CN102945965A - Preparing method of porous carbon embedding type lithium ion battery anode material - Google Patents
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- CN102945965A CN102945965A CN2012104926931A CN201210492693A CN102945965A CN 102945965 A CN102945965 A CN 102945965A CN 2012104926931 A CN2012104926931 A CN 2012104926931A CN 201210492693 A CN201210492693 A CN 201210492693A CN 102945965 A CN102945965 A CN 102945965A
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Abstract
An embodiment of the invention discloses a preparation method of a porous carbon embedding type lithium ion battery anode material. The preparation method includes preparing 0.05M of lithium salt, iron salt or manganese salt, phosphate, mixing sol liquid composed of chelating agent with set density and surfactant, adjusting pH of the sol liquid through nitric acid to be smaller than 2, adding conductive carbon with high superficial area into the sol liquid obtained under the stirring condition to obtain black mixture, evaporating and drying the black mixture to obtain black powder, keeping the black powder warm in a tubular furnace for 1-10h under the temperature larger than 300 DEG C, enabling the black powder to be cooled to the room temperature to obtain a black precursor, conducting ball milling on the black precursor, sintering un the tubular furnace under the temperature larger than 700 DEG C, keeping warm for 1-50h, and cooling to the room temperature with cooling of the furnace to obtain the anode material LiMPO4-C. The lithium ion battery anode material obtained by the method is wide in source, environment-friendly, stable in structure and excellent in electrochemical performance.
Description
Technical field
The present invention relates to technical field of lithium ion, relate in particular to a kind of preparation method of porous carbon embedded anode material for lithium-ion batteries.
Background technology
At present, lithium ion battery is because its good characteristic is novel battery with fastest developing speed, lithium ion battery has high-specific-power and high-energy-density, that the major technique that modern electronic product volume ever-smaller, the weight such as hand camera, computer, phone lighten day by day guarantees, in the large-sized battery application facet, lithium ion battery is to solve one of optimal electrical source of power of automobile exhaust pollution.Improve the lithium ion battery energy density in order to satisfy the market such as electric motor car to the demand of lithium ion battery, at first will research and develop new material, to promote energy content of battery density.
Positive electrode is one of critical material of lithium ion battery, three large raw materials at lithium ion battery: in positive and negative electrode and the electrolyte, one of Main Bottleneck of positive electrode present lithium ion battery development because all many-sided defectives such as its specific capacity, conductance become.The lithium ion anode material LiMPO of the olivine-type that attracts tremendous attention
4, such as LiFePO4 (LiFePO
4), lithium manganese phosphate (LiMnPO
4) etc., because it has abundant raw material, becomes to produce the characteristics such as cost is low, safe, environment is friendly, become lithium ion power battery cathode material Research Emphasis at home and abroad, yet the electrons/ions conductance that above-mentioned lithium ion anode material is relatively poor has seriously restricted olivine-type lithium ion anode material LiMPO
4Development.
In the last few years, people minimized in particle size in order to overcome these restrictions, mixed and improved between particle the aspect such as electron conduction and paid great effort.Wherein, also made up structure that multifrequency nature differs such as nucleocapsid structure, carbon-Material cladding system, micro-nano structure and loose structure etc.Loose structure is noticeable especially because a large amount of contact surface areas and three-dimensional conductive network are provided in these structures, yet in the loose structure, system's deficient in stability that hole is larger has also reduced the active material that loads, the less electrolyte osmosis that then affects because of surface tension in space.Therefore, novel LiMPO
4The research of compound porous structure has great significance for the problem that exists in the existing loose structure of solution and acts on.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of porous carbon embedded anode material for lithium-ion batteries, by anode material for lithium-ion batteries wide material sources, the environmental friendliness of the method preparation, Stability Analysis of Structures, chemical property is more superior.
The objective of the invention is to be achieved through the following technical solutions, a kind of preparation method of porous carbon embedded anode material for lithium-ion batteries, described preparation method comprises:
The lithium salts of preparation 0.05M, molysite or manganese salt, phosphate, and the mixed sols liquid that forms of the chelating agent of setting concentration and surfactant, and the pH that regulates this sol solutions with nitric acid extremely＜2;
Under stirring condition, in resulting sol solutions, add the conductive carbon of high surface, obtain black mixture;
Described black mixture is obtained black powder after pervaporation, the dry processing;
With described black powder in tube furnace in behind temperature insulation 1 ~ 10h of 300 ° of C, cool to room temperature with the furnace and obtain the black presoma;
Behind the abundant ball milling of described black presoma, in tube furnace in the temperature sintering of 700 ° of C and be incubated 1 ~ 50h after, cool to room temperature with the furnace and obtain positive electrode LiMPO
4-C.
Described lithium salts is lithium acetate or lithium nitrate; Described molysite is ferric oxalate or ferric nitrate; Described manganese salt is manganese acetate or manganese nitrate; Described phosphate is ammonium dihydrogen phosphate or phosphoric acid.
The setting concentration of described chelating agent is 0 ~ 0.3M.
The setting content of described surfactant is 0 ~ 50ml.
A kind of lithium ion battery, the positive electrode of described lithium ion battery are the porous carbon embedded anode material for lithium-ion batteries LiMPO according to the described method preparation of the claims 1-4
4-C.
As seen from the above technical solution provided by the invention, described preparation method comprises: the lithium salts of preparation 0.05M, molysite or manganese salt, phosphate, and the mixed sols liquid that forms of the chelating agent of setting concentration and surfactant, and the pH that regulates this sol solutions with nitric acid extremely＜2; Under stirring condition, in resulting sol solutions, add the conductive carbon of high surface, obtain black mixture; Described black mixture is obtained black powder after pervaporation, the dry processing; With described black powder in tube furnace in behind temperature insulation 1～10h of 300 ° of C, cool to room temperature with the furnace and obtain the black presoma; Behind the abundant ball milling of described black presoma, in tube furnace in the temperature sintering of 700 ° of C and be incubated 1 ~ 50h after, cool to room temperature with the furnace and obtain positive electrode LiMPO
4-C.By anode material for lithium-ion batteries wide material sources, the environmental friendliness of the method preparation, Stability Analysis of Structures, chemical property is more superior.
Description of drawings
In order to be illustrated more clearly in the technical scheme of the embodiment of the invention, the accompanying drawing of required use was done to introduce simply during the below will describe embodiment, apparently, accompanying drawing in the following describes only is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite of not paying creative work, can also obtain other accompanying drawings according to these accompanying drawings.
The porous carbon embedded method for preparing anode material of lithium-ion battery schematic flow sheet that Fig. 1 provides for the embodiment of the invention;
The resulting XRD schematic diagram of concrete experiment contrast during Fig. 2 is given an actual example by the embodiment of the invention;
Fig. 3 is the embodiment of the invention embedded LiMn that given an actual example
0.8Fe
0.2PO
4-C charging and discharging curve schematic diagram;
Fig. 4 is the embodiment of the invention common nucleocapsid LiMn that given an actual example
0.8Fe
0.2PO
4The charging and discharging curve schematic diagram;
Fig. 5 is the embodiment of the invention embedded LiMn that given an actual example
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4Multiplying power cycle performance schematic diagram;
Fig. 6 is the embodiment of the invention embedded LiMn that given an actual example
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4The AC impedance schematic diagram.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills belong to protection scope of the present invention not making the every other embodiment that obtains under the creative work prerequisite.
The advantages such as the high conductivity that the embodiment of the invention combines the high reaction activity of porous structure material and carbon composite and stability obtain that specific capacity is high, good rate capability, LiMPO that production cost is low
4-C positive electrode.Below in conjunction with accompanying drawing the embodiment of the invention is described in further detail, is illustrated in figure 1 as the porous carbon embedded method for preparing anode material of lithium-ion battery schematic flow sheet that the embodiment of the invention provides, described method comprises:
Step 11: at first prepare the lithium salts of 0.05M, molysite or manganese salt, phosphate, and the mixed sols liquid that forms of the chelating agent of setting concentration and surfactant, and the pH that regulates this sol solutions with nitric acid extremely＜2.
In specific implementation, can regulate sol solutions pH to 1 with nitric acid, above-mentioned chelating agent can be selected citric acid or tartaric acid etc., and surfactant can be selected ethylene glycol etc.In the specific implementation, the setting concentration of chelating agent can be 0 ~ 0.3M; It is 0 ~ 50ml that surfactant can be set content.
And above-mentioned lithium salts can be lithium acetate or lithium nitrate; Described molysite can be ferric oxalate or ferric nitrate; Described manganese salt can be manganese acetate or manganese nitrate; Described phosphate can be ammonium dihydrogen phosphate or phosphoric acid.For example, described lithium salts is lithium acetate (LiCH
3COO2H
2O), described molysite is ferrous oxalate (FeC
2O
42H
2O), manganese salt is manganese acetate (Mn (CH
3COO)
24H
2O), phosphate is ammonium dihydrogen phosphate (NH
4H
2PO
4).
Step 12: under stirring condition, in resulting sol solutions, add the conductive carbon of high surface, obtain black mixture.
Step 13: described black mixture is obtained black powder after pervaporation, the dry processing.
Step 14: with described black powder in tube furnace in behind temperature insulation 1 ~ 10h of 300 ° of C, cool to room temperature with the furnace and obtain the black presoma.
In specific implementation, can with black powder in tube furnace in 450 ° of C sintering and after being incubated 5h, cool to room temperature with the furnace and obtain the black presoma;
Step 15: behind the abundant ball milling of described black presoma, in tube furnace in the temperature sintering of 700 ° of C and be incubated 1 ~ 50h after, cool to room temperature with the furnace and obtain positive electrode LiMPO
4-C.
In specific implementation, can with the black presoma in tube furnace in 800 ° of C sintering and after being incubated 10h, cool to room temperature with the furnace and obtain needed positive electrode LiMPO
4-C.
The embodiment of the invention also provides a kind of lithium ion battery, and the positive electrode of described lithium ion battery is according to the prepared porous carbon embedded of above-mentioned preparation method embodiment anode material for lithium-ion batteries LiMPO
4-C.
Come above-mentioned preparation method is elaborated below in conjunction with instantiation:
(1) preparation consists of the lithium acetate of 0.05M, ferrous oxalate, and the citric acid agent of ammonium dihydrogen phosphate and 0.06M and the sol solutions of ethylene glycol are regulated deposit fluid pH to 1 with nitric acid.
(2) sol solutions of step (1) gained is added the conductive carbon acetylene black of high surface under the condition that stirs.
(3) with step (2) gained system through the evaporation, obtain black powder after the drying.
(4) with the black powder of step (3) in tube furnace in 450 ° of C sintering and cool to room temperature with the furnace after being incubated 5h and obtain the black presoma.
(5) behind the presoma ball milling with step (4) gained, in tube furnace in 800 ° of C sintering and cool to room temperature with the furnace after being incubated 15h and obtain target product LiMPO
4-C.
(1) preparation consists of the lithium acetate of 0.05M, manganese acetate, and the citric acid agent of ammonium dihydrogen phosphate and 0.06M and the sol solutions of ethylene glycol are regulated deposit fluid pH to 1 with nitric acid.
(2) sol solutions of step (1) gained is added the conductive carbon acetylene black of high surface under the condition that stirs.
(3) with step (2) gained system through the evaporation, obtain black powder after the drying.
(4) with the black powder of step (3) in tube furnace in 450 ° of C sintering and cool to room temperature with the furnace after being incubated 5h and obtain the black presoma.
(5) behind the presoma ball milling with step (4) gained, in tube furnace in 800 ° of C sintering and cool to room temperature with the furnace after being incubated 15h and obtain target product LiMPO
4-C.
Embodiment 3
(1) preparation consists of the lithium acetate of 0.05M, and manganese acetate and ferrous oxalate configure by a certain percentage, and the citric acid agent of ammonium dihydrogen phosphate and 0.06M and the sol solutions of ethylene glycol are regulated deposit fluid pH to 1 with nitric acid.
(2) sol solutions of step (1) gained is added the conductive carbon acetylene black of high surface under the condition that stirs.
(3) with step (2) gained system through the evaporation, obtain black powder after the drying.
(4) with the black powder of step (3) in tube furnace in 450 ° of C sintering and cool to room temperature with the furnace after being incubated 5h and obtain the black presoma.
(5) behind the presoma ball milling with step (4) gained, in tube furnace in 800 ° of C sintering and cool to room temperature with the furnace after being incubated 15h and obtain target product LiMPO
4-C.
(1) preparation consists of the lithium acetate of 0.05M, and manganese acetate and ferrous oxalate configure by a certain percentage, and the citric acid agent of ammonium dihydrogen phosphate and 0.06M and the sol solutions of ethylene glycol are regulated deposit fluid pH to 1 with nitric acid.
(2) sol solutions of step (1) gained is added other conductive additives such as the conductive carbon Ke Qin carbon of high surface or Graphene under the condition that stirs.
(3) with step (2) gained system through the evaporation, obtain black powder after the drying.
(4) with the black powder of step (3) in tube furnace in 450 ° of C sintering and cool to room temperature with the furnace after being incubated 5h and obtain the black presoma.
(5) behind the presoma ball milling with step (4) gained, in tube furnace in 800 ° of C sintering and cool to room temperature with the furnace after being incubated 15h and obtain target product LiMPO
4-C.
The sol solutions of other chelating agents such as (1) preparation consists of the lithium acetate of 0.05M, and manganese acetate and ferrous oxalate configure by a certain percentage, the tartaric acid of ammonium dihydrogen phosphate and 0.06M and ethylene glycol is regulated deposit fluid pH to 1 with nitric acid.
(2) sol solutions of step (1) gained is added the conductive carbon acetylene black of high surface under the condition that stirs.
(3) with step (2) gained system through the evaporation, obtain black powder after the drying.
(4) with the black powder of step (3) in tube furnace in 450 ° of C sintering and cool to room temperature with the furnace after being incubated 5h and obtain the black presoma.
(5) behind the presoma ball milling with step (4) gained, in tube furnace in 800 ° of C sintering and cool to room temperature with the furnace after being incubated 15h and obtain target product LiMPO
4-C.
(1) preparation consists of the lithium acetate of 0.05M, and manganese acetate and ferrous oxalate configure by a certain percentage, and the sol solutions of other surfactants such as the citric acid of ammonium dihydrogen phosphate and 0.06M and polyethylene glycol is regulated deposit fluid pH to 1 with nitric acid.
(2) sol solutions of step (1) gained is added the conductive carbon acetylene black of high surface under the condition that stirs.
(3) with step (2) gained system through the evaporation, obtain black powder after the drying.
(4) with the black powder of step (3) in tube furnace in 450 ° of C sintering and cool to room temperature with the furnace after being incubated 5h and obtain the black presoma.
(5) behind the presoma ball milling with step (4) gained, in tube furnace in 800 ° of C sintering and cool to room temperature with the furnace after being incubated 15h and obtain target product LiMPO
4-C.
The below is utilizing concrete experiment to come the above-mentioned prepared embedded LiMn of comparative analysis
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4Performance difference:
At first, with the embedded LiMn of above-mentioned gained
0.8Fe
0.2PO
4-C, common nucleocapsid LiMn
0.8Fe
0.2PO
4Carry out X-ray powder diffraction (XRD) with material with carbon element and analyze, be illustrated in figure 2 as the embodiment of the invention give an actual example in concrete experiment contrast resulting XRD schematic diagram, as shown in Figure 2:
Carry out the LiMn after carbon is inserted embedding
0.8Fe
0.2PO
4Do not change crystal structure, the material with carbon element of inserting simultaneously embedding is not destroyed carbon and LiMn behind high temperature
0.8Fe
0.2PO
4Be present in simultaneously in the product that obtains at last, illustrate that the present invention is applicable to the positive electrode LiMPO of whole olivine structurals
4.
Then, with the embedded LiMn of above-mentioned gained
0.8Fe
0.2PO
4-C carries out scanning electron microscope analysis and projection electronic microscope photos, wherein with common nucleocapsid LiMn
0.8Fe
0.2PO
4As a comparison, by contrast as can be known:
On the micron order yardstick, embedded LiMn
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4Have similar pattern, embedded LiMn has been described
0.8Fe
0.2PO
4-C does not change macrostructure and the form of material; And on the nanoscale yardstick, embedded LiMn
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4Have obvious difference, carbon granule is inner by uniform insert material, according to the method for the embodiment of the invention, can reach the effect of inserting the embedding material microstructure of adjusting according to the pattern of selecting material with carbon element, size, classification content etc.
Then, again with the embedded LiMn of above-mentioned gained
0.8Fe
0.2PO
4The lithium battery that-C is assembled carries out electrochemical property test, wherein with common nucleocapsid LiMn
0.8Fe
0.2PO
4As a comparison, probe temperature is room temperature, and battery voltage range is 2-4.8V(vs.Li
+/ Li).Be illustrated in figure 3 as the embodiment of the invention embedded LiMn that gives an actual example
0.8Fe
0.2PO
4-C charging and discharging curve schematic diagram; Be illustrated in figure 4 as the embodiment of the invention common nucleocapsid LiMn that gives an actual example
0.8Fe
0.2PO
4The charging and discharging curve schematic diagram; Be illustrated in figure 5 as the embodiment of the invention embedded LiMn that gives an actual example
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4Multiplying power cycle performance schematic diagram; Be illustrated in figure 6 as the embodiment of the invention embedded LiMn that gives an actual example
0.8Fe
0.2PO
4-C and common nucleocapsid LiMn
0.8Fe
0.2PO
4The AC impedance schematic diagram.
By Fig. 3 and 4 as can be known: embedded LiMn
0.8Fe
0.2PO
4-C has very high first discharge specific capacity (0.1C,〉160mAh g
-1), reactivity is obviously than common core-shell type LiMn
0.8Fe
0.2PO
4(0.1C, ~ 140mAh g
-1) height.
By Fig. 5 and 6 as can be known: embedded LiMn
0.8Fe
0.2PO
4-C has preferably high rate performance, when the multiplying power electric current increases to 0.2C, 0.5C, 1C, 2C, 5C gradually, has respectively 152,141,128,110 and 86mAh g
-1, and after the multiplying power circulation, under the 0.1C charging or discharging current, still can keep 158mAh g
-1, stability is obviously than common core-shell type LiMn
0.8Fe
0.2PO
4(remaining ~ 120mAh g
-1) good.
Above-mentioned embedded LiMn
0.8Fe
0.2PO
4-C has shown good high rate performance and cycle performance, mainly be because the introducing of embedded carbon has reduced the size of material, increase the degree of scatter of material and conductive agent, also improved wetting capacity and the material microstructure intensity of composite material to electrolyte simultaneously.
In sum, with traditional nucleocapsid structure LiMPO
4Compare the LiMPO of the prepared porous carbon embedded of embodiment of the invention structure
4-C composite material has internal layer and inserts embedding carbon and the formed intensive conductive network of outer carbon coated; have high electrical conductivity and electrolyte wettability; improved the reversible capacity of material; high rate performance also improves; this preparation method operates simple and easy cost cheapness simultaneously; easily large-scale production is for constructing high performance lithium ion battery anode composite material and the practical good basis of laying thereof.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claims.
Claims (5)
1. the preparation method of a porous carbon embedded anode material for lithium-ion batteries is characterized in that, described preparation method comprises:
The lithium salts of preparation 0.05M, molysite or manganese salt, phosphate, and the mixed sols liquid that forms of the chelating agent of setting concentration and surfactant, and the pH that regulates this sol solutions with nitric acid extremely＜2;
Under stirring condition, in resulting sol solutions, add the conductive carbon of high surface, obtain black mixture;
Described black mixture is obtained black powder after pervaporation, the dry processing;
With described black powder in tube furnace in behind temperature insulation 1 ~ 10h of 300 ° of C, cool to room temperature with the furnace and obtain the black presoma;
Behind the abundant ball milling of described black presoma, in tube furnace in the temperature sintering of 700 ° of C and be incubated 1 ~ 50h after, cool to room temperature with the furnace and obtain positive electrode LiMPO
4-C.
2. the preparation method of porous carbon embedded anode material for lithium-ion batteries as claimed in claim 1 is characterized in that,
Described lithium salts is lithium acetate or lithium nitrate; Described molysite is ferric oxalate or ferric nitrate; Described manganese salt is manganese acetate or manganese nitrate; Described phosphate is ammonium dihydrogen phosphate or phosphoric acid.
3. the preparation method of porous carbon embedded anode material for lithium-ion batteries as claimed in claim 1 is characterized in that,
The setting concentration of described chelating agent is 0 ~ 0.3M.
4. the preparation method of porous carbon embedded anode material for lithium-ion batteries as claimed in claim 1 is characterized in that,
The setting content of described surfactant is 0 ~ 50ml.
5. a lithium ion battery is characterized in that, the positive electrode of described lithium ion battery is the porous carbon embedded anode material for lithium-ion batteries LiMPO according to the described method preparation of the claims 1-4
4-C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103178261A (en) * | 2013-04-12 | 2013-06-26 | 长沙理工大学 | In-situ synthesis method of fast ion conductor embedded type lithium ion battery anode material |
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