CN104638235A - Composite carbon nano tube array coated LiFePO4(lithium iron phosphate) electrode material and preparation method thereof - Google Patents
Composite carbon nano tube array coated LiFePO4(lithium iron phosphate) electrode material and preparation method thereof Download PDFInfo
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- CN104638235A CN104638235A CN201510022101.3A CN201510022101A CN104638235A CN 104638235 A CN104638235 A CN 104638235A CN 201510022101 A CN201510022101 A CN 201510022101A CN 104638235 A CN104638235 A CN 104638235A
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Abstract
The invention relates to a composite carbon nano tube arraycoatedLiFePO4(lithium iron phosphate) electrode material and a preparation method thereof. The material comprises nano LiFePO4 fully covered with a carbon layer, wherein the LiFePO4 fully covered with the carbon layer is partially covered with a carbon nano tube array. The preparation method comprises the following steps: firstly, preparing a precursorLiFePO4; secondly preparing the LiFePO4 fully covered with the carbon layer; and finally preparing composite carbon nano tube array coated LiFePO4. Therefore, the rate capacity and energy density of a phosphate material battery are improved.
Description
Technical field
The present invention relates to a kind of electrode material and preparation method thereof, particularly relate to a kind of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material and preparation method thereof.
Background technology
LiFePO
4have that cost is low, aboundresources and structural stability and thermal stability advantages of higher, but LiFePO under normal temperature
4dynamics bad, high rate performance extreme difference, significantly limit the application in practice of this material.Pure phosphoric acid ferrous lithium and traditional positive electrode LiCoO
2, LiNiO
2, LiMn
2o
4, LiMnO
2etc. comparing, have extremely low electronic conductivity and ion diffusion rates, charge/discharge capacity is very low at higher current densities, can only discharge and recharge under minimum current density, greatly limit application in practice.Therefore, the electron conduction improving LiFePO 4 becomes a research key of lithium iron phosphate cathode material.In order to improve conductivity and shorten the transmission path of ion, electronics, improve high rate performance, people have employed the methods such as such as coated, doping, nanometer and have carried out modification to it.
Prior art proposition is at the coated one deck conductive layer of material surface to improve electronic conductivity, and in polymer battery, 80 DEG C reach 160 mAh/g with reversible capacity under 1C multiplying power.Chiang Yet-Ming research group passes through aliovalent element (Mg, Al, Zr, Ti, Nb, W) to LiFePO
4in Li carry out the electronic conductivity substituting to improve material.Result shows that the material electric conductivity after adulterating can improve 8 orders of magnitude, when charge-discharge magnification is C/10, capacity can reach 150mAh/g, the capacity of 60 mAh/g is still kept when multiplying power is 40C, and almost do not decay through 60 weeks circulation volumes, show excellent chemical property.
Carbon nano-tube is a kind of New Type of Carbon structure found in the 90's of 20th century, and be a hollow tubular structure, tube wall is the tubular structure that one or more layers Graphene is curling.This structure of carbon nano-tube has excellent electronics, machinery, mechanics, optics, calorifics and energy-storage property, thus has potential extensive use in multiple field.
Summary of the invention
When the object of the invention is to overcome the positive electrode of existing LiFePO 4 material as serondary lithium battery, multiplying power property is poor, and make the low density shortcoming of pole piece, thus provide a kind of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material and preparation method thereof.
Object of the present invention is achieved through the following technical solutions:
Composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: the nanometer LiFePO including all standing carbon-coating
4, the nanometer LiFePO of described all standing carbon-coating
4outer surface part be coated with carbon nano pipe array.
Above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: the nanometer LiFePO of described all standing carbon-coating
4thickness is 1-10 nm, and described carbon nano pipe array degree is a 0.1-0.5 μm.
The preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, it comprises the following steps: first prepare presoma LiFePO
4; Afterwards, the nanometer LiFePO of all standing carbon-coating is prepared
4; Finally, composite carbon nano-array coated LiFePO 4 for lithium ion batteries is prepared.
The preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: described presoma LiFePO
4preparation process is, 1. step, takes Li
2cO
3, Fe
2o
3, NH
4h
2pO
4and C
6h
8o
7put in solvent, adopt the process of super grinder nanometer, pulverize after drying and obtain nano-mixture.2. mixture, is carry out low temperature presintering under the protection of reducing atmosphere of 5% in purity by step, after room temperature to 350 DEG C-380 DEG C, carry out constant temperature 2 to 4 hours.3., the mixture after step 2. being processed carries out high temperature sintering to step under protection of reducing atmosphere, after being warming up to 650 DEG C, keeps constant temperature 5 to 10 hours.4., mixture is Ar and the H of 5% in purity to step
2high temperature sintering under protection of reducing atmosphere: be warming up to 650 DEG C from 350 DEG C, at 650 DEG C of constant temperature 5-10 hour, continues to drop to room temperature under reducing atmosphere, then obtains the presoma LiFePO that mean particle size is 0.2-5.0 μm after being pulverized by solid
4.
Further, the preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: the described process that takes is take Li according to mol ratio 1: 1: 2: 0.6
2cO
3, Fe
2o
3, NH
4h
2pO
4and C
6h
8o
7, described solvent is deionized water, and described crushing process adopts ball mill to carry out.
Further, the preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: the nanometer LiFePO of described preparation all standing carbon-coating
4process be that 1. step, takes organic polymer and presoma LiFePO
4, be put in respectively in aluminium oxide magnetic boat A and aluminium oxide magnetic boat B.2. step, by aluminium oxide magnetic boat A and aluminium oxide magnetic boat B, in the boiler tube of the tube furnace be put into successively by vent gas order, starts to pass into inert protective gas.3. step, regulates inert protective gas flow to be 20 to 100sccm, from room temperature to 800 DEG C.4. step, keeps 800 DEG C of constant temperature after 2 to 4 hours, drops to room temperature, obtain the nanometer LiFePO of all standing carbon-coating
4.
Further, the preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: described organic polymer takes 0.1g, presoma LiFePO
4take 1.0g, described organic polymer is polyaniline or polyvinyl chloride.
Further, the preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: described inert protective gas is N
2.
Further; the preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: described preparation composite carbon nano-array coated LiFePO 4 for lithium ion batteries process is that step is 1.; pass into inert protective gas, the throughput regulating inert protective gas is 80sccm.Step 2., after room temperature to 680 DEG C, logical C
2h
2gas as carbon source, C
2h
2gas flow is 20 ~ 50sccm, regulates inert protective gas flow to be 60sccm.3. step, after 2 hours, drops to room temperature at 600 DEG C of constant temperature, obtains composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries material.
Again further, the preparation method of above-mentioned composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, wherein: described inert protective gas is Ar.
The advantage of technical solution of the present invention is mainly reflected in: by the nanometer LiFePO of all standing carbon-coating
4layer and formed again on this carbon-coating one part cover carbon nano pipe array, improve high rate performance and the energy density of phosphate material battery.Simultaneously, reduce the granularity of phosphate material by nanometer and improve the electrical contact performance between particle at its Surface coating carbon nano pipe array, increased considerably the specific area of material simultaneously, when improving the positive electrode of existing LiFePO 4 material as serondary lithium battery, multiplying power property is poor, and makes the low density shortcoming of pole piece.Thus, space has been expanded in the technological progress for this area, and implementation result is good.
Accompanying drawing explanation
Object of the present invention, advantage and disadvantage, by for illustration and explanation for the non-limitative illustration passing through preferred embodiment below.These embodiments are only the prominent examples of application technical solution of the present invention, allly take equivalent replacement or equivalent transformation and the technical scheme that formed, all drop within the scope of protection of present invention.
Fig. 1 is preparation flow schematic diagram of the present invention.
Embodiment
Composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, its special feature is: the nanometer LiFePO including all standing carbon-coating
4, the nanometer LiFePO of this all standing carbon-coating
4outer surface part be coated with carbon nano pipe array.Further, the nanometer LiFePO of all standing carbon-coating
4thickness is 1-10 nm, and carbon nano pipe array degree is a 0.1-0.5 μm.
As shown in Figure 1, in conjunction with the process of the preparation method of this composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, its unusual part is to comprise the following steps: first prepare presoma LiFePO
4.Afterwards, the nanometer LiFePO of all standing carbon-coating is prepared
4.Finally, composite carbon nano-array coated LiFePO 4 for lithium ion batteries is prepared.
Specifically, presoma LiFePO
4preparation process is: first, takes Li
2cO
3, Fe
2o
3, NH
4h
2pO
4and C
6h
8o
7put in solvent, adopt the process of super grinder nanometer, pulverize after drying and obtain nano-mixture.During this period, the process of taking is, takes Li according to mol ratio 1: 1: 2: 0.6
2cO
3, Fe
2o
3, NH
4h
2pO
4and C
6h
8o
7, described solvent is deionized water, and described crushing process adopts ball mill to carry out.Afterwards, be carry out low temperature presintering under the protection of reducing atmosphere of 5% in purity by mixture, after room temperature to 350 DEG C-380 DEG C, carried out constant temperature 2 to 4 hours with 0.5-1 hour.Then, under protection of reducing atmosphere, carry out high temperature sintering, after being warming up to 650 DEG C, keep constant temperature 5 to 10 hours.Finally, mixture is Ar and the H of 5% in purity
2high temperature sintering under protection of reducing atmosphere: be warming up to 650 DEG C from 350 DEG C with 1 to 2 hour; at 650 DEG C of constant temperature 5-10 hour; continue within 1 to 3 hour, to drop to room temperature under reducing atmosphere, then obtain the presoma LiFePO that mean particle size is 0.2-5.0 μm after being pulverized by solid
4.
Further, the nanometer LiFePO of the preparation all standing carbon-coating of the present invention's employing
4process be:
First, organic polymer and presoma LiFePO is taken
4, be put in respectively in aluminium oxide magnetic boat A and aluminium oxide magnetic boat B.Specifically, this organic polymer takes 0.1g, presoma LiFePO
4take 1.0g, and organic polymer is polyaniline or polyvinyl chloride.
Afterwards, by aluminium oxide magnetic boat A and aluminium oxide magnetic boat B, in the boiler tube of the tube furnace be put into successively by vent gas order, start to pass into inert protective gas.In order to have preferably protected effect, inert protective gas is N
2.Further, regulate inert protective gas flow to be 20 to 100sccm, service routine heats up, with 1 hour from room temperature to 800 DEG C.
Finally, keep 800 DEG C of constant temperature after 2 to 4 hours, dropped to room temperature with two hours, obtain the nanometer LiFePO of all standing carbon-coating
4.
Again further, the preparation composite carbon nano-array coated LiFePO 4 for lithium ion batteries process adopted is,
First, pass into inert protective gas, regulate the throughput of inert protective gas to be the residual air that 80sccm drives in quartz ampoule away, in order to improve the effect removing residual air, this inert protective gas is Ar.
Afterwards, service routine heats up with 1 hour after room temperature to 680 DEG C, leads to C
2h
2gas as carbon source, C
2h
2gas flow is 20 ~ 50sccm, regulates inert protective gas flow to be 60sccm.Finally, after 2 hours, drop to room temperature with two hours at 600 DEG C of constant temperature, obtain composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries material.
Thus, LiFePO in the product of acquisition
4primary particle average grain diameter is 300-5000nm, forms the network carbon-coating structure that the thick part of 1-10 nm covers on this carbon-coating again.Meanwhile, this network carbon-coating is continuously through or partial continuous is through, and it is 1 ~ 3wt% that the content of its carbon accounts for ferric lithium phosphate precursor percentage by weight, and the average diameter of carbon nano pipe array is 0.1 μm-0.5 μm.
In conjunction with the electrochemical measurement of material of the present invention, first charge to 4.2V with C/10, then identical multiplying power current discharge is to 2.4V, and the capacity of releasing is with LiFePO
4mass Calculation reach 171mAh/g.When discharging current is increased to 5C, the discharge capacity of this material is 90mAh/g, and this result shows that composite nanostructure carbon-coating coated LiFePO 4 for lithium ion batteries positive electrode has good high-multiplying-power discharge performance.
Can be found out by above-mentioned character express, after adopting the present invention, be by the nanometer LiFePO of all standing carbon-coating
4layer and formed again on this carbon-coating one part cover carbon nano pipe array, improve high rate performance and the energy density of phosphate material battery.Simultaneously, reduce the granularity of phosphate material by nanometer and improve the electrical contact performance between particle at its Surface coating carbon nano pipe array, increased considerably the specific area of material simultaneously, when improving the positive electrode of existing LiFePO 4 material as serondary lithium battery, multiplying power property is poor, and makes the low density shortcoming of pole piece.
Claims (10)
1. composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, is characterized in that: the nanometer LiFePO including all standing carbon-coating
4, the nanometer LiFePO of described all standing carbon-coating
4outer surface part be coated with carbon nano pipe array.
2. composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 1, is characterized in that: the nanometer LiFePO of described all standing carbon-coating
4thickness is 1-10 nm, and described carbon nano pipe array degree is a 0.1-0.5 μm.
3. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material, is characterized in that comprising the following steps: first prepare presoma LiFePO
4; Afterwards, the nanometer LiFePO of all standing carbon-coating is prepared
4; Finally, composite carbon nano-array coated LiFePO 4 for lithium ion batteries is prepared.
4. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 3, is characterized in that: described presoma LiFePO
4preparation process is,
1. step, takes Li
2cO
3, Fe
2o
3, NH
4h
2pO
4and C
6h
8o
7put in solvent, adopt the process of super grinder nanometer, pulverize after drying and obtain nano-mixture;
2. mixture, is carry out low temperature presintering under the protection of reducing atmosphere of 5% in purity by step, after room temperature to 350 DEG C-380 DEG C, carry out constant temperature 2 to 4 hours;
3., the mixture after step 2. being processed carries out high temperature sintering to step under protection of reducing atmosphere, after being warming up to 650 DEG C, keeps constant temperature 5 to 10 hours;
4., mixture is Ar and the H of 5% in purity to step
2high temperature sintering under protection of reducing atmosphere: be warming up to 650 DEG C from 350 DEG C, at 650 DEG C of constant temperature 5-10 hour, continues to drop to room temperature under reducing atmosphere, then obtains the presoma LiFePO that mean particle size is 0.2-5.0 μm after being pulverized by solid
4.
5. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 4, is characterized in that: the described process that takes is take Li according to mol ratio 1: 1: 2: 0.6
2cO
3, Fe
2o
3, NH
4h
2pO
4and C
6h
8o
7, described solvent is deionized water, and described crushing process adopts ball mill to carry out.
6. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 3, is characterized in that: the nanometer LiFePO of described preparation all standing carbon-coating
4process be,
1. step, takes organic polymer and presoma LiFePO
4, be put in aluminium oxide magnetic boat A and aluminium oxide magnetic boat B respectively,
2. step, by aluminium oxide magnetic boat A and aluminium oxide magnetic boat B, in the boiler tube of the tube furnace be put into successively by vent gas order, starts to pass into inert protective gas,
3. step, regulates inert protective gas flow to be 20 to 100sccm, from room temperature to 800 DEG C,
4. step, keeps 800 DEG C of constant temperature after 2 to 4 hours, drops to room temperature, obtain the nanometer LiFePO of all standing carbon-coating
4.
7. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 6, is characterized in that: described organic polymer takes 0.1g, presoma LiFePO
4take 1.0g, described organic polymer is polyaniline or polyvinyl chloride.
8. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 6, is characterized in that: described inert protective gas is N
2.
9. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 3, is characterized in that: described preparation composite carbon nano-array coated LiFePO 4 for lithium ion batteries process is,
1. step, passes into inert protective gas, and the throughput regulating inert protective gas is 80sccm;
Step 2., after room temperature to 680 DEG C, logical C
2h
2gas as carbon source, C
2h
2gas flow is 20 ~ 50sccm, regulates inert protective gas flow to be 60sccm;
3. step, after 2 hours, drops to room temperature at 600 DEG C of constant temperature, obtains composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries material.
10. the preparation method of composite carbon nanometer tube array coated LiFePO 4 for lithium ion batteries electrode material according to claim 9, is characterized in that: described inert protective gas is Ar.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111900374A (en) * | 2020-08-06 | 2020-11-06 | 福建东方醒狮新能源有限公司 | High energy density quick charging type lithium ion power battery |
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|---|---|---|---|---|
| CN1889290A (en) * | 2005-06-28 | 2007-01-03 | 中国科学院物理研究所 | Olivine carbon bobbles composite material and use thereof |
| CN102227024A (en) * | 2011-05-23 | 2011-10-26 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate anode material for power lithium ion battery and preparation method thereof |
| CN102610814A (en) * | 2012-02-23 | 2012-07-25 | 江苏元景锂粉工业有限公司 | Composite nano-structure carbon-layer-cladded lithium iron phosphate electrode material and preparation method thereof |
-
2015
- 2015-01-16 CN CN201510022101.3A patent/CN104638235A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1889290A (en) * | 2005-06-28 | 2007-01-03 | 中国科学院物理研究所 | Olivine carbon bobbles composite material and use thereof |
| CN102227024A (en) * | 2011-05-23 | 2011-10-26 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate anode material for power lithium ion battery and preparation method thereof |
| CN102610814A (en) * | 2012-02-23 | 2012-07-25 | 江苏元景锂粉工业有限公司 | Composite nano-structure carbon-layer-cladded lithium iron phosphate electrode material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111900374A (en) * | 2020-08-06 | 2020-11-06 | 福建东方醒狮新能源有限公司 | High energy density quick charging type lithium ion power battery |
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Application publication date: 20150520 |