CN103663572A - Preparation method of nickel oxide material with superhigh specific capacity - Google Patents
Preparation method of nickel oxide material with superhigh specific capacity Download PDFInfo
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Abstract
The invention relates to a preparation method of a nickel oxide material with superhigh specific capacity. The method comprises the following steps: adding ethylene glycol liquor of a precipitant into ethylene glycol liquor of nickel salt, and refluxing and stirring to obtain a precursor; and carrying out thermal treatment on the precursor at a temperature above 250 DEG C to obtain the nickel oxide material, wherein the precipitant is sodium borohydride. According to the method provided by the invention, sodium borohydride is taken as the precipitant, and the nickel oxide electrode material with high specific capacity and good rate capability can be prepared through a simple chemical precipitation method.
Description
Technical field
The present invention relates to a kind ofly for ultracapacitor, especially the preparation method of the nickel oxide electrode material of fake capacitance, belongs to new material technology and technical field of new energies.
Background technology
Along with the sharply increase of global energy demand, the continuous minimizing of fossil oil store content, and be accompanied by the environmental problem that the use of fossil oil brings, human society is being faced with energy security and more and more stern challenge of environment protection.The novel energy such as battery, electrical condenser has caused people's concern gradually.Wherein, ultracapacitor is as a kind of novel energy-storing element between electrical condenser and battery, there is the good characteristics such as energy density is high, the speed that discharges and recharges is fast, power density is high, efficiency for charge-discharge is high, have extended cycle life, security is good and pollution-free and non-maintaining, so it there is application prospect very widely at aspects such as backup power source, substitute electric power, high-power outputs.
Ultracapacitor can be divided into two kinds by energy storage mechanism: a kind of is the electric double layer capacitance electrical condenser that separation produces based on electrode/electrolyte interfacial charge, and its charcoal with high-specific surface area that adopt is made electrode materials more; The quick reversible redox reaction formation Faraday pseudo-capacitance that another kind utilizes the surface of electrode and body to occur in mutually.Because carbon dioxide process carbon electrode is less than electric capacity, limited the application of double layer capacitor.
In recent years, more about the research of Faraday pseudo-capacitance device.Its metal oxide containing precious metals such as ruthenium oxide that adopt is made electrode materials more, wherein RuO
2the specific storage of ultracapacitor is up to 1340F/g[J.Electrochem.Soc., 151:A281-290 (2004) .], but RuO
2expensive, be difficult for realizing commercialization.Because the transition metal oxides such as nickel oxide, cobalt oxide and manganese oxide have and RuO
2similar character, therefore extremely researchist's concern, wherein nickel oxide resource is extensive, cheap, environment is friendly, is widely used on battery electrode material.
Nickel oxide electrode material for ultracapacitor makes great progress at present, and investigator is studying the nickel oxide electrode that several different methods preparation has good capacitance characteristic.Yet the preparation of nickel oxide electrode material at present also realizes by template or tensio-active agent mostly, and not only preparation process is complicated, and the specific storage of the material of pointing out is not very high or high rate performance is poor.As the employing polyacrylamides such as Wen and polyvinyl alcohol mixing macromole are done soft template, prepare sea urchin shape porous nickel oxide, be made into fake capacitance electrode, under the current rate of 5m A, specific storage only has 327F/g, performance is not fine [J Solid State Electrochem., 11:372-377 (2007) .].Sumanta Kumar Meher etc. use cetyl trimethylammonium bromide as tensio-active agent, adopt microwave method to prepare flower-shaped nickel oxide, used as electrode materials, under the current density of 2A/g, specific storage is 370F/g, specific storage neither very high [ACS Appl.Mater.Interfaces, 3:2063-2073 (2011) .].Sun etc. do by sodium lauryl sulphate the nickel oxide nano sheet that tensio-active agent prepares and do fake capacitance electrode materials, under the current density of 3A/g, specific storage is 993F/g, and special capacity fade is 445F/g under 15A/g, although capacity is very high under low current density, but its high rate performance is very poor, high current density attenuation ratio is serious [J.Mater.Chem., 21:16581-16588 (2011) .].
Also disclose at present the employing precipitator method and first prepared presoma (nickel hydroxide), and then thermal treatment is to prepare the scheme of nickel oxide again.For example CN1887728A discloses a kind of nickel oxide for electrochemical capacitor and preparation method thereof, it adopts sodium oxalate and sodium hydroxide is precipitation agent, tween-80 is tensio-active agent, through liquid-phase precipitation, ageing, obtains nickel hydroxide ultra-micro powder, then thermal treatment 2h at 250～350 ℃.Yet this method still needs to use tensio-active agent, and the specific storage of the nickel oxide making is that about 200F/g, specific storage is lower.CN102070207A discloses a kind of method of preparing nano-nickel oxide, it first adopts such as lime acetate etc. and reacts with nickel salt aqueous solution as preliminary precipitation agent, obtain nickel complex solution, and then the precipitation agents such as sodium oxalate, sodium hydroxide are joined and in nickel complex solution, react to obtain presoma, then roasting 2～8 hours at 300～600 ℃ of presoma.Although this method does not need to use tensio-active agent, but the method that it utilizes coordination precipitation and preliminary precipitation to combine, wherein the oxonium ion in coordination preliminary precipitation can form precipitation with precipitation agent negatively charged ion, it is a problem with the effective separated of the precipitation being formed with precipitation agent negatively charged ion by nickel ion,, easily introduces impurity.In addition, CN102070207A does not have to disclose the specific storage of the standby nickel oxide of this legal system yet.
Therefore, adopt simple method to prepare height ratio capacity and the nickel oxide electrode material with good high rate performance has very important theoretical and practical significance.
Summary of the invention
The problems referred to above in the face of prior art existence,, the object of this invention is to provide a kind of high specific surface area porous nickel oxide electrode material and its preparation method and application, for this area increases a kind of nontoxic inexpensive, preparation technology is simple, and has the electrode materials of high electrochemical performance.
At this, the invention provides a kind of novel preparation method with the nickel oxide material of superelevation specific storage, comprising: the ethylene glycol solution of precipitation agent is added to the ethylene glycol solution of nickel salt, return stirring obtains presoma; And at more than 250 ℃ temperature described in thermal treatment presoma obtain described nickel oxide material; Wherein, described precipitation agent is sodium borohydride.
Method of the present invention adopts sodium borohydride as precipitation agent, by simple chemical precipitation method, can prepare there is high specific storage, the nickel oxide electrode material of good high rate performance.Method of the present invention is simple, cost is low, preparation cycle is short, and without template or tensio-active agent, environmental friendliness.The prepared nickel oxide of the present invention is made into electrode of super capacitor and has shown high specific storage, good high rate performance and cyclical stability, to the widespread use of ultracapacitor, will produce significance.
Preferably, in the present invention, the ethylene glycol solution of described precipitation agent is prepared as follows: described precipitation agent is added in ethylene glycol, fully stir until gush out to form the ethylene glycol solution of described precipitation agent without obvious bubble.
Again, in the present invention, the mol ratio of described nickel salt and precipitation agent can be 1:4～1:13.Precipitation agent very little, is unfavorable for precipitation completely, and precipitation agent is too many, wastes raw material, and is also unfavorable for aftertreatment.
In the present invention, preferably, first the ethylene glycol solution of described nickel salt is heated to it, add after 150～200 ℃ again the ethylene glycol solution of described precipitation agent.The in the situation that of heating, add precipitation agent, be more conducive to reaction and carry out, thus can Reaction time shorten.
Again, described nickel salt can be nickelous nitrate and/or its hydrate, single nickel salt and/or its hydrate, nickelous chloride and/or its hydrate and/or nickelous bromide and/or its hydrate.In a preferred embodiment, nickel salt adopts Nickelous nitrate hexahydrate.
In the present invention, the time of return stirring can be 150～200 ℃, and the time of return stirring is preferably 30 minutes～and 2 hours.
Again, heat treated temperature can be 250～300 ℃, and the heat treated time is preferably 2～4 hours.
Accompanying drawing explanation
Fig. 1 illustrates nickel oxide prepared by example of the present invention and the XRD figure of presoma thereof;
Fig. 2 illustrates the TEM figure of nickel oxide prepared by example of the present invention;
Fig. 3 illustrates the SEM figure of nickel oxide prepared by example of the present invention;
Fig. 4 A illustrates the isothermal adsorption curve of nickel oxide prepared by example of the present invention;
Fig. 4 B illustrates the pore size distribution curve of nickel oxide prepared by example of the present invention;
Fig. 5 illustrates the discharge curve of nickel oxide fake capacitance electrical condenser under different current densities that adopts nickel oxide prepared by example of the present invention;
Fig. 6 illustrates the specific storage of nickel oxide fake capacitance electrical condenser under different current densities that adopts nickel oxide prepared by example of the present invention;
Fig. 7 illustrates and adopts the nickel oxide fake capacitance electrical condenser of nickel oxide prepared by example of the present invention at 4A g
-1time cyclic curve;
Fig. 8 illustrates energy density-power density curve of the nickel oxide fake capacitance electrical condenser that adopts nickel oxide prepared by example of the present invention;
Fig. 9 illustrates the XRD figure of the product of comparative example 1 preparation;
The specific storage of the fake capacitance electrical condenser that Figure 10 illustrates the product that adopts embodiments of the invention 2,3 and comparative example 1,2 preparations under different current densities.
Embodiment
Below in conjunction with accompanying drawing and following embodiment, further illustrate the present invention, should be understood that following embodiment and/or accompanying drawing are only for the present invention is described, and unrestricted the present invention.
The present invention adopts sodium borohydride etc. as precipitation agent, adopts simple heated and stirred method to prepare presoma, after calcining, obtains nickel oxide.After the nickel oxide of preparation is mixed with conductive agent, binding agent, spread upon the test of carrying out three-electrode system on collector.Utilize the feature of itself large specific surface area, uniform mesoporous aperture, high porosity to increase contacting of material and electrolytic solution, improve the utilization ratio of material, accelerate the transmission of ion, thereby improved the chemical property of nickel oxide electrode.
The following describes step of the present invention:
(1) nickel salt is dissolved in to the alcoholic solution that obtains nickel salt in alcohol, herein, nickel salt can be Nickelous nitrate hexahydrate, but should understand other suitable nickel salts is also suitable for, such as single nickel salt, nickelous chloride, nickelous bromide and hydrate thereof etc., should be understood that equally and can adopt a kind of in these nickel salts, also can adopt mixture that two or more nickel salts or its hydrate form as nickel source.The present invention adopts ethylene glycol as solvent.
(2) sodium borohydride is dissolved in ethylene glycol, then adds to the ethylene glycol solution of above-mentioned nickel salt, return stirring reaction.Preferably, sodium borohydride is dissolved in ethylene glycol, through abundant, stirs until solution is added to the ethylene glycol solution of nickel salt again after gushing out without obvious bubble.More preferably, to it, add again the ethylene glycol solution of sodium borohydride after first the ethylene glycol solution of described nickel salt being heated to 150 ℃～200 ℃.Reflux temperature can be 150 ℃～200 ℃, and return time can be 30min ~ 2h.In addition, the mol ratio of nickel salt and sodium borohydride can be 1:4～1:13.For example, when adopting Nickelous nitrate hexahydrate as nickel salt, while adopting sodium borohydride as precipitation agent, the mass ratio of Nickelous nitrate hexahydrate and sodium borohydride can be 1:1 ~ 3:8.
(3) after reaction finishes, be cooled to room temperature, products therefrom passed through successively centrifugal, filter, washing, ethanol is washed, and three times repeatedly, finally dry and obtain presoma, presoma is nickel alkoxide through XRD analysis herein.
(4) by gained presoma through thermal treatment, for example thermal treatment 2～4h at 250 ℃～300 ℃, can obtain high-ratio surface porous multi-stage oxidizing nickel nano material.
Prepared nickel oxide nano powder is mixed and spread upon on collector with conductive agent, binding agent, utilize three-electrode system to study its chemical property.Concrete operations are as follows:
(1) after the ratio of 7:2:1 is mixed active material nickel oxide, conduction charcoal acetylene black, polyfluortetraethylene of binding element in mass ratio, splash into a small amount of ethanol, grind evenly.
(2) slurry obtaining is dry in 60～100 ℃ of baking ovens, obtain electrode materials.
(3) get resulting electrode materials 3mg, evenly spread upon two about 1cm of area
2nickel foam on, draw nickel sheet wire, be pressed into electrode.
(4) take the electrode of above-mentioned preparation as working electrode, SCE as reference electrode, platinum filament is as being electrolytic solution to electrode, 2M KOH, forms three-electrode system.Adopt the method for cyclic voltammetry and constant current charge-discharge to test its chemical property.Its test result can be referring to Fig. 5～8 and 10.
Experimental results show that the synthetic high-ratio surface porous nickel oxide of the present invention does electrode materials and have excellent chemical property, can be used for preparing height ratio capacity fake capacitance electrical condenser.
Nickel oxide electrode material its preparation method provided by the invention has following features:
(1) adopt sodium borohydride as novel alkaline precipitation agent, sodium borohydride is used as reductive agent all the time, in the present invention, be first dissolved in ethylene glycol, reduce reductibility, be only applied as alkaline precipitating agent, because it dissolves rear aobvious weakly alkaline, can make nickel hydroxide homogeneous nucleation, and sodium borohydride may releasing hydrogen gas in ethylene glycol, can introduce a large amount of holes in particle growth process, so nickel oxide uniform microstructure, the porous of generation and there is larger specific surface area.
(2) utilization ratio that active material is higher and the fast transport of electrolyte ion have been demonstrate,proved in the high-specific surface area of nickel oxide and porousness quality guarantee.
(3) the porous multilevel hierarchy of nickel oxide can prevent the agglomeration traits of nano material in working cycle.
(4) in the preparation process of nickel oxide, do not introduce any tensio-active agent or soft or hard template, and only need simple reflux device, the reaction times is short, and technique is simple, and cost is low.
(5) specific storage is high, good rate capability.The nickel oxide electrode of preparation is under the current density of 2A/g, and specific storage is up to 972F/g, and during 15A/g, specific storage also reaches 930F/g, has shown excellent high rate performance.
(6) good cycling stability.The nickel oxide electrode of preparation is under the current density of 4A/g, and specific storage is 1016F/g, after activation, can reach 1400F/g, substantially unattenuated after 1000 circulations.
Further exemplify embodiment below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention., those skilled in the art can do in suitable scope and be selected by explanation herein the temperature of reaction that following example is concrete, time charging capacity etc. are only also examples in OK range,, and do not really want to be defined in the below concrete numerical value of example.
Get 0.6g Nickelous nitrate hexahydrate and be dissolved in 100mL ethylene glycol, through being heated to 190 ℃.1.2g sodium borohydride is dissolved in ethylene glycol, stirs until gush out without bubble, join in the solution of above-mentioned heating, return stirring 1h, is cooled to room temperature.Subsequently resulting product is washed through centrifugal, filtration, washing, ethanol successively, three times repeatedly, finally dried and obtain presoma.The presoma of gained is obtained being comprised of sheet structure at 250 ℃ of calcining 2h, there is the multistage subsphaeroidal nickel oxide nano material of high-ratio surface porous.By aforesaid method, prepared nickel oxide nano powder and conductive agent, binding agent are mixed and spread upon collector and form electrode.
Fig. 1 is the XRD figure spectrum of the nickel oxide that makes of the present embodiment and presoma nickel alkoxide thereof, and wherein curve a is the XRD spectra of the nickel oxide that makes of the present embodiment, coincide with the standard diagram of nickel oxide, shows that the product that this law makes is pure nickel oxide; Curve b is the XRD figure spectrum of presoma nickel alkoxide.
Fig. 2 is the transmission electron microscope photo of the nickel oxide that makes of the present embodiment, can see clearly that nickel oxide is what sheet structure, consist of, and diameter is the subsphaeroidal structure of 150-300nm left and right.
Fig. 3 is the stereoscan photograph of the nickel oxide that makes of the present embodiment, can see clearly that nickel oxide is to pile up the multistage globosity of the porous forming by nanometer sheet, and the size of spheroidal particle is in 150-300nm left and right.
Isothermal adsorption curve and the pore size distribution curve of Fig. 4 A and Fig. 4 B nickel oxide that the present embodiment makes respectively, the specific surface area of nickel oxide is 414cm
2/ g, even aperture distribution, in 3.8nm left and right.
Fig. 5 is the discharge curve under the different current densities that obtain in the constant current charge-discharge test of the electrode prepared of nickel oxide that the present embodiment makes, can find out in 0.2V left and right and have a discharge platform, and current density is higher, and discharge time is shorter.
Fig. 6 is the specific storage that obtains in the constant current charge-discharge test of the electrode prepared of nickel oxide that the present embodiment makes and the relation curve of current density, can find out under the current density of 2A/g, specific storage is up to 972F/g, during 15A/g, specific storage also can reach 930F/g, has high ratio electric capacity and good high rate performance.
Fig. 7 is nickel oxide the electrode ratio electric capacity that 1000 times circulate under the current density of 4A/g of preparing and the relation curve that discharges and recharges number of times that the present embodiment makes, can find out that material can reach 1400F/g after activated, and almost not decay after 1000 circulations.
Fig. 8 is the electrode energy density prepared of nickel oxide that the present embodiment makes and the relation curve of power density, can find out under the power density of 0.5Wh/Kg, energy density can reach 33.752KW/Kg, under the high power density of 3.75Wh/Kg, energy density also can, up to 32.29KW/Kg, have good chemical property.
Get 0.6g Nickelous nitrate hexahydrate and be dissolved in 100mL ethylene glycol, through being heated to 190 ℃.1.2g sodium borohydride is dissolved in ethylene glycol, stirs until gush out without bubble, join in the solution of above-mentioned heating, return stirring 1h, is cooled to room temperature.Subsequently resulting product is washed through centrifugal, filtration, washing, ethanol successively, three times repeatedly, finally dried and obtain presoma.The presoma of gained is obtained to the multistage nickel oxide nano material of high-ratio surface porous at 250 ℃ of calcining 4h, the nickel oxide making is prepared into its chemical property of electrode test, under the current density of 2A/g, specific storage is that 896F/g(is referring to Figure 10).
Get 0.6g Nickelous nitrate hexahydrate and be dissolved in 100mL ethylene glycol, through being heated to 190 ℃.1.2g sodium borohydride is dissolved in ethylene glycol, stirs until gush out without bubble, join in the solution of above-mentioned heating, return stirring 1h, is cooled to room temperature.Subsequently resulting product is washed through centrifugal, filtration, washing, ethanol successively, three times repeatedly, finally dried and obtain presoma.The presoma of gained is obtained to the multistage nano material of high-ratio surface porous at 300 ℃ of calcining 2h, the nickel oxide making is prepared into its chemical property of electrode test, under the current density of 2A/g, specific storage is that 636F/g(is referring to Figure 10).
Comparative example 1
Get 0.6g Nickelous nitrate hexahydrate and be dissolved in 100mL ethylene glycol, through being heated to 190 ℃.1.2g sodium borohydride is dissolved in ethylene glycol, stirs until gush out without bubble, join in the solution of above-mentioned heating, return stirring 1h, is cooled to room temperature.Subsequently resulting product is washed through centrifugal, filtration, washing, ethanol successively, three times repeatedly, finally dried and obtain presoma.The presoma of gained is obtained to the multistage nano material of high-ratio surface porous at 200 ℃ of calcining 2h, but XRD figure spectrum shows that product is not nickel oxide (referring to Fig. 9), but the peak of corresponding presoma, be prepared into its chemical property of electrode test, under the current density of 2A/g, specific storage is 1364F/g, but when 15A/g, specific storage is 720F/g, high rate performance poor (referring to Figure 10).
Comparative example 2
Get 0.6g Nickelous nitrate hexahydrate and be dissolved in 100mL ethylene glycol, through being heated to 190 ℃.1.2g sodium hydroxide is dissolved in ethylene glycol, stirs until the obvious bubble of nothing is gushed out, join in the solution of above-mentioned heating, return stirring 1h, is cooled to room temperature.Subsequently resulting product is washed through centrifugal, filtration, washing, ethanol successively, three times repeatedly, finally dried and obtain presoma.The presoma of gained is obtained to the multistage nickel oxide nano material of high-ratio surface porous at 250 ℃ of calcining 2h, the nickel oxide making is prepared into its chemical property of electrode test, under the current density of 2A/g, specific storage is that 520F/g(is referring to Figure 10).
Industrial applicability: the simple controlled applicable scale production of method preparation technology of the present invention, the nickel oxide making has high specific surface area and presents porousness, and specific storage is high, forthright good, good cycling stability doubly, especially the applicable electrode materials of making ultracapacitor, again wide application prospect.
Claims (8)
1. a preparation method with the nickel oxide material of superelevation specific storage, is characterized in that, comprising:
The ethylene glycol solution that the ethylene glycol solution of precipitation agent is added to nickel salt, return stirring obtains presoma; And
At more than 250 ℃ temperature, described in thermal treatment, presoma obtains described nickel oxide material;
Wherein, described precipitation agent is sodium borohydride.
2. preparation method according to claim 1, is characterized in that, comprising:
Described precipitation agent is added in ethylene glycol, fully stir until gush out to form the ethylene glycol solution of described precipitation agent without obvious bubble.
3. preparation method according to claim 1 and 2, is characterized in that, the mol ratio of described nickel salt and precipitation agent is 1:4～1:13.
4. preparation method according to claim 1 and 2, is characterized in that, the ethylene glycol solution of described nickel salt is heated to it, add after 150～200 ℃ again to the ethylene glycol solution of described precipitation agent.
5. preparation method according to claim 1 and 2, is characterized in that, described nickel salt is nickelous nitrate and/or its hydrate, single nickel salt and/or its hydrate, nickelous chloride and/or its hydrate and/or nickelous bromide and/or its hydrate.
6. preparation method according to claim 5, is characterized in that, described nickel salt is Nickelous nitrate hexahydrate.
7. preparation method according to claim 1 and 2, is characterized in that, the temperature of return stirring is 150～200 ℃, and the time of return stirring is 30 minutes～2 hours.
8. preparation method according to claim 1 and 2, is characterized in that, heat treated temperature is 250～300 ℃, and the heat treated time is 2～4 hours.
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| CN101665883A (en) * | 2009-10-19 | 2010-03-10 | 浙江大学 | Method for preparing nano-porous block of Fe-Sn intermetallic compound |
| CN101950680A (en) * | 2010-08-27 | 2011-01-19 | 湖北长海新能源科技有限公司 | Nano nickel oxide composite electrode for super capacitor and preparation method thereof |
| EP2634783A1 (en) * | 2010-10-27 | 2013-09-04 | Ocean's King Lighting Science&Technology Co., Ltd. | Composite electrode material, manufacturing method and application thereof |
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| CN101553431A (en) * | 2006-07-19 | 2009-10-07 | 通用汽车环球科技运作公司 | Method of making NiO and Ni nanostructures |
| CN1944276A (en) * | 2006-10-19 | 2007-04-11 | 上海大学 | Process for preparing nano nickel oxide electrode for super capacitor |
| CN101665883A (en) * | 2009-10-19 | 2010-03-10 | 浙江大学 | Method for preparing nano-porous block of Fe-Sn intermetallic compound |
| CN101950680A (en) * | 2010-08-27 | 2011-01-19 | 湖北长海新能源科技有限公司 | Nano nickel oxide composite electrode for super capacitor and preparation method thereof |
| EP2634783A1 (en) * | 2010-10-27 | 2013-09-04 | Ocean's King Lighting Science&Technology Co., Ltd. | Composite electrode material, manufacturing method and application thereof |
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Application publication date: 20140326 |