CN109742396A - A kind of nitride porous cobalt and its preparation method and application - Google Patents
A kind of nitride porous cobalt and its preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of nitride porous cobalt; belong to technical field of battery electrode materials, comprising the following steps: under protective atmosphere, cobalt source, nitrogen source, surfactant, complexing agent and high temperature resistant solvent are mixed; nitridation reaction is carried out, nitride porous cobalt is obtained；The pressure of the nitridation reaction is 600~870MPa, and temperature is 380~500 DEG C.The present invention specific pressure and at a temperature of, decompose nitrogen source, generate activated nitrogen atom, a part of activated nitrogen atom restores cobalt atom, forms active cobalt atom, and the active cobalt atom of generation is again with remaining activated nitrogen atom ining conjunction with, generation cobalt nitride.Since reaction generates soluble inorganic salt, it is dissolved in water after washing, and cobalt nitride is not soluble in water, to form nitride porous cobalt.The cobalt nitride that the present invention obtains has porous structure and higher specific discharge capacity, avoids volume change during lithium ion is embedded in and is deviate from as lithium ion battery negative material, and obtained cycle performance of lithium ion battery is good.
Description
Technical field
The present invention relates to technical field of battery electrode materials, in particular to a kind of nitride porous cobalt and preparation method thereof and answer
With.
Background technique
Rechargeable lithium ion batteries are a kind of novel energy storage devices, because its weight and volume energy is high, power density is high,
It has extended cycle life, the advantages such as self-discharge performance is low, it is considered to be most one of the energy-storage system of application prospect is widely used in just
Take the fields such as formula electronic equipment and electric car.The actual energy density of commercial li-ion battery at present (graphite is anode material)
It is unable to satisfy the growing demand of high-power not plug-in electronic product.In order to meet this requirement, to high capacity newly developed,
The key of high stability lithium ion battery is the exploration to new electrode material.
As lithium ion battery negative material, transition metal nitride is good because having superior chemical property
The features such as chemical stability and the extensive concern for causing everybody.The specific electron configuration of transition elements (IIIB-VIII race) exists
A part of d track can be captured in valence electron, when nitride participates in redox reaction, the multivalent state of generation can be deposited effectively
Energy storage capacity.In addition to this, transition metal nitride also has broad application prospects, and is such as applied to supercapacitor, fuel electricity
Pond catalyst, semiconductor, Hydrobon catalyst and electro-catalysis produce the catalyst etc. of hydrogen.The research of transition metal nitride has become
For one of the hot spot of materials science field research.
However, transition metal nitride material volume change during lithium ion is embedded in and is deviate from is serious, cyclicity
Can be not ideal enough, this is a huge problem for being applied to lithium ion battery.Common solution is and graphite
Alkene is compound, however this method can not only reduce the specific capacity of material, but also graphene is expensive, is not particularly suited for actually answering
With.
Summary of the invention
In view of this, the present invention mentions it is an object of that present invention to provide a kind of nitride porous cobalt and its preparation method and application
The nitride porous cobalt of confession has porous structure and higher specific discharge capacity, and preparation method is simple.Wherein porous structure can be with
Solve the problems, such as that cobalt nitride volume expansion is brought, activation time needed for reducing lithium ion battery material impedance and shortening.By its
The cycle performance of lithium ion battery obtained as lithium ion battery negative material is good.
The present invention provides a kind of preparation methods of nitride porous cobalt, comprising the following steps:
Under protective atmosphere, cobalt source, nitrogen source, surfactant, complexing agent and high temperature resistant solvent are mixed, nitrogenize anti-
It answers, obtains nitride porous cobalt；The pressure of the nitridation reaction is 600~870MPa, and temperature is 380~500 DEG C.
Preferably, the cobalt source includes cobalt acetate, cobalt chloride or cobaltous sulfate.
Preferably, the nitrogen source includes sodium azide.
Preferably, the surfactant includes cetyl trimethylammonium bromide, lauryl sodium sulfate or hexadecane
Base trimethyl ammonium chloride.
Preferably, the complexing agent includes sodium citrate, sodium alginate or polyvinylpyrrolidone.
Preferably, the high temperature resistant solvent includes benzene or toluene.
Preferably, the cobalt source, nitrogen source, surfactant, complexing agent mass ratio be 16~82:13~71:1~18:1
~18.
Preferably, the pressure of the nitridation reaction is 700~800MPa, and temperature is 420~450 DEG C
The present invention also provides the nitride porous cobalts that above method preparation method is prepared.
The nitride porous cobalt being prepared the present invention also provides above-mentioned preparation method is in lithium ion battery negative material
Application.
Advantageous effects: the present invention provides a kind of preparation methods of nitride porous cobalt, comprising the following steps: is protecting
Under atmosphere, cobalt source, nitrogen source, surfactant, complexing agent and high temperature resistant solvent are mixed, nitridation reaction is carried out, obtains porous nitrogen
Change cobalt；The pressure of the nitridation reaction is 600~870MPa, and temperature is 380~500 DEG C.The present invention is in specific pressure and temperature
Under degree, nitrogen source is decomposed, generate activated nitrogen atom, a part of activated nitrogen atom first restores cobalt atom, forms active cobalt
Atom, the active cobalt atom of generation in conjunction with remaining activated nitrogen atom, generate cobalt nitride again.Due to nitridation reaction can generate can
Soluble inorganic salt can be dissolved in water removal after water washing, and cobalt nitride is insoluble in water.So nitrogenizing after water washing
Cobalt can leave hole, form nitride porous cobalt.The present invention can a step obtain nitride porous cobalt, preparation method is simple.As lithium
Ion battery cathode material avoids volume change during lithium ion is embedded in and is deviate from, and obtained lithium ion battery follows
Ring performance is good.
Detailed description of the invention
Fig. 1 is the electron-microscope scanning figure of nitride porous cobalt obtained in embodiment 1；
Fig. 2 is the graph of pore diameter distribution of nitride porous cobalt obtained in embodiment 1；
Fig. 3 is to scan by lithium ion battery made from negative electrode material of the nitride porous cobalt that embodiment 2 obtains in 0.1mV/s
Cyclic voltammetry curve under rate；
Fig. 4 is the XRD diagram for the cobalt nitride that embodiment 2 obtains；
It is lithium ion battery made from negative electrode material in 0.5Ag that Fig. 5, which is using the nitride porous cobalt that embodiment 3 obtains,-1Electricity
The case where specific discharge capacity of current density changes with circulating ring number；
Fig. 6 is nitride porous cobalt electron-microscope scanning figure obtained in embodiment 4.
Specific embodiment
The present invention provides a kind of preparation methods of nitride porous cobalt, comprising the following steps:
Under protective atmosphere, cobalt source, nitrogen source, surfactant, complexing agent and high temperature resistant solvent are mixed, nitrogenize anti-
It answers, obtains nitride porous cobalt；The pressure of the nitridation reaction is 600~870MPa, and temperature is 380~500 DEG C.
The present invention is not particularly limited the protective atmosphere, selects protective atmosphere well known to those skilled in the art i.e.
It can.The preferred nitrogen of the present invention is protective atmosphere.
In the present invention, the cobalt source preferably includes cobalt acetate, cobalt chloride or cobaltous sulfate, more preferably includes cobalt acetate；Institute
It states nitrogen source and preferably includes sodium azide；The surfactant preferably includes cetyl trimethylammonium bromide, dodecyl sulphur
Sour sodium or hexadecyltrimethylammonium chloride；The complexing agent preferably includes lemon acid sodium, sodium alginate or polyvinylpyrrolidone,
It more preferably include sodium citrate；The high temperature resistant solvent preferably includes benzene or toluene.
In the present invention, the cobalt source, nitrogen source, surfactant, complexing agent mass ratio be preferably 16~82:13~
71:1~18:1~18, more preferably 30~60:20~50:5~15:5~15, most preferably 40~50:30~40:7~10:
7~10.
The present invention is not particularly limited the dosage of the high temperature resistant solvent, selects dosage well known to those skilled in the art
?.
In the present invention, the pressure of the nitridation reaction is 600~870MPa, preferably 700~800MPa, the nitridation
The temperature of reaction is 380~500 DEG C, preferably 420~450 DEG C；The time of the nitridation reaction is preferably 6~48h, more preferably
For 16~36h, most preferably 20~30h.
The method that the present invention mixes cobalt source, nitrogen source, surfactant, complexing agent and high temperature resistant solvent does not have special limit
It is fixed, select mixed method well known to those skilled in the art.The present invention is preferably stirred.In the present invention, described
The time of stirring is preferably 10~30min, more preferably 15~20min；The present invention is not particularly limited the rate of stirring, choosing
With stirring rate well known to those skilled in the art.
The present invention specific pressure and at a temperature of, decompose nitrogen source, generate activated nitrogen atom, a part of activated nitrogen atom
First cobalt atom is restored, forms active cobalt atom, the active cobalt atom of generation in conjunction with remaining activated nitrogen atom, is given birth to again
At cobalt nitride.Since nitridation reaction can generate soluble inorganic salt, it is dissolved in water removal after water washing, and cobalt nitride is insoluble
In water to form nitride porous cobalt.The active cobalt atom of generation is also the catalyst of nitridation reaction simultaneously, avoids other urge
The addition of agent avoids the post-processing step for removing other catalyst, simplifies preparation method.
In the present invention, the nitridation reaction preferably carries out in closed reactors.In the present invention, the cobalt source,
The volume of gained mixed liquor is preferably the 40 of reaction kettle volume after nitrogen source, surfactant, complexing agent and the mixing of high temperature resistant solvent
~65%.In the present invention, before starting the reaction, the pressure in reactor be normal pressure, due to reactor be it is closed, with anti-
The progress answered, the pressure in reactor gradually rise, pressure needed for providing nitridation reaction.In the present invention, described closed anti-
Answering device is preferably closed stainless steel cauldron.The present invention can provide high pressure due to reacting in sealing reaction kettle
Reaction condition prepares cobalt nitride at a lower temperature, avoids routine and needs to nitrogenize oxygen under the conditions of high temperature (> 700 DEG C)
Change cobalt.
It in the present invention, further preferably include that gained nitridation reaction liquid is successively cooled to room temperature, is washed after the nitridation reaction
It washs, filter and dries, obtain nitride porous cobalt.
The present invention is not particularly limited cooling rate, and cooling well known to those skilled in the art is selected to consider carefully.
In the present invention, the washing preferably successively includes that alcohol is washed and washed.
In the present invention, the detergent that the alcohol is washed is preferably ethyl alcohol.The method and number that the present invention washes alcohol are without spy
It is different to limit, select washing methods well known to those skilled in the art.The present invention goes to be dissolved in organic solvent by alcohol washout
Impurity.
In the present invention, the washing preferably makes to be washed with distilled water.The present invention does not have the method and number of washing
Particular determination selects method well known to those skilled in the art and number.The present invention is dissolved in the miscellaneous of water by washing to remove
Matter.
In the present invention, each alcohol is all washed after washing, and the number that the successively alcohol is washed and washed is preferably 3~5 times.
In the present invention, the temperature of the drying is preferably 60~100 DEG C, and more preferably 80~90 DEG C；The drying
Time is preferably 6~12h, more preferably 8~10h.The present invention is not particularly limited dry method, selects art technology
Drying means known to personnel, in the present invention, it is preferred to for vacuum drying.
The present invention also provides the nitride porous cobalts that above method preparation method is prepared.
In the present invention, there are large number of orifices in the pore diameter range of 1~2nm and 3~5nm for the cobalt nitride, and there is micropore to be situated between
Pore structure；The value of the quality specific volume of the cobalt nitride is 38.8515m2/g.
The nitride porous cobalt being prepared the present invention also provides above-mentioned preparation method is in lithium ion battery negative material
Application.
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
In nitrogen-protecting glove box, by 0.5g cetyl trimethylammonium bromide, 0.2g sodium citrate, 1g sodium azide
It is added sequentially in 33.3mL benzene, stirs 10 minutes with 0.5g cobalt acetate, it is anti-that mixture is put into the stainless steel that volume is 50mL
It answers in kettle, seals；Reaction kettle is placed in crucible furnace again, heats 6 hours at 400 DEG C, is then naturally cooled to reaction kettle
Room temperature takes out mixture.Said mixture is successively used to dehydrated alcohol and distillation water washing 3 times, filtering is then true at 60 DEG C
Sky is 12 hours dry, and nitride porous cobalt can be obtained.
Fig. 1 is the electron-microscope scanning figure of nitride porous cobalt obtained in embodiment 1, can clearly be found out by Fig. 1 and to be synthesized
Cobalt nitride is in tufted, and the length is between 0.2~2 μm.
Fig. 2 be embodiment 1 obtained in nitride porous cobalt graph of pore diameter distribution, as seen from Figure 2 1~2nm and 3~
The pore diameter range of 5nm illustrates that the cobalt nitride of synthesis has microcosmic meso-hole structure, it is swollen to can solve cobalt nitride volume there are large number of orifices
The problem that expansible band comes, and porous structure can reduce material impedance and shorten required activation time.
Embodiment 2
In nitrogen-protecting glove box, by 0.5g hexadecyltrimethylammonium chloride, 0.2g sodium citrate, 1g sodium azide
It is added sequentially in 33.3mL benzene, stirs 20 minutes with 0.5g cobalt chloride, it is anti-that mixture is put into the stainless steel that volume is 50mL
It answers in kettle, seals；Reaction kettle is placed in crucible furnace again, heats 24 hours at 420 DEG C, is then naturally cooled to reaction kettle
Room temperature takes out mixture.Said mixture is successively used to dehydrated alcohol and distillation water washing 5 times, filtering is then true at 80 DEG C
Sky is 10 hours dry, and nitride porous cobalt can be obtained.
Preparation method of lithium ion battery:
The preparation of working electrode: by prepared nitride porous cobalt and conductive black Super-P, 5% PVDF (inclined difluoro
Ethylene) N-methyl pyrrolidone solution mixing, wherein nitride porous cobalt, conductive black Super-P, PVDF mass ratio be 8:1:
1.Excessive N-methyl pyrrolidones is added by mixed pulp dilution, is stirred for 24 hours under the conditions of Room-temperature seal.By gained black
Slurry is coated uniformly on the copper foil weighed in advance, is weighed again after 80 DEG C of vacuum dry 12h, is calculated according to ratio living in electrode
The amount of property substance, it is ensured that active material is in 1.5mg cm-1Left and right.
The assembling of battery: assembling whole process all carries out in the glove box for having argon gas to protect.Battery assembly model uses
Commercialized 2025 type button cell is to electrode, 1molL with pour lithium slice-1LiPF6Dimethyl carbonate and ethylene carbonate
(volume ratio 1:1) solution is electrolyte, and polymer porous film is diaphragm.It is finally sealed with sealing machine, it is ensured that the leakproofness of battery.
Fig. 3 is to scan by lithium ion battery made from negative electrode material of the nitride porous cobalt that embodiment 2 obtains in 0.1mV/s
Cyclic voltammetry curve under rate.It can be seen from the figure that cyclic voltammetry curve there are apparent redox peaks, show that there are oxygen
Change reduction reaction, the second circle is approximate with third circle circulation to be overlapped, and shows there is good cyclical stability.
Fig. 4 is the XRD diagram for the cobalt nitride that embodiment 2 obtains, as shown in Figure 4, nitride porous cobalt knot obtained in embodiment 2
Crystalline substance is preferable, is hexagonal phase crystal.
Embodiment 3
In nitrogen-protecting glove box, by 0.5g cetyl trimethylammonium bromide, 0.5g sodium citrate, 1g Azide
Sodium, 0.5g cobalt chloride are added sequentially in 33.3mL benzene, are stirred 30 minutes, and it is anti-that mixture is put into the stainless steel that volume is 50mL
It answers in kettle, seals；Reaction kettle is placed in crucible furnace again, heats 48 hours at 400 DEG C, is then naturally cooled to reaction kettle
Room temperature takes out mixture.Said mixture is successively used to dehydrated alcohol, distillation water washing 6 times, filtering is then true at 100 DEG C
Sky is 6 hours dry, obtains nitride porous cobalt.
It is lithium ion battery made from negative electrode material in 0.5Ag that Fig. 5, which is using the nitride porous cobalt that embodiment 3 obtains,-1Electricity
The case where specific discharge capacity of current density changes with circulating ring number, (the nitride porous cobalt that embodiment 3 obtains is negative electrode material preparation
The method of lithium ion battery is identical as the method in embodiment 2) as shown in Figure 5, the cobalt nitride obtained using embodiment 3 is electrode material
The lithium ion battery of material has extraordinary cycle performance, and capacity reaches after having carried out 150 cycle charge-discharges
774.7mAh/g。
Embodiment 4
In nitrogen-protecting glove box, by 0.5g cetyl trimethylammonium bromide, 0.2g sodium citrate, 1g sodium azide
It is added sequentially in 33.3mL benzene, stirs 30 minutes with 1g cobalt chloride, mixture is put into the stainless steel reaction that volume is 45mL
In kettle, sealing；Reaction kettle is placed in crucible furnace again, is heated 20 hours at 450 DEG C, then naturally cools to room to reaction kettle
Temperature takes out mixture.Said mixture is successively used to dehydrated alcohol and distillation water washing 4 times, filtering is then true at 100 DEG C
Sky is 8 hours dry, and nitride porous cobalt can be obtained.
Fig. 6 is nitride porous cobalt electron-microscope scanning figure obtained in embodiment 4.It will be appreciated from fig. 6 that more obtained in embodiment 4
Hole cobalt nitride is in bulk.By Fig. 1 and Fig. 6 it is found that reaction time and temperature will affect the pattern of product, different-shape will affect hole
Road structure, and then influence the battery performance as negative electrode of lithium ion battery.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of nitride porous cobalt, comprising the following steps:
Under protective atmosphere, nitridation reaction is carried out after cobalt source, nitrogen source, surfactant, complexing agent and high temperature resistant solvent are mixed,
Obtain nitride porous cobalt；The pressure of the nitridation reaction is 600~870MPa, and temperature is 380 DEG C~500 DEG C.
2. preparation method according to claim 1, which is characterized in that the cobalt source includes cobalt acetate, cobalt chloride or sulfuric acid
Cobalt.
3. preparation method according to claim 1, which is characterized in that the nitrogen source includes sodium azide.
4. preparation method according to claim 1, which is characterized in that the surfactant includes cetyl trimethyl
Ammonium bromide, lauryl sodium sulfate or hexadecyltrimethylammonium chloride.
5. preparation method according to claim 1, which is characterized in that the complexing agent includes sodium citrate, sodium alginate
Or polyvinylpyrrolidone.
6. preparation method according to claim 1, which is characterized in that the high temperature resistant solvent includes benzene or toluene.
7. preparation method described in any one according to claim 1~6, which is characterized in that the cobalt source, nitrogen source, surface are living
Property agent and complexing agent mass ratio be 16~82:13~71:1~18:1~18.
8. preparation method according to claim 1, which is characterized in that the pressure of the nitridation reaction is 700~800MPa,
Temperature is 420~450 DEG C.
9. the nitride porous cobalt that preparation method described in claim 1~8 any one is prepared.
10. the nitride porous cobalt that preparation method described in claim 1~8 any one is prepared is negative as lithium ion battery
The application of pole material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110180576A (en) * | 2019-06-13 | 2019-08-30 | 东北师范大学 | Hard template method prepares the method and application of porous rich nitrogen cobalt nitride |
| CN114214634A (en) * | 2021-11-05 | 2022-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of graphite plate loaded porous nanosheet cobalt nitride-zinc oxide, product and application |
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| CN103021672B (en) * | 2012-12-12 | 2016-01-06 | 常州大学 | A kind of spherical metal nitride material and preparation method thereof and application |
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| CN103021672B (en) * | 2012-12-12 | 2016-01-06 | 常州大学 | A kind of spherical metal nitride material and preparation method thereof and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110180576A (en) * | 2019-06-13 | 2019-08-30 | 东北师范大学 | Hard template method prepares the method and application of porous rich nitrogen cobalt nitride |
| CN114214634A (en) * | 2021-11-05 | 2022-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of graphite plate loaded porous nanosheet cobalt nitride-zinc oxide, product and application |
| CN114214634B (en) * | 2021-11-05 | 2023-11-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation, product and application of graphite plate loaded porous nano-sheet cobalt nitride-zinc oxide |
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Application publication date: 20190510 |