cycle performance, higher relatively capacity becomes the focus of power lithium-ion battery positive electrode research.
At present, synthetic LiNi 0.5Mn 1.5O 4The method of material mainly contains solid phase method and liquid phase method.For example, CN101148263A discloses a kind of preparation method of high-voltage lithium ion anode material nickel manganese oxygen, this preparation method belongs to high temperature solid-state method, concrete steps are as follows: after nickel source compound, manganese source compound and Li source compound are mixed by stoichiometric proportion, carry out high temperature sintering again and obtain high voltage nickel manganese oxygen material.Though solid phase method is simple to operate, mass production easily, for synthetic multicomponent material, reactant mixes inhomogeneous, causes material component nonstoichiometry ratio easily, influences its chemical property.Coprecipitation is a kind of synthetic method of easy realization of industrialization in the liquid phase method, and it can realize the even mixing of molecular level, and therefore, co-precipitation-high temperature solid-state method becomes the important method of synthetic multicomponent material gradually.For example, CN101335348A discloses and has a kind ofly prepared 5V spherical cathode material LiNi with carbonate deposition as presoma 0.5Mn 1.5O 4Method, the material of this method preparation is the purity height not only, and has higher specific capacity.CN101752553A also discloses a kind of 5V anode material for lithium-ion batteries LiNi 0.5Mn 1.5O 4Synthetic method, this method adopts oxalate precipitation agent, the material that synthesizes is octahedra spinelle pattern, has higher specific capacity and cycle performance.But for the preparation of multicomponent material presoma, coprecipitation also has significant disadvantages, and such as the difference of multiple lithium metal ion owing to solubility product, settling velocity is inconsistent to cause the fluctuation of body phase component, so that influences the chemical property of product.
 
Summary of the invention
The purpose of this invention is to provide a kind of cell positive material LiNi 0.5Mn 1.5O 4The preparation method, this preparation method's technological operation is simple, good stability, the material of preparing has higher specific capacity, excellent high rate performance.
In order to solve the problems of the technologies described above, the invention provides a kind of cell positive material LiNi 0.5Mn 1.5O 4The preparation method, the method includes the steps of: step 1, nickel source compound, manganese source compound according to the stoichiometric equation weighing, and are dissolved in deionized water, make nickel, the manganese ion total concentration is the mixed solution of 0.5 ~ 2mol/L; Step 2, employing deionized water configuration quality percentage is 0.1% ~ 0.8% dispersant solution, and add the solubility precipitation reagent of 1 ~ 1.2 times of stoichiometric amount, and making the mixed solution of dispersant and precipitation reagent after fully mixing, the solubility of this mixed solution is 0.5 ~ 2mol/L; Step 3, the mixed solution that the mixed solution that step 1 is made and step 2 make mixes, and control pH value is 8 ~ 10, and mixing speed is 100 ~ 800r/min, and controlling temperature is 40 ~ 100 ℃, the reaction time is 5 ~ 24h, obtains the precipitation of nickeliferous manganese; Step 4, the nickeliferous manganese that step 3 is made be deposited in 500 ℃ ~ 800 ℃ down calcining 5 ~ 15h obtain nickeliferous Mn oxide; Step 5 after nickeliferous Mn oxide and Li source compound fully mixed by stoichiometric proportion, at 600 ℃ ~ 1000 ℃ calcining 10 ~ 48h, obtains high voltage LiNi 0.5Mn 1.5O 4
Above-mentioned cell positive material LiNi 0.5Mn 1.5O 4The preparation method, wherein, described step 5 also comprises after the calcining fast cooling to 600 ~ 700 ℃ again, insulation 5 ~ 25h obtains high voltage LiNi 0.5Mn 1.5O 4
Above-mentioned cell positive material LiNi 0.5Mn 1.5O 4The preparation method, wherein, described dispersant is any one in nonionic, anionic, the cationic-type polyacrylamide.
Above-mentioned cell positive material LiNi 0.5Mn 1.5O 4The preparation method, wherein, described manganese source compound is any one or the combination in manganese sulfate, manganese nitrate and the manganese acetate.
Above-mentioned cell positive material LiNi 0.5Mn 1.5O 4The preparation method, wherein, described nickel source compound is any one or the combination in nickelous sulfate, nickel nitrate and the nickel acetate.
Above-mentioned cell positive material LiNi 0.5Mn 1.5O 4The preparation method, wherein, described solubility precipitation reagent is any one or the combination in sodium carbonate, sodium acid carbonate, NaOH, sodium oxalate, ammonium carbonate, carbonic hydroammonium and the ammonium oxalate.
Above-mentioned cell positive material LiNi 0.5Mn 1.5O 4The preparation method, wherein, described Li source compound is any one or the combination in lithium hydroxide, lithium carbonate, the oxalic acid and in the lithium acetate.
The present invention is directed to the synthetic LiNi of coprecipitation 0.5Mn 1.5O 4In the materials process, cause the component fluctuation easily because settling velocity is inconsistent, thereby influence the shortcoming of performance, proposed by in coprecipitation process, adding the synthesis technique of dispersant, improve the homogeneity of component with this, the existence of dispersant plays a part original position and disperses;
The present invention adopts coprecipitation to synthesize nickel manganese precipitation, and makes LiNi in conjunction with high temperature solid state reaction by under the condition that exists at dispersant 0.5Mn 1.5O 4Material, this preparation method's technological operation is simple, good stability, is easy to large-scale production, and the material of preparing has excellent high rate performance and cycle performance.
 
Description of drawings
Cell positive material LiNi of the present invention 0.5Mn 1.5O 4The preparation method provided by following embodiment and accompanying drawing.
Fig. 1 is the LiNi of the embodiment of the invention one preparation 0.5Mn 1.5O 4The X-ray diffractogram of material.
Fig. 2 is the sem photograph of the carbonate deposition that makes in the embodiment of the invention one preparation process.
Fig. 3 is the sem photograph of the Ni, Mn oxide that makes in the embodiment of the invention one preparation process.
Fig. 4 is the LiNi of the embodiment of the invention one preparation 0.5Mn 1.5O 4The sem photograph of material.
Fig. 5 is the LiNi of the embodiment of the invention one preparation 0.5Mn 1.5O 4The charging and discharging curve of material.
Fig. 6 is the LiNi of the embodiment of the invention one preparation 0.5Mn 1.5O 4The little current cycle performance curve of material.
Fig. 7 is the LiNi of the embodiment of the invention one preparation 0.5Mn 1.5O 4The big current cycle performance curve of material.
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Embodiment
Below with reference to Fig. 1~Fig. 7 to cell positive material LiNi of the present invention 0.5Mn 1.5O 4The preparation method be described in further detail.
Embodiment one
Mol ratio by l:3 takes by weighing 0.05mol nickelous sulfate and 0.15mol manganese sulfate, is dissolved in that deionized water is mixed with Mn, the Ni total ion concentration is the mixed solution of 1mol/L; With polyacrylamide (PAAM, non-ionic dispersing agent) is dissolved in deionized water, make mass percent and be 0.5% dispersant solution, 1.2 times sodium carbonate of stoichiometric proportion consumption is joined in the polyacrylamide solution, obtain the mixed precipitation agent solution of polyacrylamide and sodium carbonate after the stirring and dissolving; Adopt pump to squeeze in the reactor that band stirs above-mentioned two kinds of mixed solutions, and control pH value is 8.3, mixing speed is 400r/min, and the reaction time is 20h, through multiple times of filtration and washing, obtains carbonate deposition after the oven dry; Above-mentioned carbonate deposition at 600 ℃ of following heat treatment 5h, is obtained the oxide of nickeliferous manganese; The oxide of above-mentioned nickeliferous manganese and 1.1 times lithium carbonate of stoichiometric proportion consumption are fully ground, and after mixing, 900 ℃ are incubated calcining 20h down in box type furnace, obtain LiNi 0.5Mn 1.5O 4Powder.
This LiNi 0.5Mn 1.5O 4The X-ray diffraction of powder (XRD) is schemed as shown in Figure 1, reference standard card, this LiNi 0.5Mn 1.5O 4Material is spinel-type LiNi 0.5Mn 1.5O 4
This LiNi 0.5Mn 1.5O 4The ESEM of the carbonate deposition of material (SEM) is schemed as shown in Figure 2, and precipitation is the type ball-type.
This LiNi 0.5Mn 1.5O 4The ESEM of the Ni, Mn oxide of material (SEM) figure as shown in Figure 3, oxide is loose porous, and reunites and be the secondary spherical particle, distribution of particles is more even.
This LiNi 0.5Mn 1.5O 4The ESEM of material (SEM) is schemed as shown in Figure 4, and product is reunited by the nanoscale primary particle and is the micron order second particle as can see from Figure 4, has crystallinity preferably, primary particle particle diameter 100 ~ 200nm, second particle particle diameter 2um ~ 3um.
This LiNi 0.5Mn 1.5O 4Material discharges and recharges the interval 3.5 ~ 4.9, and charging current is 0.2C, discharging current be under the condition of 0.2C charging and discharging curve as shown in Figure 5, its charging and discharging curve has two voltage platforms that differ 50mV near 4.7V, this corresponds respectively to Ni 2+/ Ni 3+And Ni 3+/ Ni 4+Redox reaction.Simultaneously, a little platform also appears near the 4V, this be since when synthetic temperature higher, LiNi 0.5Mn 1.5O 4Easy oxygen loss makes part Mn 4+Be reduced into Mn 3+Its specific discharge capacity reaches 136mAh/g.
This LiNi 0.5Mn 1.5O 4Material discharges and recharges the interval 3.5 ~ 4.9, and charging current is 0.2C, and discharging current is that little current cycle performance curve circulates capability retention 95% 50 times as shown in Figure 6 under the condition of 0.2C.
This LiNi 0.5Mn 1.5O 4Material discharges and recharges the interval 3.5 ~ 4.9, and charging current is 0.5C, discharging current be under the condition of 20C big current cycle performance curve as shown in Figure 7, specific discharge capacity reaches 120mAh/g, circulates capability retention 85% 100 times.
As seen, use the LiNi of preparation method's preparation of present embodiment 0.5Mn 1.5O 4Has higher specific capacity, excellent high rate performance.
 
Embodiment two
Mol ratio by l:3 takes by weighing 0.05mol nickelous sulfate and 0.15mol manganese sulfate, is dissolved in that deionized water is mixed with Mn, the Ni total ion concentration is the mixed solution of 1mol/L; With polyacrylamide (PAAM, non-ionic dispersing agent) is dissolved in deionized water, make mass percent and be 0.5% dispersant solution, 1.2 times sodium carbonate of stoichiometric proportion consumption is joined in the polyacrylamide solution, obtain the mixed precipitation agent solution of polyacrylamide and sodium carbonate after the stirring and dissolving; Adopt pump to squeeze in the reactor that band stirs above-mentioned two kinds of mixed solutions, and control pH value is 8.5, mixing speed is 400r/min, and the reaction time is 20h, through multiple times of filtration and washing, obtains carbonate deposition after the oven dry; Above-mentioned carbonate deposition at 600 ℃ of following heat treatment 5h, is obtained the oxide of nickeliferous manganese; The oxide of above-mentioned nickeliferous manganese and 1.1 times lithium carbonate of stoichiometric proportion consumption are fully ground, and after mixing, 700 ℃ are incubated calcining 20h down in box type furnace, obtain LiNi 0.5Mn 1.5O 4Powder.
 
Embodiment three
Mol ratio by l:3 takes by weighing 0.1mol nickelous sulfate and 0.2mol manganese sulfate, is dissolved in that deionized water is mixed with Mn, the Ni total ion concentration is the mixed solution of 1mol/L; With polyacrylamide (PAAM, non-ionic dispersing agent) is dissolved in deionized water, make mass percent and be 0.5% dispersant solution, 1.2 times sodium carbonate of stoichiometric proportion consumption is joined in the polyacrylamide solution, obtain the mixed precipitation agent solution of polyacrylamide and sodium carbonate after the stirring and dissolving; Adopt pump to squeeze in the reactor that band stirs above-mentioned two kinds of mixed solutions, and control pH value is 8.3, mixing speed is 400r/min, and the reaction time is 20h, through multiple times of filtration and washing, obtains carbonate deposition after the oven dry; Above-mentioned carbonate deposition at 700 ℃ of following heat treatment 5h, is obtained the oxide of nickeliferous manganese; The oxide of above-mentioned nickeliferous manganese and 1.1 times lithium carbonate of stoichiometric proportion consumption are fully ground, and after mixing, 900 ℃ are incubated calcining 20h down in box type furnace, obtain LiNi 0.5Mn 1.5O 4Powder.
 
Embodiment four
Mol ratio by l:3 takes by weighing 0.05mol nickelous sulfate and 0.15mol manganese sulfate, is dissolved in that deionized water is mixed with Mn, the Ni total ion concentration is the mixed solution of 1mol/L; With polyacrylamide (PAAM, non-ionic dispersing agent) is dissolved in deionized water, make mass percent and be 0.5% dispersant solution, 1.2 times sodium acid carbonate of stoichiometric proportion consumption is joined in the polyacrylamide solution, obtain the mixed precipitation agent solution of polyacrylamide and sodium carbonate after the stirring and dissolving; Adopt pump to squeeze in the reactor that band stirs above-mentioned two kinds of mixed solutions, and control pH value is 8, mixing speed is 400r/min, and the reaction time is 20h, through multiple times of filtration and washing, obtains carbonate deposition after the oven dry; Above-mentioned carbonate deposition at 600 ℃ of following heat treatment 5h, is obtained the oxide of nickeliferous manganese; The oxide of above-mentioned nickeliferous manganese and 1.1 times lithium carbonate of stoichiometric proportion consumption are fully ground, and after mixing, 900 ℃ are incubated calcining 20h down in box type furnace, and short annealing to 700 ℃ insulation 15h obtains LiNi again 0.5Mn 1.5O 4Powder.
 
Embodiment five
Mol ratio by l:3 takes by weighing 0.1mol nickelous sulfate and 0.2mol manganese sulfate, is dissolved in that deionized water is mixed with Mn, the Ni total ion concentration is the mixed solution of 1mol/L; With polyacrylamide (PAAM, non-ionic dispersing agent) is dissolved in deionized water, make mass percent and be 0.2% dispersant solution, 1.2 times sodium carbonate of stoichiometric proportion consumption is joined in the polyacrylamide solution, obtain the mixed precipitation agent solution of polyacrylamide and sodium carbonate after the stirring and dissolving; Adopt pump to squeeze in the reactor that band stirs above-mentioned two kinds of mixed solutions, and control pH value is 8.3, mixing speed is 400r/min, and the reaction time is 20h, through multiple times of filtration and washing, obtains carbonate deposition after the oven dry; Above-mentioned carbonate deposition at 600 ℃ of following heat treatment 5h, is obtained the oxide of nickeliferous manganese; The oxide of above-mentioned nickeliferous manganese and 1.1 times lithium carbonate of stoichiometric proportion consumption are fully ground, and after mixing, 900 ℃ are incubated calcining 20h down in box type furnace, and short annealing to 700 ℃ insulation 5h obtains LiNi again 0.5Mn 1.5O 4Powder.
The present invention is based on the original position peptizaiton of dispersant, utilize coprecipitation to obtain the precipitation of component homogeneous, and synthesize height ratio capacity in conjunction with high temperature solid state reaction, excellent performance LiNi 0.5Mn 1.5O 4Material.This preparation method's technological operation is simple, and good stability is easy to large-scale production.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.

Claims (7)

1. cell positive material LiNi 0.5Mn 1.5O 4The preparation method, it is characterized in that, may further comprise the steps:
Step 1 according to the stoichiometric equation weighing, and is dissolved in deionized water with nickel source compound, manganese source compound, makes nickel, the manganese ion total concentration is the mixed solution of 0.5 ~ 2mol/L;
Step 2, employing deionized water configuration quality percentage is 0.1% ~ 0.8% dispersant solution, and add the solubility precipitation reagent of 1 ~ 1.2 times of stoichiometric amount, and making the mixed solution of dispersant and precipitation reagent after fully mixing, the solubility of this mixed solution is 0.5 ~ 2mol/L;
Step 3, the mixed solution that the mixed solution that step 1 is made and step 2 make mixes, and control pH value is 8 ~ 10, and mixing speed is 100 ~ 800r/min, and controlling temperature is 40 ~ 100 ℃, the reaction time is 5 ~ 24h, obtains the precipitation of nickeliferous manganese;
Step 4, the nickeliferous manganese that step 3 is made be deposited in 500 ℃ ~ 800 ℃ down calcining 5 ~ 15h obtain nickeliferous Mn oxide;
Step 5 after nickeliferous Mn oxide and Li source compound fully mixed by stoichiometric proportion, at 600 ℃ ~ 1000 ℃ calcining 10 ~ 48h, obtains high voltage LiNi 0.5Mn 1.5O 4
2. cell positive material LiNi as claimed in claim 1 0.5Mn 1.5O 4The preparation method, it is characterized in that described step 5 also comprises after the calcining fast cooling to 600 ~ 700 ℃ again, insulation 5 ~ 25h obtains high voltage LiNi 0.5Mn 1.5O 4
3. cell positive material LiNi as claimed in claim 1 0.5Mn 1.5O 4The preparation method, it is characterized in that described dispersant is any one in nonionic, anionic, the cationic-type polyacrylamide.
4. cell positive material LiNi as claimed in claim 1 0.5Mn 1.5O 4The preparation method, it is characterized in that described manganese source compound is any one or the combination in manganese sulfate, manganese nitrate and the manganese acetate.
5. cell positive material LiNi as claimed in claim 1 0.5Mn 1.5O 4The preparation method, it is characterized in that described nickel source compound is any one or the combination in nickelous sulfate, nickel nitrate and the nickel acetate.
6. cell positive material LiNi as claimed in claim 1 0.5Mn 1.5O 4The preparation method, it is characterized in that described solubility precipitation reagent is any one or the combination in sodium carbonate, sodium acid carbonate, NaOH, sodium oxalate, ammonium carbonate, carbonic hydroammonium and the ammonium oxalate.
7. cell positive material LiNi as claimed in claim 1 0.5Mn 1.5O 4The preparation method, it is characterized in that described Li source compound is any one or the combination in lithium hydroxide, lithium carbonate, the oxalic acid and in the lithium acetate.
CN2011104445392A 2011-12-28 2011-12-28 Preparation method for battery anode material LiNi0.5Mn1.5O4 Pending CN103187564A (en)

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CN106450222A (en) * 2016-11-17 2017-02-22 兰州理工大学 Preparation method of hollow spherical lithium nickel manganese oxide capable of automatically regulating pore diameter

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CN104282903A (en) * 2013-07-08 2015-01-14 三星Sdi株式会社 Cathode active material, method of preparing the cathode material, cathode, and lithium secondary battery including the same
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CN103413929B (en) * 2013-07-30 2015-07-01 南京航空航天大学 Preparation method for spherical Ni1/4Mn3/4CO3 precursor and LiNi0.5Mn1.5O4
CN103904320B (en) * 2014-03-17 2016-06-22 华南理工大学 A kind of high-voltage lithium ion battery cathode material with spinel structure and preparation method thereof
CN103904320A (en) * 2014-03-17 2014-07-02 华南理工大学 High-voltage lithium ion battery positive electrode material with spinel structure and preparation method thereof
CN105800700A (en) * 2014-12-30 2016-07-27 河南科隆新能源有限公司 Preparation method for positive electrode material of lithium battery
CN105800700B (en) * 2014-12-30 2019-10-25 河南科隆新能源有限公司 A kind of preparation method of lithium electricity positive electrode
CN106450222A (en) * 2016-11-17 2017-02-22 兰州理工大学 Preparation method of hollow spherical lithium nickel manganese oxide capable of automatically regulating pore diameter
CN106450222B (en) * 2016-11-17 2019-01-15 兰州理工大学 Can autonomous adjustment aperture hollow sphere nickel ion doped preparation method

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Application publication date: 20130703