CN109671937A - A kind of in-situ synthetic method of transiens metal oxide/graphene composite material - Google Patents
A kind of in-situ synthetic method of transiens metal oxide/graphene composite material Download PDFInfo
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- CN109671937A CN109671937A CN201811572258.3A CN201811572258A CN109671937A CN 109671937 A CN109671937 A CN 109671937A CN 201811572258 A CN201811572258 A CN 201811572258A CN 109671937 A CN109671937 A CN 109671937A
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
A kind of in-situ synthetic method of transiens metal oxide/graphene composite material of the invention, step are as follows: soluble ferric iron salt, transition metal salt and cerium salt are dissolved in deionized water, are mixed to get homogeneous solution；Precipitating reagent is added, until pH reaches 10 or more, stirring is complete to precipitating, it is still aging, after carrying out hydro-thermal reaction, neutrality is filtered and be washed to, hydroxide composite precipitating is obtained after drying；It weighs graphite and potassium permanganate is mixed and added into the concentrated sulfuric acid and phosphoric acid mix acid liquor, be persistently stirred to react rear ice-water bath, precipitating is added, and corresponding amount H is added2O2, continue stirring and ultrasonic wave dispersion；Product obtains transiens metal oxide/graphene composite material by washing, centrifugation, dry and sintering.The present invention is directly added into hydroxide precipitating during preparing graphite oxide, so that graphene oxide growth in situ on hydroxide matrix, reaches existing Volumetric expansion when alleviating metal oxide for negative electrode of lithium ion battery.
Description
Technical field:
The invention belongs to technical field of lithium ion battery negative, and in particular to a kind of transiens metal oxide/stone
The in-situ synthetic method of black alkene composite material.
Background technique:
Compared with traditional secondary cell, lithium ion battery because have energy density height, safety non-pollution, self discharge it is small,
The advantages that operating temperature is wide, have extended cycle life, memory-less effect, attracts extensive attention.Lithium ion battery is widely used in portable
The fields such as formula electronic equipment (such as mobile phone, digital camera, video camera, laptop) and electric tool, and gradually to
The fields such as electric bicycle, electric car, new energy energy storage are expanded.
Currently, graphite is the most common material of negative electrode of lithium ion battery, although it is with electronic conductivity height, cycle life
It is long, low in cost, the advantages such as have a safety feature, but the theoretical specific capacity of graphite only has 372mAh/g, it is difficult to meet high-performance, height
The demand of the lithium ion battery of capacity.The energy density and specific capacity of transition metal oxide negative electrode material are higher than graphite, and
It is from a wealth of sources, cheap, preparation is simple, there is superior chemical property, however its there is tight in charge and discharge process
The Volumetric expansion of weight, will lead to electrode material dusting, active specy falls off, and causes the capacity of electrode significantly to decay, surely
It is qualitative to be difficult to be protected.A large number of studies show that rationally being set if suitable conductive carbon material modifying metallic oxide can be selected
Structure and pattern are counted, can effectively enhance its electric conductivity, alleviate the Volumetric expansion of electrode material.Graphene is by single layer
The Colloidal particles of carbon atom composition, are sp2It is netted that the high-density raw sublayer that hydbridized carbon atoms are constituted arranges the honeycomb to be formed
Structure has excellent electrical conductivity, higher specific surface area (2600m2/ g), excellent thermal property and mechanical performance,
It is used widely in nanoelectronic, hydrogen storage, supercapacitor and sensor field.
It include using for metal simple-substance to be placed in graphene oxide water solution in existing graphene composite material preparation method,
Obtain the modes such as metal oxide/graphene complex after the black solid product generated after placement is freeze-dried, but with
When negative electrode of lithium ion battery the problem of generally existing volume expansion.
Summary of the invention:
The purpose of the present invention is overcoming above-mentioned the shortcomings of the prior art, a kind of transiens metal oxide/stone is provided
The in-situ synthetic method of black alkene composite material using the excellent electric conductivity of graphene and then alleviates gold by in-situ synthesis
Belong to oxide and be used for existing Volumetric expansion when negative electrode of lithium ion battery, prepares a kind of high capacity, high performance transition gold
Belong to oxide/graphene composite material.
To achieve the above object, the invention adopts the following technical scheme:
A kind of in-situ synthetic method of transiens metal oxide/graphene composite material, comprising the following steps:
(1) by soluble ferric iron salt, soluble transition metal salt, and soluble cerium salt 1:(0.01-0.5 in molar ratio):
(0.01-0.1), is dissolved in deionized water respectively, is uniformly mixed, and forms homogeneous solution；
(2) precipitating reagent is added dropwise into homogeneous solution, and is stirred continuously during dropwise addition, until pH value of solution reach 10 with
On, stop being added dropwise, continue after stirring 1-3h, stand at room temperature, after being aged 4h, hydro-thermal reaction is carried out, using filtering and water
It is washed till neutrality, transition metal hydroxide complex precipitate is obtained after drying, in which: the hydrothermal temperature is 120-
180 DEG C, time 3-10h；
(3) in mass ratio it is 1:(3-4), it weighs graphite and potassium permanganate is uniformly mixed, be added and the concentrated sulfuric acid and phosphoric acid are housed
In the three-necked flask of mix acid liquor, after being persistently stirred to react 12h, after obtaining celadon solution, then ice-water bath 1-5h, hydrogen-oxygen is added
Compound precipitating, later in the H for being slowly added to celadon liquor capacity 1/20-1/52O2, continue ultrasonic wavelength-division after stirring 30-40min
1-2h is dissipated, transiens metal hydroxides/graphene oxide suspension of mutually cladding growth is obtained.
(4) transiens metal hydroxides/graphene oxide suspension through drying, roasts after washing, being centrifuged,
Obtain transiens composite oxide of metal/graphene, wherein the calcination atmosphere is oxygen-free atmosphere, under maturing temperature is
300-500 DEG C, calcining time 3-6h.
In the step (1), soluble ferric iron salt is one of ferric nitrate, ferric sulfate or iron chloride, soluble ferric iron salt
It is used as matrix.
In the step (1), soluble transition metal salt is metallic cobalt, metallic zinc, manganese metal or Titanium it is solvable
Property nitrate, one of sulfate or chlorate, the described soluble transition metal salt addition is one or more.
In the step (1), soluble cerium salt is one of cerous nitrate or cerium chloride.
In the step (1), the mass ratio of deionized water and soluble ferric iron salt is (10-25): 1.
In the step (2), precipitating reagent is one of sodium hydroxide, ammonium hydroxide or urea element, drop rate 1-500
Drop/minute.
In the step (2), hydro-thermal reaction carries out in hydrothermal reaction kettle.
In the step (3), concentrated sulfuric acid concentration is 98%, and the proportion of the concentrated sulfuric acid and phosphoric acid is 1:1.
In the step (3), the mass percent of graphite and hydroxide precipitating is (0.01-20): 100.
In the step (3), H is added2O2Afterwards, solution rapidly goes to glassy yellow by celadon.
In the step (3), using Hummers method is improved, addition hydroxide is heavy during preparing graphene oxide
It forms sediment, obtains transiens metal hydroxides/graphene oxide suspension.
In the step (4), calcination atmosphere is nitrogen atmosphere or inert gas atmosphere.
In the step (4), drying process carries out in a vacuum drying oven, and drying temperature is 60 DEG C.
In the step (4), transiens composite oxide of metal/graphene composite material of preparation is used as lithium-ion electric
Pond cathode, through detecting, current density 100mA/g, after 100 circulations, specific capacity reaches 1210-1260mAh/g, coulomb effect
Rate reaches 99.5% or more.
Beneficial effects of the present invention:
(1) present invention is directly added into transition metal hydrogen-oxygen using in-situ synthesis during synthesizing graphene oxide
The compound of compound, simple process is easy to operate, and production cost is low；
(2) the transiens metal oxide/graphene composite material of the method for the present invention preparation has porous structure, specific surface
Product reaches 100-200m2/ g, CeO2Be conducive to the generation of nanometer rods, graphene uniform is dispersed between product grain gap, this
Structure can buffer Volumetric expansion of metal oxide during charge and discharge cycles, and improve electrode reaction dynamics
Performance.
Detailed description of the invention:
Fig. 1 is the XRD diagram of transiens metal oxide/graphene composite material prepared by the embodiment of the present invention 1；
Fig. 2 is the SEM figure of transiens metal oxide/graphene composite material prepared by the embodiment of the present invention 1；
Fig. 3 is that transiens metal oxide/graphene composite material prepared by the embodiment of the present invention 1 is used as lithium ion battery
The cyclic curve figure of cathode；
Fig. 4 is the SEM figure of transiens metal oxide/graphene composite material prepared by the embodiment of the present invention 4.
Specific embodiment:
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1
(1) ferric nitrate, cobalt nitrate and cerous nitrate are dissolved in deionized water with molar ratio 1:0.1:0.02 respectively, are mixed
Homogeneous solution is obtained after closing uniform stirring；(2) ammonium hydroxide is added in solution with 100 drops/minute, until pH reaches 10, continues to hold
Continuous stirring is put into precipitating at room temperature after still aging 4h, in hydrothermal reaction kettle completely, in 160 DEG C of hydro-thermal reaction 6h,
Neutrality is filtered and be washed to, obtains Fe after drying2O3-Co2O3-CeO2Complex hydroxide precipitating；(3) using improved
Hummers method prepares graphene oxide: weighing a certain amount of graphite and potassium permanganate is uniformly mixed, be added and 98% concentrated sulfuric acid is housed
In the three-necked flask of phosphoric acid mix acid liquor, it is persistently stirred to react 12h, after obtained celadon solution, hydrogen is added in ice-water bath 2h
Oxide precipitation (the mass percent ratio of graphite is 10%), is slowly added to the H of 10mL later2O2, solution is fast by celadon at this time
Speed becomes glassy yellow, continues ultrasonic wave after stirring 30min and disperses 1h, obtains the transiens metal hydroxide of mutually cladding growth
Object/graphene oxide suspension；(4) transiens metal hydroxides/graphene oxide suspension is by washing, centrifugation
Afterwards, filter cake is placed in 60 DEG C of vacuum oven and is sufficiently dried, lower 400 DEG C of nitrogen atmosphere roast 4 hours, obtain Fe2O3-
Co2O3-CeO2/ graphene negative electrode material, specific surface area reach 200m2/ g, XRD diagram is as shown in Figure 1, object is mutually mainly Fe2O3
Phase, SEM figure is as shown in Fig. 2, the negative electrode material is used as the cyclic curve figure of negative electrode of lithium ion battery as shown in figure 3, close in electric current
Degree is under 100mA/g after 100 circulations, and specific capacity is stablized in 1254mAh/g, coulombic efficiency 99.57%.
Embodiment 2
(1) iron chloride, manganese sulfate and cerium chloride are dissolved in deionized water with molar ratio 1:0.5:0.06 respectively, are mixed
Homogeneous solution is obtained after closing uniform stirring；(2) ammonium hydroxide is added in solution with 300 drops/minute, until pH reaches 10, continues to hold
Continuous stirring is put into precipitating in hydrothermal reaction kettle after still aging 4h at room temperature, in 180 DEG C of hydro-thermal reaction 4h, mistake completely
Neutrality is filtered and be washed to, obtains Fe after drying2O3-MnO2-CeO2Complex hydroxide precipitating；(3) improved Hummers is used
Method prepares graphite oxide: weighing a certain amount of graphite and potassium permanganate is uniformly mixed, be added mixed equipped with 98% concentrated sulfuric acid and phosphoric acid
In the three-necked flask for closing acid solution, it is persistently stirred to react 12h, it is heavy that hydroxide is added in ice-water bath 2h after obtained celadon solution
It forms sediment (the mass percent ratio of graphite is 5%), is slowly added to the H of 10mL later2O2, solution is rapidly gone to bright by celadon at this time
Yellow continues ultrasonic wave after stirring 30min and disperses 1h, obtains transiens metal hydroxides/oxidation stone of mutually cladding growth
The suspension of black alkene；(4) transiens metal hydroxides/graphene oxide suspension sets filter cake after washing, being centrifuged
Sufficiently dry in 60 DEG C of vacuum oven, lower 400 DEG C of nitrogen atmosphere roast 5 hours, obtain Fe2O3-MnO2-CeO2/ graphite
Alkene negative electrode material, specific surface area reach 150m2/ g, in the case where current density is 100mA/g after 100 circulations, specific capacity is stablized
In 1219mAh/g, coulombic efficiency 99.53%.
Embodiment 3
(1) ferric sulfate, titanium sulfate and cerium chloride are dissolved in deionized water with molar ratio 1:0.3:0.03 respectively, are mixed
Homogeneous solution is obtained after closing uniform stirring；(2) ammonium hydroxide is added in solution with 400 drops/minute, until pH reaches 10, continues to hold
Continuous stirring is put into precipitating in hydrothermal reaction kettle after still aging 4h at room temperature, in 140 DEG C of hydro-thermal reaction 5h, mistake completely
Neutrality is filtered and be washed to, obtains Fe after drying2O3-TiO2-CeO2Complex hydroxide precipitating；(3) improved Hummers is used
Method prepares graphite oxide: weighing a certain amount of graphite and potassium permanganate is uniformly mixed, be added mixed equipped with 98% concentrated sulfuric acid and phosphoric acid
In the three-necked flask for closing acid solution, it is persistently stirred to react 12h, it is heavy that hydroxide is added in ice-water bath 2h after obtained celadon solution
It forms sediment (the mass percent ratio of graphite is 20%), is slowly added to the H of 10mL later2O2, solution is rapidly gone to bright by celadon at this time
Yellow continues ultrasonic wave after stirring 30min and disperses 1h, obtains transiens metal hydroxides/oxidation stone of mutually cladding growth
The suspension of black alkene；(4) transiens metal hydroxides/graphene oxide suspension product will be filtered after washing, being centrifuged
Cake, which is placed in 60 DEG C of vacuum oven, sufficiently to be dried, and lower 500 DEG C of nitrogen atmosphere roast 6 hours, obtains Fe2O3-TiO2-CeO2/
Graphene negative electrode material, specific surface area reach 160m2/ g, in the case where current density is 100mA/g after 100 circulations, specific capacity
Stablize in 1232mAh/g, coulombic efficiency 99.55%.
Embodiment 4
(1) ferric sulfate, zinc chloride and cerous nitrate are dissolved in deionized water with molar ratio 1:0.5:0.1 respectively, are mixed
Homogeneous solution is obtained after uniform stirring；(2) ammonium hydroxide is added in solution with 500 drops/minute, until pH reaches 10, is continued for
Stirring is put into precipitating in hydrothermal reaction kettle after still aging 4h at room temperature completely, in 120 DEG C of hydro-thermal reaction 6h, filtering
And it is washed to neutrality, Fe is obtained after drying2O3-ZnO2-CeO2Complex hydroxide precipitating；(3) improved Hummers method is used
It prepares graphite oxide: weighing a certain amount of graphite and potassium permanganate is uniformly mixed, be added and mixed equipped with 98% concentrated sulfuric acid and phosphoric acid
In the three-necked flask of acid solution, it is persistently stirred to react 12h, hydroxide precipitating is added in ice-water bath 2h after obtained celadon solution
(the mass percent ratio of graphite is 15%), is slowly added to the H of 10mL later2O2, solution is rapidly gone to bright orange by celadon at this time
Color continues ultrasonic wave after stirring 30min and disperses 1h, obtains transiens metal hydroxides/graphite oxide of mutually cladding growth
The suspension of alkene；(4) transiens metal hydroxides/graphene oxide suspension product is after washing, being centrifuged, by filter cake
It is placed in 60 DEG C of vacuum oven and sufficiently dries, lower 400 DEG C of nitrogen atmosphere roast 3 hours, obtain Fe2O3-ZnO2-CeO2/ stone
Black alkene negative electrode material, SEM scheme as shown in figure 4, specific surface area reaches 180m2/ g passes through 100 in the case where current density is 100mA/g
After circulation, specific capacity is stablized in 1247mAh/g, coulombic efficiency 99.54%.
Claims (7)
1. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material, which is characterized in that including following step
It is rapid:
(1) by soluble ferric iron salt, soluble transition metal salt, and soluble cerium salt in molar ratio 1: (0.01-0.5):
(0.01-0.1), is dissolved in deionized water respectively, is uniformly mixed, and forms homogeneous solution；
(2) precipitating reagent is added dropwise into homogeneous solution, and is stirred continuously during dropwise addition, until pH value of solution reaches 10 or more, stops
It is only added dropwise, continues after stirring 1-3h, stand at room temperature, after being aged 4h, hydro-thermal reaction is carried out, in filtering and being washed to
Property, transition metal hydroxide complex precipitate is obtained after drying, in which: the hydrothermal temperature is 120-180 DEG C, when
Between be 3-10h；
(3) be in mass ratio 1: (3-4) weighs graphite and potassium permanganate is uniformly mixed, be added and mix equipped with the concentrated sulfuric acid and phosphoric acid
In the three-necked flask of acid solution, after being persistently stirred to react 12h, after obtaining celadon solution, then ice-water bath 1-5h, hydroxide is added
Precipitating, later in the H for being slowly added to celadon liquor capacity 1/20-1/52O2, continue ultrasonic wave after stirring 30-40min and disperse 1-
2h obtains transiens metal hydroxides/graphene oxide suspension of mutually cladding growth；
(4) transiens metal hydroxides/graphene oxide suspension, through drying, roasting, obtains after washing, being centrifuged
Transiens composite oxide of metal/graphene, wherein the calcination atmosphere is oxygen-free atmosphere, and maturing temperature is lower 300-500
DEG C, calcining time 3-6h.
2. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material according to claim 1,
It is characterized in that, in the step (1), soluble ferric iron salt is one of ferric nitrate, ferric sulfate or iron chloride, soluble ferric iron salt
It is used as matrix.
3. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material according to claim 1,
Be characterized in that, in the step (1), soluble transition metal salt is metallic cobalt, metallic zinc, manganese metal or Titanium it is solvable
Property nitrate, one of sulfate or chlorate, the described soluble transition metal salt addition is one or more.
4. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material according to claim 1,
It is characterized in that, in the step (1), soluble cerium salt is one of cerous nitrate or cerium chloride.
5. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material according to claim 1,
It is characterized in that, in the step (3), the mass percent of graphite and hydroxide precipitating is (0.01-20): 100.
6. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material according to claim 1,
It is characterized in that, in the step (4), calcination atmosphere is nitrogen atmosphere or inert gas atmosphere.
7. a kind of in-situ synthetic method of transiens metal oxide/graphene composite material according to claim 1,
It is characterized in that, in the step (4), transiens composite oxide of metal/graphene composite material of preparation is used as lithium ion
Battery cathode, through detecting, current density 100mA/g, after 100 circulations, specific capacity reaches 1210-1260mAh/g, coulomb
Efficiency reaches 99.5% or more.
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| CN115651696B (en) * | 2022-10-24 | 2023-07-18 | 滨州乾坤化工机械有限公司 | Desulfurizing agent for liquefied petroleum gas and preparation method thereof |
| CN116139690A (en) * | 2023-02-20 | 2023-05-23 | 无锡红旗除尘设备有限公司 | Iron-smelting blast furnace waste gas treatment system |
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