CN103214041A - Cobalt sulfide preparation method - Google Patents
Cobalt sulfide preparation method Download PDFInfo
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- CN103214041A CN103214041A CN2013100649949A CN201310064994A CN103214041A CN 103214041 A CN103214041 A CN 103214041A CN 2013100649949 A CN2013100649949 A CN 2013100649949A CN 201310064994 A CN201310064994 A CN 201310064994A CN 103214041 A CN103214041 A CN 103214041A
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Abstract
The invention discloses a cobalt sulfide preparation method comprising the steps that: 1.72mmol of cobalt nitrate and 1.31mmol of thiourea are dissolved in a solvent; the solution is sealed in a 25mL stainless steel autoclave with a liner of polytetrafluoroethylene; a reaction is carried out for 24h under a temperature of 160 DEG C; a precipitate is fetched, and is washed twice respectively by using deionized water and anhydrous ethanol; and the product is dried for 24h under a temperature of 60 DEG C, such that cobalt sulfide with a hollow structure is obtained. The cobalt sulfide provided by the invention has yarn-ball-shaped, cabbage-shaped, and snowflake-shaped hollow structures, such that the cobalt sulfide has excellent capacitance characteristics and good charge-discharge performance. A maximal capacitor value under a current density of 5mAcm<-2> is 389FG<-1>, and a capacitor value under a current density of 50mAcm<-2> is 277FG<-1>. The cobalt sulfide can be widely applied in super capacitor materials and electrode materials.
Description
Technical field
The present invention relates to a kind of preparation method of capacitance material or electrode materials of excellent electrochemical performance, relate in particular to the preparation method of a kind of cobaltous sulfide (CoS).
Background technology
Self-assembly is meant basic structural units such as molecule and nano particle under equilibrium conditions, spontaneously conclude on the thermodynamics on stable, the structure by the non covalent bond effect determine, the process of special aggregate on the performance.Atom and atom get up to form molecule by the covalent linkage key joint, belong to traditional molecular chemistry, do not belong within the category that self-assembly defines; Self-assembly belongs to the supramolecular chemistry that acts on based on a little less than the intermolecular non covalent bond.The physical and chemical process that organic molecule and other structural units are spontaneously concluded the ergasia that becomes various forms such as point with definite structure, line, unimolecular layer, multilayer film, piece, vesica, micella, microtubule, spillikin by non covalent bond under certain conditions also belongs to self assembling process.DNA's is synthetic, the transcribing of RNA, regulation and control and the proteinic self assembling process that all belongs to such as synthetic and folding.Self-assembling technique is a kind of emerging technology, and has unprecedented advantage, all comes into one's own in every respect.For example, when synthetic materials or preparation ergasia, aspect material choice, will obtain unprecedented facility and flexible; Self-assembled material has diversity, can form unimolecular layer, film, vesica, micella, microtubule, spillikin and more complicated organic/metal, organic/inorganic, biology/abiotic mixture etc. by self-assembly, its diversity is considerably beyond the prepared material of additive method; Self-assembled material varied, unique properties will be widely used in numerous areas such as photoelectron, bio-pharmaceuticals, chemical industry, and some field is wherein produced unpredictable promoter action.The design of nanometer self-assembled material under mild conditions is the important topic that scientists is constantly explored with synthesizing always.
Since the seventies in 20th century, transient metal sulfide has obtained showing great attention to owing to have special photoelectric property.Because they have some unique performances, as light, electrical property and chemical property, make it be widely used in every field, for example they can be used as photosensitizers, Hydrobon catalyst, solid lubricant, the cathode material of high-density battery, magneticsubstance.At present, realization semi-conductor nano particles size and pattern are controlled is the key that changes the semi-conductor nano particles photoelectric properties.
Cobaltous sulfide has many phases, and the member is more, and according to relevant, what prepared has CoS, a Co
3S
4, CoS
2And Co
9S
8Deng.Wherein, CoS is crucial magneticsubstance and electrochemical capacitance material.
In the traditional synthesis, the semi-conductor transient metal sulfide is realized by solid state reaction, but this method has its weak point, and solid state reaction generally is meant high temperature solid state reaction, therefore its operational difficulty, cost height, energy consumption height more and more are not suitable for the requirement of social sustainable development.As everyone knows, the light of material, electricity, chemical property usually need the control to size and pattern thereof, thereby simple, convenient and economic preparation method is the present stage scientists problem that needs emphasis to solve.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of cobaltous sulfide is provided.Cobaltous sulfide material with method of the present invention preparation has good dispersity, the few reunion, and the crystal grain well-crystallized, crystal face appears characteristics such as complete.
The objective of the invention is to be achieved through the following technical solutions: a kind of preparation method of cobaltous sulfide, this method comprises the steps: 1.72mmol Xiao Suangu and 1.31mmol thiocarbamide are dissolved in the solvent, the liner that is sealed in 25mL is in the stainless steel autoclave of tetrafluoroethylene, react 24h down at 160 ℃, then with its cool to room temperature, take out throw out, clean respectively 2 times with deionized water and dehydrated alcohol, at last with product dry 24h under 60 ℃, the cobaltous sulfide that obtains having the Openworks shape structure; Described solvent by n-propyl alcohol and water by volume 1:1 mix form or by methyl alcohol and water by volume 1:1 mix form or by hydrogen peroxide and water by volume 3:7 mix and form.
The invention has the beneficial effects as follows, use the cobaltous sulfide of method preparation of the present invention, have high-specific surface area, have good capacitance characteristic; In addition, the CoS of preparation has the Openworks shape structure, shows the favorable charge-discharge performance, is 5 mA cm in current density
-2Having the highest capacitance down is 389F G
-1, be 50 mA cm in current density
-2The time capacitance be 277 F G
-1Therefore, the cobaltous sulfide of method preparation of the present invention can be widely used in electrochemical capacitance material and electrode materials.
Description of drawings
Fig. 1 is that CoS Openworks shape structure of the present invention is reacted the resulting SEM figure of 24h down at 160 ℃;
Fig. 2 is that CoS Openworks shape structure of the present invention is reacted the resulting EDX collection of illustrative plates of 24h down at 160 ℃;
Fig. 3 is that CoS Openworks shape structure of the present invention is reacted the resulting XRD figure spectrum of 24h down at 160 ℃;
Fig. 4 is volume ratio (A) 1:9(B of n-propyl alcohol and deionized water in the CoS Openworks shape structural modification solvent composition of the present invention) 3:7(C) 1:1(D) the SEM figure of 7:3 products therefrom;
Fig. 5 is volume ratio (A) 1:9(B of methyl alcohol and deionized water in the CoS Openworks shape structural modification solvent composition of the present invention) 3:7(C) 1:1(D) the SEM figure of 7:3 products therefrom;
Fig. 6 is volume ratio (A) 1:9(B of hydrogen peroxide and deionized water in the CoS Openworks shape structural modification solvent composition of the present invention) 3:7(C) 1:1(D) the SEM figure of 7:3 products therefrom;
Fig. 7 is CoS Openworks shape structure of the present invention changes the CoS electrode of scanning speed gained in 6mol/L KOH electrolytic solution a CV curve.
Embodiment
The preparation method of cobaltous sulfide of the present invention, step is as follows:
1.72mmol Xiao Suangu and 1.31mmol thiocarbamide are dissolved in the solvent, the liner that is sealed in 25mL is in the stainless steel autoclave of tetrafluoroethylene, react 24h down at 160 ℃, then with its cool to room temperature, take out throw out, clean respectively 2 times with deionized water and dehydrated alcohol, at last with product dry 24h under 60 ℃, the cobaltous sulfide that obtains having the Openworks shape structure.Described solvent by n-propyl alcohol and water by volume 1:1 mix and form, or by methyl alcohol and water by volume 1:1 mix and form, or by hydrogen peroxide and water by volume 3:7 mix and form.
Carry out the sign and the analysis of material below in conjunction with accompanying drawing 1-3.
1, observes the surface topography of CoS Openworks shape structure with SEM: adopt JSM-5610LV type scanning electronic microscope that the surface topography of CoS Openworks shape structure is observed.As seen from Figure 1, at 160 ℃ down behind the reaction 24h, having formed diameter and be the little spherical structure of knitting wool shape about 0.6-10 μ m, is that the sheet structure self-assembly of 300-500nm forms by thickness, and level is obvious.
2, detecting CoS Openworks shape structural element with EDX forms: adopt the JSM-5610LV type attached X-ray energy spectrum of joining of scanning electronic microscope (EDX) under the 15kV high pressure element that CoS Openworks shape structure is contained to be analyzed.As seen from Figure 2, two kinds of atoms of elements of Co and S are than being 1:1, and promptly also provable products therefrom is defined as CoS.
3, XRD analysis CoS Openworks shape structure and material are formed: Fig. 3 is the XRD figure spectrum of CoS Openworks shape structure, and as seen from the figure, products therefrom is CoS.All corresponding to the CoS of hexagonal system, its corresponding card is JCPDS No.65-8977 to all peak positions among the figure, and not assorted peak shows that products therefrom purity is than higher in the spectrum.
In order further to inquire into the influence factor of product pattern, it is 1:1 that its reaction conditions all keeps the mol ratio of Xiao Suangu and thiocarbamide, and temperature of reaction is 160 ℃, and the reaction times is when being 24h, by changing the component of solvent in the reactant, the pattern of research CoS Openworks shape structure.
When 1, n-propyl alcohol is as solvent composition to the influence of CoS pattern: its result is as shown in Figure 4.When the volume ratio of n-propyl alcohol and deionized water is 1:9 (as Fig. 4 A), formed diameter and be the bead about 2 μ m, its surface irregularity injustice.Continue to increase the concentration of n-propyl alcohol, making its volume ratio with deionized water is 3:7(such as Fig. 4 B), form still be a bead, but its surperficial one-tenth rule is concavo-convex, and the linear structure about 25nm is covered in spherome surface.When the volume ratio of n-propyl alcohol and deionized water is 1:1, (see Fig. 4 C), spherome surface said encirclement by linear structure fully, make the integral diameter of spheroid increase to 3-5 μ m, be similar to the spherical engraved structure of knitting wool.When the volume ratio of n-propyl alcohol and deionized water is increased to 7:3, be covered in the structure destroyed slightly (as Fig. 4 D) of spherome surface.Contrast can get, solvent by n-propyl alcohol and water by volume 1:1 to mix when forming its pattern the most special and have high-specific surface area, its electrochemical properties is good.
When 2, methyl alcohol is as solvent composition to the influence of CoS pattern: as shown in Figure 5.When the volume ratio of methyl alcohol and deionized water is 1:9 (as Fig. 5 A), form the spheroid about 3 μ m, and the spherome surface smoother.Continue to increase the concentration of methyl alcohol, when making the volume ratio of methyl alcohol and deionized water be 3:7 (seeing Fig. 5 B), the spheroid size does not have obvious variation, but spherome surface has covered the irregular sheet structure about 10nm, is similar to Chinese cabbage shape engraved structure.When the volume ratio that increases methyl alcohol and deionized water arrives 1:1 (as Fig. 5 C), the spherome surface sheet structure increases, but the spheroid size still remains unchanged substantially.But when the volume ratio of methyl alcohol and deionized water is increased to 7:3 (as Fig. 5 D), the spherome surface coarse injustice that becomes.Contrast can get, solvent by methyl alcohol and water by volume 1:1 to mix when forming its pattern the most special and have high-specific surface area, its electrochemical properties is good.
When 3, hydrogen peroxide is as solvent composition to the influence of CoS pattern: as shown in Figure 6, when the volume ratio of hydrogen peroxide and deionized water is 1:9, form the irregular sheet paradigmatic structure about 5 μ m, by form (as Fig. 6 A) of the sheet structure rule of 1 μ m.Continue to increase the ratio of hydrogen peroxide, when making the volume ratio of hydrogen peroxide and deionized water be 3:7 (as Fig. 6 B), formed similar flakes rule six-sided structure, its surface is densification more.When the volume ratio of hydrogen peroxide and deionized water is increased to 1:1, (see Fig. 6 C), still keep its six-sided structure, mixed and disorderly but internal structure becomes.When the volume ratio of hydrogen peroxide and deionized water is increased to 7:3, only generate the microsphere (as Fig. 6 D) of the sheet structure formation of several 1 μ m.Contrast can get, solvent by hydrogen peroxide and water by volume 1:1 to mix when forming its pattern the most special and have high-specific surface area, its electrochemical properties is good.
In sum, the difference of solvent composition can obtain different patterns: spheroid and sheet structure, and can make spherome surface cover sheet structure by changing consumption, thus increase the specific surface area of spheroid, be beneficial to its practical application.
Because the serious day by day and fossil oil of environmental pollution is exhausted day by day, the research of energy storage material becomes the focus of research gradually.In the middle of numerous technology, electrochemical capacitor or electrochemical capacitance have become focus, and this is because they are compared with secondary rechargeable battery, has higher specific power and longer recycling number of times; And compare with traditional double layer capacitor, it has higher specific energy again.The electrochemical capacitance electrical condenser has had in real life widely to be used, and for example is applied to the electronics that moves, backup power source supply system and hybrid vehicle.Though in the known material, RuO
2Has the highest ratio electricity (720-760Fg
-1), but RuO
2The cost of material is too expensive, is difficult to be applied in the actual production.Therefore, it is low to seek cost, but the material higher than electric capacity becomes research emphasis.But in research in the past, the preparation of metallic sulfide often needs to cost an arm and a leg and have toxic raw material.CoS Openworks shape structure that this experiment employing Xiao Suangu and thiocarbamide have passed through Hydrothermal Preparation, the advantages of nontoxic raw materials of using in the experimentation, with low cost, and the preparation method is simple.Below mainly detect by the chemical property of CV test to CoS Openworks shape structure.
The preparation of electrode
With massfraction is 70% CoS product, 15% graphite, and 12.5% acetylene black (purity〉99.9%) and 2.5% polytetrafluorethylepowder powder mix, and grind evenly in agate mortar.Add the mashed prod that several ethanol preparation become to mix afterwards.At last it is being pressed under 20MPa pressure on the nickel foam of 1cm * 1cm, then at vacuum drying oven inner drying 24h.
The CV characteristic of CoS Openworks shape structure
Fig. 7 shown different scanning speeds (5mV/s, 10mV/s, 20mV/s, 50mV/s) under, the CV characteristic of CoS Openworks shape structure.As shown in the figure, the shape of the CV curve of material obviously is different from the ideal rectangle structure of two electric capacity electricity layers, and tangible reversible electronic transfer process is all arranged among each figure, the capacitance characteristic of hence one can see that this material capacitance characteristic that is as the criterion.
In sum, our success prepared CoS Openworks shape structure with special appearance: knitting wool group Openworks shape, Chinese cabbage Openworks shape, snowflake Openworks shape.Learn that by changing solvent CoS Openworks shape structure forms by the sheet structure self-assembly.Because the pattern of CoS Openworks shape structure is special, therefore its chemical property (CV) is tested.The result shows that the CoS Openworks shape structure of preparing with high-specific surface area has good capacitance characteristic, belongs to the electric capacity of pseudo-capacitance characteristic, has the prospect that is widely used in electrochemical capacitance material and electrode materials.
Claims (1)
1. the preparation method of a cobaltous sulfide, it is characterized in that, this method comprises the steps: 1.72mmol Xiao Suangu and 1.31mmol thiocarbamide are dissolved in the solvent, the liner that is sealed in 25mL is in the stainless steel autoclave of tetrafluoroethylene, reacts 24h down at 160 ℃, then with its cool to room temperature, take out throw out, clean respectively 2 times with deionized water and dehydrated alcohol, at last with product dry 24h under 60 ℃, the cobaltous sulfide that obtains having the Openworks shape structure; Described solvent by n-propyl alcohol and water by volume 1:1 mix form or by methyl alcohol and water by volume 1:1 mix form or by hydrogen peroxide and water by volume 3:7 mix and form.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103971953A (en) * | 2014-04-29 | 2014-08-06 | 同济大学 | Method for synthesizing NiS/Co3S4 composite electrode material with solvothermal method |
| CN104402065A (en) * | 2014-11-03 | 2015-03-11 | 沈阳化工大学 | Preparation method of spheroidic CoS2 nanometer powder |
| CN104399494A (en) * | 2014-12-10 | 2015-03-11 | 吉林大学 | Carbon-coated cobalt sulfide material as well as preparing method thereof and application of carbon-coated cobalt sulfide material in aspect of water cracking hydrogen production |
| CN105399147A (en) * | 2015-11-05 | 2016-03-16 | 沈阳化工大学 | Octahedral-structure CoS2 powder anode material for thermal batteries and preparation method thereof |
| CN106238072A (en) * | 2016-08-01 | 2016-12-21 | 湖南大学 | Cobalt sulfide photocatalyst and its preparation method and application |
| CN106824228A (en) * | 2017-03-21 | 2017-06-13 | 合肥工业大学 | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof |
| CN109603858A (en) * | 2018-12-14 | 2019-04-12 | 中国科学院海洋研究所 | A kind of double activated analogue enztme material and its preparation and application |
| CN109817911A (en) * | 2019-01-09 | 2019-05-28 | 武汉科技大学 | A kind of nine cobalts of flower-shaped porous eight vulcanization carry sulphur composite material and preparation method |
| CN109873156A (en) * | 2019-02-18 | 2019-06-11 | 上海交通大学 | A kind of preparation method and its battery assembly of high capacity Mg secondary cell cobalt sulfide positive electrode |
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| CN103971953B (en) * | 2014-04-29 | 2017-04-05 | 同济大学 | A kind of solvent structure NiS/Co3S4The method of combination electrode material |
| CN103971953A (en) * | 2014-04-29 | 2014-08-06 | 同济大学 | Method for synthesizing NiS/Co3S4 composite electrode material with solvothermal method |
| CN104402065A (en) * | 2014-11-03 | 2015-03-11 | 沈阳化工大学 | Preparation method of spheroidic CoS2 nanometer powder |
| CN104399494A (en) * | 2014-12-10 | 2015-03-11 | 吉林大学 | Carbon-coated cobalt sulfide material as well as preparing method thereof and application of carbon-coated cobalt sulfide material in aspect of water cracking hydrogen production |
| CN104399494B (en) * | 2014-12-10 | 2016-04-20 | 吉林大学 | The coated cobalt sulfide material of a kind of carbon, preparation method and the application in water-splitting product hydrogen thereof |
| CN105399147A (en) * | 2015-11-05 | 2016-03-16 | 沈阳化工大学 | Octahedral-structure CoS2 powder anode material for thermal batteries and preparation method thereof |
| CN106238072A (en) * | 2016-08-01 | 2016-12-21 | 湖南大学 | Cobalt sulfide photocatalyst and its preparation method and application |
| CN106238072B (en) * | 2016-08-01 | 2018-11-20 | 湖南大学 | Cobalt sulfide photochemical catalyst and its preparation method and application |
| CN106824228A (en) * | 2017-03-21 | 2017-06-13 | 合肥工业大学 | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof |
| CN106824228B (en) * | 2017-03-21 | 2019-06-18 | 合肥工业大学 | A kind of flower-shaped cobalt sulfide photochemical catalyst and preparation method thereof |
| CN109603858A (en) * | 2018-12-14 | 2019-04-12 | 中国科学院海洋研究所 | A kind of double activated analogue enztme material and its preparation and application |
| CN109603858B (en) * | 2018-12-14 | 2021-11-16 | 中国科学院海洋研究所 | Double-activity mimic enzyme material and preparation and application thereof |
| CN109817911A (en) * | 2019-01-09 | 2019-05-28 | 武汉科技大学 | A kind of nine cobalts of flower-shaped porous eight vulcanization carry sulphur composite material and preparation method |
| CN109873156A (en) * | 2019-02-18 | 2019-06-11 | 上海交通大学 | A kind of preparation method and its battery assembly of high capacity Mg secondary cell cobalt sulfide positive electrode |
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Application publication date: 20130724 |