CN104787732A - Solid phase preparation method of cobalt 0.85 selenium compound - Google Patents
Solid phase preparation method of cobalt 0.85 selenium compound Download PDFInfo
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Abstract
The invention provides a solid phase preparation method of a cobalt 0.85 selenium compound. The method comprises the following steps: 1, adding a mill ball, cobalt powder and selenium powder into a milling pot; 2, introducing an inert gas into the milling pot to realize protection, sealing, and carrying out a ball milling reaction; 3, taking out the mill ball after the milling reaction, pouring the above obtained product into a container, and collecting; 4, wrapping the collected product by filter paper, and putting the wrapped product in a Soxhlet extractor; and 5, refluxing at 120DEG C with ethylene diamine as a solvent above 8 times, taking out the obtained substance, and drying to obtain the cobalt 0.85 selenium nano-material. The method is a process of exploration of synthesis of nonstoichiometric compounds through physical and chemical reactions by using an industrial molding ball milling technology, and material characterization ways of the compound show that the method is an optical technology for synthesizing the cobalt 0.85 selenium compound. The method has the advantages of simple synthesis process, high output and good repeatability, and the prepared compound has uniform dimensions, has an atom utilization rate approaching 100%, and accords with green chemical engineering requirements.
Description
Technical field
What the present invention relates to is a kind of preparation method storing up hydrogen compound, specifically a kind of cobalt
0.85the method for preparing solid phase of selenium storage hydrogen compound.
Background technology
Solid-phase ball milling method is a kind of important method preparing super-fine material.At present, ball grinding technique only plays a role in the mixing of material and the grinding of raw material.Traditional sense is said, is all realized by high temperature (heat energy) or chemical transformation for the generation of novel substance, transformation of crystal or lattice deformability, is namely realized by high temperature solution phase method and vapor phase process.And the mechanical energy utilizing mill ball effect to produce is participated in directly or caused chemical reaction is that a kind of new compound prepares thinking.The ultimate principle of machinery mechanochemical method is the change utilizing mechanical energy to come induced chemical reaction or induced material tissue, stuctures and properties, prepares novel material with this.As a kind of new technology, it can reduce reactant fusing point (being approximately 60% of normal condition), reduce reaction activity, grain refining, greatly improve powder activity and improve distribution of material homogeneity and the combination at interface between reinforcement and matrix, promote solid state ion diffusivity coefficient, expanding the chemical reaction of whole system to from an active site, is a kind of material synthesis technology of efficient, energy-conservation, easy handling.
In recent years, along with the exhaustion day by day of traditional energy material, social every profession and trade is outstanding all the more and obvious to the requirement of new forms of energy.Hydrogen Energy (energy discharged in the reaction of taking as the leading factor with hydrogen and isotropic substance thereof or in state change process) has good burning performance, calorific value is high, of many uses, the good characteristic such as abundance, cleanliness without any pollution determines its critical role in future source of energy system.The hydrogen storage material of development of new heavy body and hydrogen storage technology become one of focus of Hydrogen Energy area research.Current hydrogen storage material research is just by traditional hydrogen storage alloy (abundant raw materials, but hydrogen storage capability is low, actual capacity is close to theoretical hydrogen storage capability) to novel light hydrogen storage material, (hydrogen storage capability is high, but reversibility is poor, service temperature is high, and dynamic performance is slow) future development.
At present, cobalt
0.85selenium is more and more subject to the attention of researcher, as: hydrothermal method such as University of Anhui Song Ji bright grade has prepared cobalt
0.85selenium nanometer sheet, at room temperature product has larger specific surface area and has high paramagnetism, has good absorption to organic dye methylene blue, can be used for the organic dye in absorption effluent, has good application in sewage disposal; The researchists such as Liu prepare cobalt by thermojet technology
0.85selenium nanocrystal, its band gap is 1.16eV, and band gap, close to the optimum value of solar cell application, can be applied to the photoelectric energies such as dye sensitization solar battery and transform industry; The researchists such as Abhik prepare cobalt by hydrothermal method
0.85selenium nanocrystal, has the features such as high fake capacitance characteristic, high electric capacity anelasticity and high weather resistance, can be applicable to the active material of electrical condenser.At present, cobalt is prepared
0.85the synthetic method of selenium compound is only liquid phase method synthesis, and Solid phase synthesis has no report.
Day by day go deep into extensive along with to the research of hydrogen storage material, a series of Co-X (X=B, BN, CNT, P, S, Si) hydrogen storage material is also developed successfully in succession.Further investigation shows that non-metallic element that above-mentioned hydrogen storage material adds also serves vital effect for the raising of the hydrogen storage property of Co based hydrogen storage material.The introducing of light hydrogen occluding material simultaneously not only increases its surface-area, shortens hydrogen trap distance, adds the boundary number of crystal grain, weaken hydrogen simultaneously and overflow from the spontaneity of non-metallic material.The two effectively integrate the collaborative emission and absorption facilitated hydrogen, kinetics and the thermomechanical property of hydrogen is put in the suction improving material, improves hydrogen storage capability.
Summary of the invention
The object of the present invention is to provide a kind of simple, be suitable for the homogeneous cobalt of industrial production, repeatability size distribution that is good, low cost
0.85the method for preparing solid phase of selenium compound.
The object of the present invention is achieved like this:
(1) mill ball, cobalt powder, selenium powder are joined in grinding pot;
(2) grinding pot filling with inert gas is protected, after sealing, carry out ball-milling reaction;
(3), after grinding terminates, take out mill ball, product is poured in container and collects;
(4) the product filter paper of collection is wrapped put into apparatus,Soxhlet's;
(5) at 120 DEG C, solvent is reflux more than 8 times under the condition of quadrol; Take out and dry, obtain pure cobalt
0.85selenium nano material.
The present invention can also comprise:
(1) rotating speed of the ball-milling reaction described in is 600 revs/min.
(2) mol ratio of cobalt powder and selenium powder is between 1:2 to 1:3.
(3) between mass ratio 1:10 to the 1:15 of cobalt powder and selenium powder mixture and abrading-ball.
Of the present inventionly prepare cobalt
0.85the method of selenium nano particles, it is the exploration carrying out large-scale preparation synthesis with solid phase method, operationally, compared to the hydrothermal method of harshness, it is easier that the method practices such as thermojet heat are got up, experimental installation is simple, output is high, reproducible, preparing product size uniform, atom utilization, close to 100%, meets the requirement of green chemical industry.In addition, the present invention is by prepared cobalt
0.85selenium compound is applied to solid-state hydrogen storage material neighborhood does not also have report.
The cobalt of the present invention's synthesis
0.85selenium nano material is different from traditional aqueous phase preparation method, and the present invention is the exploration utilizing the shaping ball grinding technique of industry to be synthesized at nonstoichiometric compound by physics, chemical action, characterizes means analysis determination cobalt by material
0.85the best techniques means that selenium compound generates.It is simple that the inventive method has synthesizing mean, and output is high, reproducible, preparing product size uniform, and atom utilization, close to 100%, meets the requirement of green chemical industry.
The present invention is different from the reaction of traditional solid-phase ball milling, except starting material being mixed with except powder porphyrize, utilize mill ball and the mutual of raw material to collide the mechanical energy produced, by physics, chemical action, under room temperature condition, cause the chemical reaction that chemical bond generates.The present invention proposes a kind of new approaches preparing compound, by the inventive method can effectively reduce reaction activation energy, greatly improve powder activity, promote solid state ion diffusivity coefficient, and the chemical reaction of whole system is expanded to from an active site, be a kind of fabrication of new materials synthetic technology of efficient, energy-conservation, easy handling.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction schematic diagram of reaction starting material cobalt powder;
Fig. 2 is the X-ray powder diffraction schematic diagram of answering starting material selenium powder;
Fig. 3 is the X-ray powder diffraction schematic diagram preparing material under general ball milling condition;
Fig. 4 is cobalt of the present invention, selenium mol ratio 1:2,600 revs/min of X-ray powder diffraction schematic diagram before quadrol reflow treatment;
Fig. 5 is cobalt of the present invention, selenium mol ratio 1:2,600 revs/min of X-ray powder diffraction schematic diagram after quadrol reflow treatment;
Fig. 6 is cobalt of the present invention, selenium mol ratio 1:3,600 revs/min of X-ray powder diffraction schematic diagram after quadrol reflow treatment;
Fig. 7 is cobalt of the present invention, selenium mol ratio 1:1,600 revs/min of X-ray powder diffraction schematic diagram after quadrol reflow treatment;
Fig. 8 is cobalt of the present invention
0.85cobalt element XPS Analysis schematic diagram in selenium compound;
Fig. 9 is cobalt of the present invention
0.85selenium element XPS Analysis schematic diagram in selenium compound;
Figure 10 is cobalt of the present invention
0.85the scanning electronic microscope schematic diagram of selenium compound particle;
Figure 11 is cobalt of the present invention
0.85the projection electron microscope schematic diagram of selenium compound particle;
Figure 12 is invention cobalt
0.85the specific surface area situation schematic diagram of selenium compound;
Figure 13 is cobalt of the present invention
0.85the storage hydrogen situation schematic diagram of selenium compound;
Figure 14 is cobalt of the present invention
0.85the circulation of selenium compound is inhaled and is put hydrogen situation schematic diagram.
Embodiment
For a better understanding of the present invention, below by example, the present invention is described.
In concrete operations of the present invention, strictly do not limit described ball mill kind to ball mill not limit, but preferably high energy ball mill, includes but not limited to planetary high-energy ball mill, three-dimensional vibrating type high energy ball mill, stirring-type high energy ball mill, roll type high energy ball mill.Ball-milling Time of the present invention can be continuous print Ball-milling Time, also can be interval ball milling, i.e. first ball milling for some time, midfeather for some time, and then continue total Ball-milling Time of ball milling, wherein interval time is 10-60 minute, and the Ball-milling Time removing interval time is 6 hours.
Specific embodiments 1
(1) by mol ratio be cobalt powder, the selenium powder of 1:2, mill ball joins in the ball grinder of clean dried; The ball grinder loading sample is put into glove box and carry out filling with inert gas protection (note, filling with inert gas protection is herein because Co is when aerobic exists, and the oxidation of Co can occur in mechanical milling process);
(2) ball sealer grinding jar, is contained on ball mill by the ball grinder of good seal, carries out ball milling, grinds 6 hours under the rotating speed of 600 revs/min;
(3) take out abrading-ball, ball milling product is poured in small beaker, collect ball milling product;
(4) the product filter paper of collection is wrapped the apparatus,Soxhlet's put into and assemble;
(5) with round-bottomed flask bottom heating mantle heats, quadrol is heated to 120 DEG C and carries out the excessive selenium of backflow dissolving, treat that the quadrol in round-bottomed flask is all evaporated in apparatus,Soxhlet's, so circulation 8 times;
(6) take out paper bag, collect sample and wash away the quadrol solvent of sample surfaces, sample is carried out X-ray powder diffraction test.
(7) test result is cobalt
0.85selenium compound, test result as shown in Figure 5.
Specific embodiments 2
(1) by mol ratio be cobalt powder, the selenium powder of 1:3, abrading-ball joins in the zirconia ball grinding jar of clean dried, the ball grinder loading sample is put into glove box and carry out filling with inert gas protection (attention, filling with inert gas protection is herein because Co is when aerobic exists, and the oxidation of Co can occur in mechanical milling process);
(2) ball sealer grinding jar, is contained on high energy ball mill by the ball grinder of good seal, carries out ball milling, ball milling 6 hours under the rotating speed of 600 revs/min;
(3) take out abrading-ball, ball milling product is poured in small beaker, collect ball milling product;
(4) the product filter paper of collection is wrapped the apparatus,Soxhlet's put into and assemble;
(5) with round-bottomed flask bottom heating mantle heats, quadrol is heated to 120 DEG C and carries out the excessive selenium of backflow dissolving, treat that the quadrol in round-bottomed flask is all evaporated in apparatus,Soxhlet's, so circulation 8 times;
(6) take out paper bag, collect sample and wash away the quadrol solvent of sample surfaces, sample is carried out X-ray powder diffraction test and corresponding scanning, transmission test.
(7) test result is cobalt
0.85selenium compound nano material, test result as shown in Figure 6.
Specific embodiments 3
(1) by mol ratio be cobalt powder, the selenium powder of 1:1, abrading-ball joins in the zirconia ball grinding jar of clean dried, the ball grinder loading sample is put into glove box and carry out applying argon gas protection (attention, filling with inert gas protection is herein because Co is when aerobic exists, and the oxidation of Co can occur in mechanical milling process);
(2) ball sealer grinding jar, is contained on high energy ball mill by the ball grinder of good seal, carries out ball milling, ball milling 6 hours under the rotating speed of 600 revs/min;
(3) take out abrading-ball, ball milling product is poured in small beaker, collect ball milling product;
(4) the product filter paper of collection is wrapped the apparatus,Soxhlet's put into and assemble;
(5) with round-bottomed flask bottom heating mantle heats, quadrol is heated to 120 DEG C and carries out the excessive selenium of backflow dissolving, treat that the quadrol in round-bottomed flask is all evaporated in apparatus,Soxhlet's, so circulation 8 times;
(6) take out paper bag, collect sample and wash away the quadrol solvent of sample surfaces, sample is carried out X-ray powder diffraction test.
(7) test result is cobalt
0.85the mixture of selenium compound and simple substance cobalt, test result as shown in Figure 7.
Specific embodiments 4
(1) by mol ratio be cobalt powder, the selenium powder of 1:3, abrading-ball joins in the zirconia ball grinding jar of clean dried, the ball grinder loading sample is put into glove box and carry out applying argon gas protection (attention, filling with inert gas protection is herein because Co is when aerobic exists, and the oxidation of Co can occur in mechanical milling process);
(2) ball sealer grinding jar, is contained on high energy ball mill by the ball grinder of good seal, carries out ball milling, ball milling 6 hours under the rotating speed of 400 revs/min;
(3) take out abrading-ball, ball milling product is poured in small beaker, collect ball milling product;
(4) the product filter paper of collection is wrapped the apparatus,Soxhlet's put into and assemble;
(5) with round-bottomed flask bottom heating mantle heats, quadrol is heated to 120 DEG C and carries out the excessive selenium of backflow dissolving, treat that the quadrol in round-bottomed flask is all evaporated in apparatus,Soxhlet's, so circulation 8 times;
(6) take out paper bag, collect sample and wash away the quadrol solvent of sample surfaces, sample is carried out X-ray powder diffraction test.
(7) test result is simple substance cobalt.
The invention provides a kind of to cobalt
0.85the method for preparing solid phase of selenium store hydrogen compound, and this material first time is applied to Chu Qing field, its first hydrogen storage capability be 0.81wt%, and cyclical stability is good, and through the circulation of 50 times, capacity still remains on more than 80%.Ball grinding technique shaping in applicable industry, is different from traditional ball milling mixing, by regulating the molar ratio of reactant and the mass ratio of mill ball and reactant, compares, successfully prepare cobalt first through hundreds of experimental summaries
0.85selenium compound.And utilize surname extraction technology, quadrol is solvent, the backflow more than 8 times, by purification of products, cobalt
0.85the size of selenium can remain on about 10nm.The cobalt of more than the 10g order of magnitude can be carried out by the inventive method method
0.85the preparation of selenium nano material, significant in industrial production.
Fig. 1, Fig. 2 are raw-material X-ray powder diffraction schematic diagram, therefrom can analyze, and raw-material purity is high, and without other impurity, starting material are crystallization phases.Drawn by the contrast of standard card: raw material cobalt is the mixing of six side's phase cobalts and Emission in Cubic cobalt, raw material selenium is six single side's phases.
Fig. 3 is the X-ray powder diffraction schematic diagram preparing material under general ball milling condition, therefrom can analyze, cobalt powder and selenium powder still exist, under the mechanical effect of mill ball, raw material cobalt is generated the cobalt of single six side's phases by chemical reaction by initial mixed phase, selenium still keeps crystalline state.Because rotational speed of ball-mill is lower, mill ball comparatively small amt, the undesirable mechanical energy causing producing in process of lapping of the proportioning of reaction raw materials is less, be not enough to the energy barrier reached needed for reaction, do not react by local solid, transfer energy in whole system, only accomplished the Homogeneous phase mixing of material, but do not generated new compound.
Fig. 4 is cobalt, selenium mol ratio 1:2,600 revs/min of X-ray powder diffraction schematic diagram before quadrol reflow treatment, therefrom can analyze, under the mechanical effect of mill ball, fixing suitable starting material mol ratio, mill ball and raw-material mass ratio, under the parameters such as specific rotating speed and reaction times, obtain required cobalt
0.85selenium compound, and the excessive unreacted of part selenium powder completely.Prove that this Parameter Conditions can reach the synthesis of material.
Fig. 5 is cobalt, selenium mol ratio 1:2, and 600 revs/min of X-ray powder diffraction schematic diagram after quadrol reflow treatment, therefrom can analyze, through the backflow of quadrol, due to similar intermiscibility, the quadrol of heat can dissolve the unreacted selenium powder of part, finally obtains single cobalt
0.85selenium pure phase compound.Meanwhile, the selenium be dissolved in quadrol is operated by solvent evaporation experiment, and then obtains the recovery of selenium powder, and second stage employ.The method is both cost-saving turn improves atom utilization, meets the related request of green chemical industry.
Fig. 6 is cobalt, selenium mol ratio 1:3, and 600 revs/min of X-ray powder diffraction schematic diagram after quadrol reflow treatment, therefrom can analyze, and the unreacted selenium of dissolving through quadrol is removed.Because reaction parameter is suitable, so generate the cobalt of pure phase
0.85selenium compound.
Fig. 7 is cobalt, selenium mol ratio 1:1, and 600 revs/min of X-ray powder diffraction schematic diagram after quadrol reflow treatment, therefrom can analyze, and the unreacted selenium of dissolving through quadrol is removed.Molar ratio due to reactant does not reach suitable requirement, and raw material cobalt is excessive so generate simple substance cobalt and cobalt
0.85the mixture of selenium.
Fig. 8, Fig. 9 are respectively prepared cobalt
0.85cobalt, selenium element XPS Analysis schematic diagram in selenium, therefrom can analyze, the product of preparation is pure phase material, do not have the chemical combination state of other impurity, and be satisfied with mol ratio Co:Se=0.85:1, cobalt presents part nominal price, surface is with part positive charge, ensure that its solution can stable existence, do unordered pedesis, be conducive to the preservation of long-time sample.
Figure 11 to Figure 12 is prepared cobalt
0.85the morphology characterization part of selenium.Therefrom can analyze, the product of preparation is that particle size is homogeneous, is about 10nm, due to little particle size and then there is large specific surface area, its activity is higher, is conducive to surface adsorption, chemical property is active, is conducive to, better in electrolyte contacts, improving its hydrogen storage capability.
Figure 13, Figure 14 are prepared cobalt
0.85the hydrogen storage property of selenium compound characterizes.Can draw from Figure 13 its first hydrogen storage capability be 0.81wt% (for 202mAh/g), curve has two platforms, first platform voltage 1.30 ~ 1.38V, owing to electrochemical reduction storage hydrogen, second charging platform 1.40V, owing to cobalt
0.85selenium compound crystals Ku Basi adsorption effect and surface hydrogen absorption comprehensive, the discharge curve of electrode also has 2 obvious discharge platforms: first discharge platform voltage is 1.20V, and the voltage of second discharge platform is 0.3V.We think: these two discharge platforms correspond respectively to cobalt
0.85the releasing of crystals H of selenium compound and the releasing of surface adsorption H.
As can be seen from Figure 14, prepared cobalt
0.85selenium compound cyclical stability is good, and through the circulation of 50 times, capacity still remains on more than 80%, meets the requirement of industrial production and national defense construction, the cobalt prepared by the present invention
0.85selenium compound has broad prospects as hydrogen storage material.
Claims (5)
1. a cobalt
0.85the method for preparing solid phase of selenium compound, is characterized in that;
(1) mill ball, cobalt powder, selenium powder are joined in grinding pot;
(2) grinding pot filling with inert gas is protected, after sealing, carry out ball-milling reaction;
(3), after grinding terminates, take out mill ball, product is poured in container and collects;
(4) the product filter paper of collection is wrapped put into apparatus,Soxhlet's;
(5) at 120 DEG C, solvent is reflux more than 8 times under the condition of quadrol; Take out and dry, obtain pure cobalt
0.85selenium nano material.
2. cobalt according to claim 1
0.85the method for preparing solid phase of selenium compound, is characterized in that: the rotating speed of described ball-milling reaction is 600 revs/min.
3. cobalt according to claim 1 and 2
0.85the method for preparing solid phase of selenium compound, is characterized in that: the mol ratio of cobalt powder and selenium powder is between 1:2 to 1:3.
4. cobalt according to claim 1 and 2
0.85the method for preparing solid phase of selenium compound, is characterized in that: between mass ratio 1:10 to the 1:15 of cobalt powder and selenium powder mixture and abrading-ball.
5. cobalt according to claim 3
0.85the method for preparing solid phase of selenium compound, is characterized in that: between mass ratio 1:10 to the 1:15 of cobalt powder and selenium powder mixture and abrading-ball.
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| CN106012678A (en) * | 2016-06-07 | 2016-10-12 | 青岛大学 | Process for preparing cobalt selenide composite carbon paper |
| CN105957723B (en) * | 2016-05-31 | 2018-06-01 | 浙江大学 | A kind of method that chemical vapour deposition technique prepares cobaltous selenide super capacitor material |
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| SU1726371A1 (en) * | 1990-03-21 | 1992-04-15 | Молдавский государственный университет им.В.И.Ленина | Cobalt (ii) hydroselenite (2-water) |
| CN1159211C (en) * | 2002-06-07 | 2004-07-28 | 清华大学 | Synthesis of several metal selenides and tellurides as semiconductor material |
| CN102616753B (en) * | 2012-04-11 | 2013-09-18 | 桂林理工大学 | Low-temperature mechanical alloying method for preparing sulphur selenide submicro powder material |
| CN103949274B (en) * | 2014-05-07 | 2016-05-18 | 安徽师范大学 | A kind of Co0.85Se catalyst material and preparation method |
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| C.E.M. CAMPOS ET AL.: "Hexagonal CoSe formation in mechanical alloyed Co75Se25 mixture", 《SOLID STATE COMMUNICATIONS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105957723B (en) * | 2016-05-31 | 2018-06-01 | 浙江大学 | A kind of method that chemical vapour deposition technique prepares cobaltous selenide super capacitor material |
| CN106012678A (en) * | 2016-06-07 | 2016-10-12 | 青岛大学 | Process for preparing cobalt selenide composite carbon paper |
| CN106012678B (en) * | 2016-06-07 | 2018-06-05 | 青岛大学 | A kind of technique for preparing the compound carbon paper of cobaltous selenide |
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