CN103943379A - Preparation method for graphene load flower-shaped porous nickel oxide composite materials - Google Patents
Preparation method for graphene load flower-shaped porous nickel oxide composite materials Download PDFInfo
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- CN103943379A CN103943379A CN201410110704.4A CN201410110704A CN103943379A CN 103943379 A CN103943379 A CN 103943379A CN 201410110704 A CN201410110704 A CN 201410110704A CN 103943379 A CN103943379 A CN 103943379A
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a preparation method for graphene load flower-shaped porous nickel oxide composite materials. The preparation method is characterized in that graphene serves as a matrix, and flaky porous nickel oxide is assembled into flower-shaped nickel oxide balls and grows on the graphene matrix. The graphene serving as a matrix framework has good electric conductivity, the flower-shaped nickel oxide micro balls can achieve good electric conductivity through the graphene, and the appearance electric conductivity of the composite materials is improved. The width of a nickel oxide piece is 200-300 nm, the length of the nickel oxide piece is 400-600 nm, the thickness of the nickel oxide piece is 5-10 nm, mesopores of 2-10 nm are distributed in the flaky layer structure, and the diameter of the formed flower-shaped nickel oxide micro balls is 1-3 micrometers. The graphene load flower-shaped porous nickel oxide composite materials prepared through a hydrothermal method have the advantages of being large in specific surface area, high in single electrode capacity, good in cycle performance and the like, and suitable for supercapacitor electrode materials.
Description
Technical field
The present invention relates to a kind of preparation method's, particularly a kind of graphene-supported flower-shaped porous nickel oxide of the graphene/nickel oxide composite material as super capacitor material the preparation method of composite material, belong to electrochemistry and capacitor material and manufacture field.
Background technology
Ultracapacitor is the novel energy-storing element of a kind of performance between traditional capacitor and chemical cell, has than the higher energy density of traditional capacitor and than the higher power density of common batteries and longer cycle life.Ultracapacitor is widely used the fields such as industrial large-sized ups power system, electric automobile, military project and Aero-Space at present, and people mainly concentrate in the preparation of high performance electrode material the research of ultracapacitor.
Along with the continuous raising that practical application requires the indices of energy storage device, current energy storage device standard design ability cannot practical requirement.Battery is for a long time in field extensive uses such as automobile, electronics, communication, military affairs, Aero-Space, medical treatment, and the energy density of battery is relatively large, can meet the application needs of many occasions.Yet also there is certain defect in battery: the charging interval is long, power density is relatively low etc.In some high impulse application, battery is difficult to meet system.Compare with conventional batteries, ultracapacitor has higher energy density, power density and long circulation life etc., as a kind of clean, efficient novel energy-storing device, receive more and more researchers' concern, in fields such as electric automobile, mobile communication, science and techniques of defence, there is wide application and development prospect.
Nickel oxide is as a kind of metal oxide, has nonhazardous, abundant raw material, the advantage such as cheap, be widely used in a lot of fields, and it has higher capacity as ultracapacitor.But nickel oxide has fatal shortcoming as capacitance material: conductivity is poor, and nickel oxide material is easily reunited.After this problem solves, to novel green capacitor, preparation has important value.
Graphene (graphene) is a kind of individual layer bi-dimensional cellular shape (only including hexagonal primitive unit cell) lattice structure by the tightly packed one-tenth of carbon atom, and it is by sp
2the mono-layer graphite sheet that the carbon atom close-packed arrays of hydridization forms.There is superpower conductivity, superpower hardness, thermal conductive resin, it is well applied in field of compound material.
Summary of the invention
The object of the invention is to overcome the defect that nickel oxide exists as ultracapacitor, make the super capacitor material of high power capacity, environmental protection.The invention provides graphene-supported a kind of flower-shaped nickel oxide composite material with loose structure and preparation method thereof, its characteristic feature is that nickel oxide sheet is assembled into the compound of flower-like structure and graphene sheet layer.As matrix skeleton Graphene, have good conductivity, flower-shaped nickel oxide microballoon can be realized its satisfactory electrical conductivity by loading on graphene film, has improved the apparent conductivity of composite material.
For achieving the above object, the present invention adopts following technical scheme.
The preparation method of a kind of graphene-supported flower-shaped porous oxidation nickel composite material of the present invention, concrete steps are:
A. measure glycerine and deionized water that volume ratio is 1:7 ~ 1:1, add beaker, stir 0.5 h, become the solution of homogeneous;
B. the Graphene of being prepared by 30 mg ~ 60 mg adds in the mixed solution of step a gained, ultrasonic 1 ~ 24 h;
C. after the Graphene adding until step b disperses completely, then add the water soluble nickel salt of certain mass, precipitation reagent and surfactant, stir; The mass ratio of Graphene and water soluble nickel salt is 1:12.5 ~ 1:16.7; Water soluble nickel salt is nickel nitrate; Precipitation reagent is ethylenediamine; Surfactant is softex kw.
D. the solution of step c gained is proceeded to reactor, under the condition of 120 ~ 200 ℃, constant temperature keeps 6 ~ 48 h, and centrifugal, alcohol wash three times, wash three times, is dried 12 h at 80 ℃, obtains precursor samples;
E. the presoma of preparation is placed in quartz boat, proceeds to tube furnace, with the speed of 10 ~ 50 mL/min, pass into the air in argon gas inert gas drain; At the temperature lower calcinations of 400 ~ 600 ℃ 1 ~ 24 h, finally obtain flower-shaped porous nickel oxide/graphene composite material.
Water soluble nickel salt described in the inventive method is except nickel nitrate, and also available nickel chloride or nickelous sulfate substitute; Described precipitation reagent is except ethylenediamine, and also available urea, ammoniacal liquor or carbonic hydroammonium substitute; Described surfactant is except softex kw, and also available neopelex or polyvinylpyrrolidone substitute.
The Graphene using in the present invention is to adopt the process of conventional known to make, and its preparation method is as follows:
By potassium peroxydisulfate (K
2s
2o
8) 2.5 g, phosphorus pentoxide (P
2o
5) 2.5 g, be dissolved in the 12 mL concentrated sulfuric acids, be heated to 80 ℃; Then 3 g native graphites are added to above-mentioned solution, be incubated 80 ℃, 4.5 hours; Be cooled to room temperature, with after 500 mL deionized water dilutions, standing over night; Filter, with the floating residual acid that goes of 0.2 mm filter; Dry in 60 ℃ of vacuum drying chambers; The pre-oxidation thing obtaining is joined in the concentrated sulfuric acid of 120 mL ice baths, under agitation slowly add 15 g KMnO
4, in the process adding, maintain the temperature at below 20 ℃.Then be that temperature is controlled at 35 ℃ of stirring 2 h.Add 250 mL deionized water dilutions, in dilution, also will in ice bath, make temperature lower than 50 ℃.Stir again 2 h, then add 0.7 L deionized water, and add at once the H of 20 mL30%
2o
2, mixture produces bubble, and color has become glassy yellow by brown, reaction terminating after approximately 0.5 h.Said mixture is filtered, and wash with the 1:10 watery hydrochloric acid of 1 L, filter to remove part metals ion; With 1L water washing, filter again, to remove unnecessary acid; Above-mentioned solution is dissolved in 1 L water, and then ultrasonic 0.5 h left and right under 100 W ultrasonic powers, obtains graphite oxide solution (GO), and after centrifugation, the product that obtains brownish black at air drying obtains the graphene oxide needing.Predecessor graphene oxide 0.2 g is placed under the protection of inert gas, at 200 ~ 500 ℃, carries out pyrolysis processing, make graphite oxide dehydration, the oxygen-containing functional groups such as decarboxylize, hydroxyl, obtain graphene nanometer sheet.
advantage and disadvantage of the present invention
Nickel oxide with pure phase is compared, and the nano composite material that we prepare possesses following outstanding structure and performance characteristics, and preparation method's of the present invention outstanding feature is:
(1) technique is simple, and process prepared by composite material operates at low temperatures, and manufacturing cycle is short; Output is large, and efficiency is high, can scale application.
(2) design feature of the graphene-supported flower-shaped porous oxidation nickel composite material of preparing is: in nickel oxide lamellar structure, be covered with equably the mesoporous of 2-10 nm, improved the specific area of material; The flower-shaped nickel oxide Sphere growth being self-assembled into by sheet nickel oxide, on Graphene matrix, has overcome the shortcoming of nickel oxide poorly conductive.Meanwhile, because Graphene has superpower heat conduction and ductility, to stablizing the structure of this composite material, there is great effect.
(3) capacitive property of the graphene-supported flower-shaped porous oxidation nickel composite material of preparing by this simple method is greatly improved, the electric capacity that this composite material obtains under the current density of 200 mA/g is 413 F/g to the maximum, far above the specific capacity of the simple nickel oxide of current report.
Graphene-supported flower-shaped porous oxidation nickel composite material has successfully overcome two shortcomings of simple nickel oxide, is a kind of prospect electrode material for super capacitor that has very much.
Accompanying drawing explanation
The XRD collection of illustrative plates of the graphene-supported flower-shaped porous oxidation nickel composite material of Fig. 1.
The SEM picture of the graphene-supported flower-shaped porous oxidation nickel composite material of Fig. 2.
The TEM picture of the graphene-supported flower-shaped porous oxidation nickel composite material of Fig. 3.
The charging and discharging curve of the graphene-supported flower-shaped porous oxidation nickel composite material of Fig. 4.
Embodiment
Below by embodiment, further illustrate method of the present invention.
embodiment 1
One, by traditional known process, prepare Graphene
By potassium peroxydisulfate (K
2s
2o
8) 2.5 g, phosphorus pentoxide (P
2o
5) 2.5 g, be dissolved in the 12 mL concentrated sulfuric acids, be heated to 80 ℃; Then 3 g native graphites are added to above-mentioned solution, be incubated 80 ℃, 4.5 hours; Be cooled to room temperature, with after 500 mL deionized water dilutions, standing over night; Filter, with the floating residual acid that goes of 0.2 mm filter; Dry in 60 ℃ of vacuum drying chambers; The pre-oxidation thing obtaining is joined in the concentrated sulfuric acid of 120 mL ice baths, under agitation slowly add 15 g KMnO
4, in the process adding, maintain the temperature at below 20 ℃.Then be that temperature is controlled at 35 ℃ of stirring 2 h.Add 250 mL deionized water dilutions, in dilution, also will in ice bath, make temperature lower than 50 ℃.Stir again 2 h, then add 0.7 L deionized water, and add at once the H of 20 mL30%
2o
2, mixture produces bubble, and color has become glassy yellow by brown, reaction terminating after approximately 0.5 h.Said mixture is filtered, and wash with the 1:10 watery hydrochloric acid of 1 L, filter to remove part metals ion; With 1L water washing, filter again, to remove unnecessary acid; Above-mentioned solution is dissolved in 1 L water, and then ultrasonic 0.5 h left and right under 100 W ultrasonic powers, obtains graphite oxide solution (GO), and after centrifugation, the product that obtains brownish black at air drying obtains the graphene oxide needing.Predecessor graphene oxide 0.2 g is placed under the protection of inert gas, at 200 ~ 500 ℃, carries out pyrolysis processing, make graphite oxide dehydration, the oxygen-containing functional groups such as decarboxylize, hydroxyl, obtain graphene nanometer sheet.
Two, prepare graphene-supported nickel oxide composite material
Preparation method's step is as follows:
1) in beaker, add the glycerine of 30 mL and the deionized water of 50 mL, stir, become the solution of homogeneous, then add the above-mentioned Graphene making of 45 mg, ultrasonic 24 h in this solution.
2) after having dissolved substantially, Graphene adds 0.6 g NiNO
36H
2o, 2 mL ethylenediamines and 0.5 g neopelex, stir 0.5 h, and above-mentioned solution is proceeded in reactor.Reactor is placed in to Muffle furnace, is warming up to 160 ℃, constant temperature keeps 24 hours.
3) question response still cooling after, the solution in reactor is proceeded in beaker, then by this precursor solution under 12000 rpm centrifugal 3 minutes, wash again 3 times, to remove the impurity of not participating in reaction, then, at 80 ℃, dry 12 h, obtain dry precursor samples.
4) then the presoma of preparation is placed in quartz boat, proceeds to tube furnace, with the speed of 10 mL/min, pass into the air in nitrogen drain, then the programming rate with 5 ℃/min is heated to 600 ℃ of insulation 1 h.Treat that sample is cooled to room temperature, obtain the composite material of nickel oxide and Graphene.
make the electric performance test of material:
By product and the acetylene black of preparation, after PTFE evenly mixes according to 85:10:5 ratio, on twin rollers, make film, then be pressed in nickel foam as work electrode, capacity measurement adopts three-electrode system, and active material is work electrode, Pt electrode is as to electrode, saturated calomel electrode, as reference electrode, is carried out constant current charge-discharge test, through can be calculated the single electrode electric capacity of material.
As shown in Figure 1, we have successfully prepared graphene-supported flower-shaped porous oxidation nickel composite material, free from admixture peak in this product to the XRD of product as seen from the figure.Fig. 2 and Fig. 3 are ESEM (SEM) and transmission electron microscope (TEM) photos of the composite material of preparation, can find out that nickel oxide is flower-like structure, these flower-shaped nickel oxide are comprised of the structure of sheet, are covered with the mesoporous of 2-10 nm in lamellar structure, are a kind of netted structure.From Fig. 4 constant current charge-discharge figure, the ratio electric capacity that we can calculate that the composite material of preparation obtains under 200 mA/g current densities is 413 F/g.
embodiment 2
The preparation of Graphene is with the above embodiments 1.
1) in beaker, add the glycerine of 10 mL and the deionized water of 70 mL, stir, become the solution of homogeneous, then add 40 mg Graphenes, ultrasonic 10 h in this solution.
2) after having dissolved substantially, Graphene adds 0.5 g NiCl
26H
2o, 1.8 g urea and 0.5 g neopelex, stir 0.5 h.Above-mentioned solution is proceeded in reactor.Reactor is placed in to Muffle furnace, is warming up to 120 ℃, constant temperature keeps 48 hours.
3) question response still cooling after, the solution in reactor is proceeded in beaker, then by this precursor solution under 8000 rpm centrifugal 5 minutes, washing, alcohol wash each 3 times, to remove the impurity of not participating in reaction, then, at 80 ℃, dry 12h, obtains dry precursor samples.
4) then precursor samples is placed in quartz boat, proceeds to tube furnace, with the speed of 40 mL/min, pass into the air in nitrogen drain, then the programming rate with 5 ℃/min is heated to 500 ℃ of insulation 12 h.Treat that sample is cooled to room temperature, enter to obtain the composite material of nickel oxide and Graphene.
The electric performance test method of composite material is with embodiment 1, and the capacity that the material of preparation records through electro-chemical test is 410 F/g.
embodiment 3
The preparation of Graphene is with the above embodiments 1.
1) in flask, add the glycerine of 40 mL and the deionized water of 40 mL, stir, become the solution of homogeneous, then add 60 mg Graphenes, ultrasonic 4 h in this solution.
2) after having dissolved substantially, Graphene adds 1 g NiSO
46H
2o, 5.4 g carbonic hydroammonium and 0.7 g polyvinylpyrrolidone, stir 0.5 h.Above-mentioned solution is proceeded in reactor.Reactor is placed in to Muffle furnace, is warming up to 200 ℃, constant temperature keeps 6 hours.
3) question response still cooling after, the solution in reactor is proceeded in beaker, then by this precursor solution under 6000 rpm centrifugal 10 minutes, washing, alcohol wash each 3 times, to remove the impurity of not participating in reaction, then, at 80 ℃, dry 12 h, obtain dry precursor samples.
4) precursor samples then obtaining is placed in quartz boat, proceeds to tube furnace, with the speed of 20 mL/min, passes into the air in nitrogen drain, and then the programming rate with 5 ℃/min is heated to 400 ℃ of insulation 8 h.Treat sample cool to room temperature, obtain the composite material of nickel oxide and Graphene.
The electric performance test method of composite material is with embodiment 1, and the capacity that the material of preparation records through electro-chemical test is 392.4 F/g.
embodiment 4
The preparation of Graphene is with the above embodiments 1.
1) in beaker, add the glycerine of 25 mL and the deionized water of 55 mL, stir, become the solution of homogeneous, then add 30 mg Graphenes, ultrasonic 1 h in this solution.
2) after having dissolved substantially, Graphene adds 0.5 g NiCl
26H
2o, 1.8 g ethylenediamines, 0.75 g softex kw, stirs 0.5 h.Above-mentioned solution is proceeded in reactor.Reactor is placed in to Muffle furnace, is warming up to 180 ℃, constant temperature keeps 24 hours.
3) after cooling, the solution in reactor is proceeded in beaker, then by this precursor solution under 10000 rpm centrifugal 5 minutes, washing, alcohol wash each 3 times, to remove the impurity of not participating in reaction, then, at 80 ℃, dry 12 h, obtain dry precursor samples.
4) precursor samples then obtaining is placed in quartz boat, proceeds to tube furnace, with the speed of 30 mL/min, passes into the air in nitrogen drain, and then the programming rate with 5 ℃/min is heated to 600 ℃ of insulation 2 h.Treat sample cool to room temperature, obtain the composite material of nickel oxide and Graphene.
The electric performance test method of composite material is with embodiment 1, and the capacity that the material of preparation records through electro-chemical test is 379 F/g.
embodiment 5
The preparation of Graphene is with the above embodiments 1.
1) in beaker, add the glycerine of 20 mL and the deionized water of 60 mL, stir, become the solution of homogeneous, then add 50 mg Graphenes, ultrasonic 24 h in this solution.
2) after having dissolved substantially, Graphene adds 1g NiSO
46H
2o, 3.6 g urea, 1 g neopelex, stirs 0.5 h.Above-mentioned solution is proceeded in reactor.Reactor is placed in to Muffle furnace, is warming up to 200 ℃, constant temperature keeps 36 hours.
3) question response still cooling after, the solution in reactor is proceeded in beaker, then by this precursor solution under 4000 rpm centrifugal 10 minutes, washing, alcohol wash each 3 times, to remove the impurity of not participating in reaction, then, at 80 ℃, dry 12h, obtains dry precursor samples.
4) precursor samples then obtaining is placed in quartz boat, proceeds to tube furnace, with the speed of 50 mL/min, passes into the air in nitrogen drain, and then the programming rate with 5 ℃/min is heated to 200 ℃ of insulation 24 h.Treat sample cool to room temperature, obtain the composite material of nickel oxide and Graphene.
The electric performance test method of composite material is with embodiment 1, and the capacity that the material of preparation records through electro-chemical test is 351.4 F/g.
Claims (2)
1. a preparation method for graphene-supported flower-shaped porous oxidation nickel composite material, is characterized in that, the method detailed process and step are:
A. measure glycerine and deionized water that volume ratio is 1:7 ~ 1:1, add beaker, stir 0.5 h, become the solution of homogeneous;
B. the Graphene of being prepared by 30 mg ~ 60 mg adds in the mixed solution of step a gained, ultrasonic 1 ~ 24 h;
C. after the Graphene adding until step b disperses completely, then add the water soluble nickel salt of certain mass, precipitation reagent and surfactant, stir; The mass ratio of Graphene and water soluble nickel salt is 1:12.5 ~ 1:16.7; Water soluble nickel salt is nickel nitrate; Precipitation reagent is ethylenediamine; Surfactant is softex kw;
D. the solution of step c gained is proceeded to reactor, under the condition of 120 ~ 200 ℃, constant temperature keeps 6 ~ 48 h, and centrifugal, alcohol wash three times, wash three times, is dried 12 h at 80 ℃, obtains precursor samples;
E. the presoma of preparation is placed in quartz boat, proceeds to tube furnace, with the speed of 10 ~ 50 mL/min, pass into the air in argon gas inert gas drain; At the temperature lower calcinations of 400 ~ 600 ℃ 1 ~ 24 h, finally obtain flower-shaped porous nickel oxide/graphene composite material.
2. the preparation method of a kind of graphene-supported flower-shaped porous oxidation nickel composite material according to claim 1, is characterized in that described water soluble nickel salt is for except nickel nitrate, and also available nickel chloride or nickelous sulfate substitute; Described precipitation reagent is except ethylenediamine, and also available urea, ammoniacal liquor or carbonic hydroammonium substitute; Described surfactant is except softex kw, and also available neopelex or polyvinylpyrrolidone substitute.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105244176A (en) * | 2015-10-12 | 2016-01-13 | 上海应用技术学院 | Flower type Ni<3>S<2>/graphene three-dimensional composite electrode material and preparation method thereof |
| CN106018507A (en) * | 2016-05-16 | 2016-10-12 | 天津理工大学 | Preparation method of mesoporous nickel oxide having excellent ammonia gas sensitive properties |
| CN106192445A (en) * | 2016-06-24 | 2016-12-07 | 苏州益可泰电子材料有限公司 | The preparation method of wear resistant belt |
| CN107140717A (en) * | 2017-05-19 | 2017-09-08 | 湘潭大学 | A kind of graphene/NiO nano composite aerogel capacitive desalination electrodes and preparation method thereof |
| CN109433225A (en) * | 2018-08-24 | 2019-03-08 | 北京镭硼科技有限责任公司 | A kind of preparation method and application of the grapheme material of palladium/nickel alloy load |
| CN111333127A (en) * | 2020-03-05 | 2020-06-26 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| CN111333128A (en) * | 2020-03-05 | 2020-06-26 | 西北工业大学 | Preparation method of high-uniformity nickel oxide |
| CN112397697A (en) * | 2020-11-16 | 2021-02-23 | 河北零点新能源科技有限公司 | Preparation method of flower-shaped nickel oxide/carbon composite material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105244176A (en) * | 2015-10-12 | 2016-01-13 | 上海应用技术学院 | Flower type Ni<3>S<2>/graphene three-dimensional composite electrode material and preparation method thereof |
| CN105244176B (en) * | 2015-10-12 | 2017-09-29 | 上海应用技术学院 | A kind of Ni of flower pattern3S2/ graphene three-dimensional combination electrode material and preparation method thereof |
| CN106018507A (en) * | 2016-05-16 | 2016-10-12 | 天津理工大学 | Preparation method of mesoporous nickel oxide having excellent ammonia gas sensitive properties |
| CN106018507B (en) * | 2016-05-16 | 2018-05-15 | 天津理工大学 | A kind of preparation method of the mesoporous nickel oxide with ammonia air-sensitive performance |
| CN106192445A (en) * | 2016-06-24 | 2016-12-07 | 苏州益可泰电子材料有限公司 | The preparation method of wear resistant belt |
| CN107140717A (en) * | 2017-05-19 | 2017-09-08 | 湘潭大学 | A kind of graphene/NiO nano composite aerogel capacitive desalination electrodes and preparation method thereof |
| CN109433225A (en) * | 2018-08-24 | 2019-03-08 | 北京镭硼科技有限责任公司 | A kind of preparation method and application of the grapheme material of palladium/nickel alloy load |
| CN111333127A (en) * | 2020-03-05 | 2020-06-26 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| CN111333128A (en) * | 2020-03-05 | 2020-06-26 | 西北工业大学 | Preparation method of high-uniformity nickel oxide |
| CN111333128B (en) * | 2020-03-05 | 2021-04-13 | 西北工业大学 | Preparation method of high-uniformity nickel oxide |
| CN111333127B (en) * | 2020-03-05 | 2021-04-23 | 西北工业大学 | Hierarchical porous honeycomb nickel oxide microsphere and preparation method thereof |
| US11174171B2 (en) | 2020-03-05 | 2021-11-16 | Northwestern Polytechnical University | Hierarchical porous honeycombed nickel oxide microsphere and preparation method thereof |
| CN112397697A (en) * | 2020-11-16 | 2021-02-23 | 河北零点新能源科技有限公司 | Preparation method of flower-shaped nickel oxide/carbon composite material |
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Application publication date: 20140723 |