CN109904428A - A kind of preparation method of ferrous selenide/carbon composite - Google Patents
A kind of preparation method of ferrous selenide/carbon composite Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of ferrous selenide/carbon composite, comprising the following steps: (1) is added to in the dissolution of dopamine source and the solvent insoluble to source of iron dopamine source with source of iron, removes solvent after mixing, obtain powder A；(2) powder A is pyrolyzed in 400~700 DEG C under vacuum, obtains powder B；(3) powder B is mixed with selenium powder, is pyrolyzed at 600~900 DEG C, obtain ferrous selenide/carbon composite.
Description
Technical field
The invention belongs to ceramic technology fields, and in particular to a kind of ferrous selenide/carbon composite function ceramics and predecessor are former
Position cladding prepares ferrous selenide/carbon composite function ceramics preparation method.
Background technique
Currently, lithium ion battery is the best high-energy battery system of development prospect, but with industries such as number, traffic numbers
Lithium ion battery dependence is aggravated, the problem of lithium will face resource critical shortage.The research and development of sodium-ion battery can be with
Alleviate the limited development of the battery as caused by lithium resource shortage to a certain extent.If developed on this basis cell performance
Excellent, safety and stability the electrode material of energy, sodium-ion battery have bigger market competition advantage than lithium ion battery.Metallic selenium
The one kind of compound as metal sulfide, since selenium atom is bigger than sulphur atom diameter, metallicity is stronger, so that metal selenide
There is bigger interlamellar spacing and higher conductivity compared with metal sulfide.Two ferrous selenide FeSe2Energy gap (Eg=1.0eV) compared with
Narrow, conductivity is higher, with FeS2Crystal is similar, has the potentiality applied to sodium-ion battery.Other selenizing iron compounds are same
Sample has similar electrochemistry storage sodium activity, therefore the research of metal selenide also needs constantly to explore and excavate at present.
Summary of the invention
In view of the above-mentioned problems, the purpose of the present invention is to provide a kind of ferrous selenide of electrochemical performance/carbon composite woods
Material and its preparation method and application.
In a first aspect, the present invention provides a kind of ferrous selenide/carbon composite, the ferrous selenide/carbon composite contains selenium
Change iron and carbon, the ferrous selenide/carbon composite is in uniform laminar structured, and is evenly distributed in lamellar structure poroid
Structure.
According to the present invention, ferrous selenide/carbon composite is in uniform laminar structured, and is uniformly distributed in lamellar structure
There is cavernous structure, this sheet porous structure can effectively facilitate electrolyte and diffuse to material surface, so that electric charge transfer speed
To accelerate, while guaranteeing that charge significantly shortens to the migration path of active component, charge can realize electrochemical reaction with fast transferring,
Compared with common chondritic, on the one hand porous sheet structure ensure that active component can come into full contact with electrolyte, separately
Between one side lamellar structure different zones be connected, can sheet surfaces realize charge migration, will not encounter chondritic each other it
Between electric charge transfer the case where being hindered by interface.Therefore material has higher theoretical capacity in charge and discharge process in the present invention,
Good rate capability and have preferable cyclical stability.
Preferably, ferrous selenide forms carbon coating in situ by carbon coating formation spherical morphology while between being grown on lamellar structure
Ferrous selenide composite ceramic material structure.
Preferably, the mass ratio of ferrous selenide and carbon is 7:1~3:1 in the ferrous selenide/carbon composite.
Preferably, it is described it is laminar structured in piece size be 200nm~3 μm, with a thickness of 10~50nm.
Preferably, the aperture in the cavernous structure is 5~30nm.
Preferably, the ferrous selenide is FeSe, FeSe2And Fe7Se8One or more of mixtures.
Second aspect, the present invention provide the preparation method of above-mentioned ferrous selenide/carbon composite, comprising the following steps:
(1) dopamine source is added to source of iron in the dissolution of dopamine source and the solvent insoluble to source of iron, is removed after mixing
Solvent is removed, powder A is obtained；
(2) powder A is pyrolyzed in 400~700 DEG C under vacuum, obtains powder B；
(3) powder B is mixed with selenium powder, is pyrolyzed at 600~900 DEG C, obtain ferrous selenide/carbon composite.
The present invention utilizes liquid phase coating method and high temperature solid-state method, by dopamine source at shorter time, higher temperature
The presoma with sheet porous structure pattern is prepared by high temperature solid state reaction with source of iron, then passes through solid phase selenization
Sheet porous structure iron selenium compound/carbon composite of uniform morphology is obtained, the electric conductivity for enhancing the material is conducive to.It should
Preparation method is easy to operate, low in cost, safe and non-toxic, is expected to realize industrialized production.
Preferably, the dopamine source is selected from least one of dopamine, DOPA amine salt, it is preferable that the dopamine
Salt is Dopamine hydrochloride.
Preferably, the source of iron is iron acylate, it preferably is selected from ferric oxalate, ferric acetate, ammonium ferric oxalate, ferric citrate
At least one of.
Preferably, the mass ratio of dopamine source and source of iron is 1:3~1:10 in step (1).
Preferably, the solvent is selected from least one of isopropanol, n-butanol, n-octyl alcohol, n-hexyl alcohol.
Preferably, the uniformly mixed mode be under the revolving speed with 100~800r/min stirring 8~for 24 hours, preferably 18
~for 24 hours.
Preferably, vacuum degree is -0.1~-0.05MPa in step (2), risen to the heating rate of 5~15 DEG C/min
400~700 DEG C, soaking time is 0.01~2 hour, preferably 0.1~2 hour.
Preferably, the mass ratio of powder B and selenium powder is 1:2~1:5 in step (3).
Preferably, vacuum degree is -0.1~-0.05MPa in step (3), risen to the heating rate of 5~15 DEG C/min
600~900 DEG C, soaking time is 0.01~2 hour, preferably 0.1~2 hour.
Preferably, filling into inert gas after heat preservation keeps reaction system pressure consistent with air pressure in step (3).
The third aspect, the present invention provide a kind of sodium-ion battery cathode, contain any of the above-described kind of ferrous selenide/carbon composite wood
Material.
Fourth aspect, the present invention provide a kind of sodium-ion battery, contain above-mentioned sodium-ion battery cathode.
Sodium-ion battery of the invention is low in cost, there is higher theoretical capacity, good rate capability in charge and discharge process
And there is preferable cyclical stability.
The present invention realizes the composite ceramics knot of carbon coating ferrous selenide by predecessor in-situ synthetic method in synthetic technology
Structure does not need many more manipulations, and the simple synthesis cost of synthetic technology is low, and preparation process is easy to regulate and control.Obtained by fabricated in situ of the present invention
Carbon and ferrous selenide form In-situ reaction structure in product, and material is tightly combined, and peomote its electric property and mechanical strength,
Important structure basis is provided in later period application for it.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) figure of the embodiment of the present invention 1.
Fig. 2 is scanning electron microscope (SEM) figure of the embodiment of the present invention 1.
Fig. 3 is the chemical property figure of the embodiment of the present invention 1.
Fig. 4 is scanning electron microscope (SEM) figure of the embodiment of the present invention 2.
Fig. 5 is the chemical property figure chemical property figure of the embodiment of the present invention 3,4.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
It is disclosed a kind of ferrous selenide/carbon composite.Fig. 2 shows the ferrous selenide/carbon of an embodiment of the present invention is compound
The SEM photograph of material.As shown in Fig. 2, ferrous selenide/the carbon composite is in uniform sheet/ball composite growth structure, and
Cavernous structure is evenly distributed in lamellar structure.Ferrous selenide/the carbon composite contains ferrous selenide and carbon, wherein ferrous selenide with
Little particle is dispersed in lamella porous carbon structure surface.Compared with sheet selenizing iron construction, the structure in the present invention can be effectively improved
The electric conductivity and charging-discharging structure stability of material further promote the storage sodium performance of material.
Laminar structured middle size can be 200nm~3 μm, and thickness can be 10~50nm.It, can be under this size
Guarantee to keep shorter charge diffusion path while material structure stability, to realize the electrochemical reaction process of high speed.Piece
Spacing in layer structure between lamella can be 10~200nm.
Aperture in cavernous structure can be 5~30nm.Under this size, material and electrolyte can be further promoted
Contact, shortens the path of charge migration, reduces the time of charge migration, accelerates electrochemical reaction process.
The ratio of ferrous selenide and carbon is adjustable in ferrous selenide/carbon composite, such as its mass ratio can be 10:1~3:1.?
It under the ratio, can effectively show the storage sodium performance of ferrous selenide itself, while by the supporting role of porous sheet carbon structure, make
Two kinds of structures promote mutually the performance of collaboration promotion composite construction entirety.
The chemical composition of ferrous selenide can be Fe7Se8、FeSe、FeSe2。Fe7Se8Can embody simultaneously the metallicity of material with
The storage sodium performance of selenides.
Ferrous selenide/carbon composite of the disclosure can be prepared with predecessor in-stiu coating method.Hereinafter, as an example, specific
Illustrate preparation method.
Firstly, being added in dopamine source with source of iron in the dissolution of dopamine source and the solvent insoluble to source of iron, mixing is equal
Solvent is removed after even, obtains powder A.Realize that dopamine to effective cladding on source of iron surface, only passes through the mistake by the process
Dopamine source just can be achieved to the uniformly cladding in situ of source of iron, the covered effect and direct mixed phase ratio in journey, and covered effect is more
Uniformly.
Dopamine source can be selected from least one of dopamine, DOPA amine salt.It is preferable to use DOPA amine salt, more preferably use
Dopamine hydrochloride.
Source of iron is necessary for iron acylate, while meeting the feature for being not readily dissolved in organic solvent.Iron acylate can be selected from
At least one of ferric oxalate, ferric acetate, ammonium ferric oxalate, ferric citrate.
The mass ratio of dopamine source and source of iron can be 1:3~1:10.It can guarantee Dopaminergics raw material in the quality ratio
To the abundant cladding of source of iron, and excessively later period carbon content will not be caused excessive because of cladding, lead to asking for composite construction capacity decline
Topic.
Solvent is not particularly limited, as long as to the dissolution of dopamine source and insoluble to source of iron, can make under this condition more
Ba Anyuan is coated on source of iron surface and source of iron does not change, and provides structure basis for the ferrous selenide synthesis of later period original position.Solvent
At least one of such as can be isopropanol, cyclohexanol, n-octyl alcohol.
Dopamine source is added to source of iron to after the dissolution of dopamine source and the solvent insoluble to source of iron, dopamine source is molten
Solution, source of iron keep insoluble, obtain suspension.Solvent is removed after the suspension is stirred a period of time, obtains powder A.Stirring bar
Part is, for example, the stirring 8 under the revolving speed of 100~800r/min~for 24 hours under blender, and preferably 18~for 24 hours.Remove the mode of solvent
It is evaporated after can be suction filtration.In powder A, dopamine source coats source of iron.
Then, powder A is pyrolyzed.Pyrolysis can carry out under vacuum conditions, and vacuum degree for example, -0.1~-
0.05MPa.Used device may be, for example, vacuum tube furnace.Vacuum tube furnace can be in multiple atmosphere and operated under vacuum.?
The lower heating rate that can efficiently control reaction of vacuum condition reaction.Pyrolysis temperature can be 400~700 DEG C.If temperature mistake
Low, then dopamine carbonizing degree is insufficient and degree of graphitization is lower；If temperature is excessively high, carburizing reagent acutely leads to carbon-coating knot
Structure destroys.In some embodiments, pyrolysis temperature can be risen to from room temperature with the heating rate of 5~15 DEG C/min.Using the liter
Warm rate can guarantee that the decomposition reaction of dopamine and source of iron carries out simultaneously, to meet the requirement of selenylation reaction in situ.When pyrolysis
Between can be 0.1~2 hour.
Powder A be also easy to produce during heat treatment it is laminar structured, and it is laminar structured in can be uniformly distributed many holes
Shape structure.Specifically, the hydroxyl and amino dehydrating condensation in dopamine source and dopamine source form sheet by auto polymerization and gather
Dopamine, further carbonization becomes nitrogen-doped carbon lamellar structure to this sheet poly-dopamine during high temperature pyrolysis, simultaneously
It decomposes gas evolution and brings cavernous structure.Source of iron surface coats more close partial dopamine, then in-stiu coating is in source of iron table
Face forms spherical carbon coating ferriferous oxide structure.Surface coated carbon does not separate in pyrolytic process with sheet carbon, passes through
The abundant key of polymerization early period connects, and continuous structure is still kept in carbonization pyrolytic process, thus forms porous sheet carbon and ball
The pattern of shape carbon-encapsulated iron oxide.After powder A pyrolysis, powder B is obtained.Contain Fe in powder B3O4/ C compound, the compound
In uniform laminar structured, and cavernous structure is evenly distributed in lamellar structure.
Then, by powder B and selenium powder hybrid reaction, ferrous selenide/carbon composite is obtained.
After powder B is reacted with selenium powder, ferriferous oxide is changed into iron selenides, and the microscopic appearance of powder B is kept not substantially
Become, i.e., ferrous selenide/carbon composite is also in uniform laminar structured, and cavernous structure is evenly distributed in lamellar structure.
The mass ratio of powder B and selenium powder can be 1:2~1:5.The selenium of ferriferous oxide can be effectively realized using the mass ratio
Change without remaining extra selenium powder.
Powder B can be carried out under vacuum conditions with reacting for selenium powder, and vacuum degree is, for example, -0.1~-0.05MPa.It is used
Device may be, for example, vacuum tube furnace.Vacuum tube furnace can be in multiple atmosphere and operated under vacuum.Under vacuum condition reaction
The heating rate of reaction can be efficiently controlled.Reaction temperature can be 600~900 DEG C.It, cannot abundant selenium if temperature is too low
Change, while remaining selenium and causing performance impairment in the product；If temperature is excessively high, prototype structure is damaged.In some embodiments,
Reaction temperature can be risen to from room temperature with the heating rate of 5~15 DEG C/min.Use the heating rate that sample can be guaranteed with steady
Selenylation reaction occurs for fixed reaction rate, and rate will lead to reaction side reaction slowly excessively and generate, selenium volatilization cause cannot effective selenizing,
Heating rate is too fast selenium powder can be made to liquefy after fail to spread the uniformity for just reacting, thus influencing product in time.When reaction
Between can be 1 hour.Inert gas such as argon gas etc. can be filled into after heat preservation keeps overpressure consistent with air pressure, to make
Suck-back, which is not easy, when obtaining in-furnace temperature decline penetrates into air impact product structure.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
3:1 in mass ratio disperses Dopamine hydrochloride and ammonium ferric oxalate in aqueous isopropanol, on magnetic stirring apparatus
Being uniformly mixed for 24 hours with the revolving speed stirring of 200r/min dissolves Dopamine hydrochloride, keeps ammonium ferric oxalate insoluble, obtains light green
Suspension, solution are evaporated after filtering, and obtain light green powder A1.
By powder A1 in low temperature tube furnace vacuum degree be (pressure gauge is -0.1MPa or so) under the conditions of from room temperature with 10
DEG C/min, 600 DEG C of pyrolysis 1h are heated to, ferriferous oxide/carbon matrix precursor powder B1 is obtained.
Product B1 and selenium powder are weighed according to mass ratio 1:2, product B1 and selenium powder grinding are placed on crucible, are packed into tubular type
Furnace simultaneously vacuumizes (pressure gauge is -0.1MPa or so), rises to 600 DEG C from room temperature with the heating rate of 5 DEG C/min, keeps the temperature 1h, protects
Argon gas is filled into after temperature makes overpressure zero.Obtain the compound selenizing iron composite material sodium-ion battery cathode of layer structure carbon
Material.
Resulting product particles Rigaku D/max2000PCX- x ray diffractometer x is analyzed into sample, discovery product contains
There is ferrous selenide (Fe7Se8), see Fig. 1.The JSM-6700F type scanning electron microscopy that resulting product Japan Electronics Corporation is produced
Mirror is observed, as shown in Figure 2, it can be seen that product is of uniform morphology laminar structured, and is uniformly divided in lamellar structure
The many cavernous structures of cloth.Observation is schemed by SEM it is found that the size of piece is 1~2 μm, with a thickness of 20~50nm.Hole in cavernous structure
Diameter is 20~30nm.
Embodiment 2
5:1 in mass ratio disperses Dopamine hydrochloride and ferric citrate in aqueous isopropanol, on magnetic stirring apparatus
It stirs 18h to be uniformly mixed, obtains light green suspension, solution is evaporated after filtering, and obtains light green powder A2.
By powder A2 in low temperature tube furnace vacuum degree be (pressure gauge is -0.08MPa or so) under the conditions of from room temperature with
15 DEG C/min, 700 DEG C of pyrolysis 1h are heated to, Fe is obtained3O4/ C forerunner powder B2.
Product B2 and selenium powder are weighed according to mass ratio 1:3, product B and selenium powder grinding are placed on crucible, are packed into tubular type
Furnace simultaneously vacuumizes (pressure gauge is -0.08MPa or so), rises to 700 DEG C from room temperature with the heating rate of 7 DEG C/min, keeps the temperature 1h, protects
Argon gas is filled into after temperature makes overpressure zero.Obtain the compound selenizing iron composite material sodium-ion battery cathode of layer structure carbon
Material.
The SEM figure of products therefrom is as shown in Figure 4, it can be seen that product is of uniform morphology laminar structured, and lamella
Many cavernous structures are uniformly distributed in structure.The size of piece is 2~3 μm, with a thickness of 40~50nm.Aperture in cavernous structure is
30~50nm.
Embodiment 3
8:1 in mass ratio disperses ferric oxalate and Dopamine hydrochloride in aqueous isopropanol, stirs on magnetic stirring apparatus
It is uniformly mixed for 24 hours, obtains light green suspension, solution is evaporated after filtering, and obtains light green powder A3.
By powder A3 in low temperature tube furnace vacuum degree be (pressure gauge is -0.06MPa or so) under the conditions of from room temperature with 7
DEG C/min, 500 degree of pyrolysis 1h are heated to, Fe is obtained3O4/ C forerunner powder B3.
Product B3 and selenium powder are weighed according to mass ratio 1:5, product B3 and selenium powder grinding are placed on crucible, are packed into tubular type
Furnace simultaneously vacuumizes (pressure gauge is -0.07MPa or so), rises to 900 DEG C from room temperature with the heating rate of 15 DEG C/min, keeps the temperature 1h,
Argon gas is filled into after heat preservation makes overpressure zero.It is negative to obtain the compound selenizing iron composite material sodium-ion battery of layer structure carbon
Pole material.
The structure and composition test result of products therefrom is similar to Example 1.
Embodiment 4
10:1 in mass ratio disperses ferric acetate and Dopamine hydrochloride in aqueous isopropanol, stirs on magnetic stirring apparatus
20h is uniformly mixed, and obtains light green suspension, solution is evaporated, and obtains light green powder A4.
By powder A4 in low temperature tube furnace vacuum degree be (pressure gauge is -0.06MPa or so) under the conditions of from room temperature with 5
DEG C/min, 400 DEG C of pyrolysis 1h are heated to, Fe is obtained3O4/ C forerunner powder B4.
Product B4 and selenium powder are weighed according to mass ratio 1:4, product B4 and selenium point grinding are placed on crucible, are packed into tubular type
Furnace simultaneously vacuumizes (pressure gauge is -0.06MPa or so), rises to 800 DEG C from room temperature with the heating rate of 10 DEG C/min, keeps the temperature 1h,
Argon gas is filled into after heat preservation makes overpressure zero.It is negative to obtain the compound selenizing iron composite material sodium-ion battery of layer structure carbon
Pole material.
The structure and composition test result of products therefrom is similar to Example 1.
Electrochemical property test
The resulting product of each embodiment is prepared into button sodium-ion battery, specific encapsulation step is as follows: will be active
After powder, conductive agent (super-p), bonding agent (carboxyl methyl cellulose) are according to the proportion grinding uniformly of mass ratio 8:1:1, system
At slurry, uniformly slurry is applied on copper foil with coating device, then in 80 DEG C of vacuum oven dry 12h.Later by electrode
Piece is assembled into sodium ion half-cell, carries out constant current charge-discharge test to battery using new prestige electrochemical workstation, test voltage is
0.01-3.0V, test current density size are 0.1-10A g-1, the test result of embodiment 1 is shown in Fig. 3, the test knot of embodiment 3
Fruit sees Fig. 5, and the test result of embodiment 4 is shown in Fig. 5.From test result it is found that different embodiment samples show excellent times
Rate performance.
Claims (9)
1. a kind of preparation method of ferrous selenide/carbon composite, which comprises the following steps:
(1) dopamine source is added to source of iron in the dissolution of dopamine source and the solvent insoluble to source of iron, is removed after mixing
Solvent is removed, powder A is obtained；
(2) powder A is pyrolyzed in 400~700 DEG C under vacuum, obtains powder B；
(3) powder B is mixed with selenium powder, is pyrolyzed at 600~900 DEG C, obtain ferrous selenide/carbon composite.
2. preparation method according to claim 1, which is characterized in that the dopamine source is selected from dopamine, DOPA amine salt
At least one of, it is preferable that the DOPA amine salt is Dopamine hydrochloride；The source of iron is iron acylate, preferably is selected from oxalic acid
At least one of iron, ferric acetate, ammonium ferric oxalate, ferric citrate.
3. preparation method according to claim 1 or 2, which is characterized in that in step (1), the matter in dopamine source and source of iron
Amount is than being 1:3~1:10.
4. preparation method according to any one of claim 1 to 3, which is characterized in that the solvent is selected from isopropanol, just
At least one of octanol, cyclohexanol.
5. preparation method according to any one of claim 1 to 4, which is characterized in that the uniformly mixed mode is
With stir 8 under the revolving speed of 100~800r/min~for 24 hours, preferably 18~for 24 hours.
6. preparation method according to any one of claim 1 to 5, which is characterized in that in step (2), vacuum degree be-
0.05~-0.1MPa rises to 400~700 DEG C with the heating rate of 5~15 DEG C/min, and soaking time is 0.01~2 hour.
7. preparation method according to any one of claim 1 to 6, which is characterized in that in step (3), powder B and selenium powder
Mass ratio be 1:2~1:5.
8. preparation method according to any one of claim 1 to 7, which is characterized in that in step (3), vacuum degree be-
0.05~-0.1MPa rises to 600~900 DEG C with the heating rate of 5~15 DEG C/min, and soaking time is 0.01~2 hour.
9. preparation method according to any one of claim 1 to 8, which is characterized in that in step (3), after heat preservation
Filling into inert gas keeps reaction system pressure consistent with air pressure.
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