CN107093715A - A kind of cuprous ion modified phosphate ferrous lithium electrode material and preparation method thereof - Google Patents
A kind of cuprous ion modified phosphate ferrous lithium electrode material and preparation method thereof Download PDFInfo
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- CN107093715A CN107093715A CN201710237490.0A CN201710237490A CN107093715A CN 107093715 A CN107093715 A CN 107093715A CN 201710237490 A CN201710237490 A CN 201710237490A CN 107093715 A CN107093715 A CN 107093715A
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Abstract
The invention discloses a kind of cuprous ion modified phosphate ferrous lithium electrode material and preparation method thereof.The electrode material is a kind of single-size of the sub-micron grade of the 4nm carbon-coatings of Surface coating 3, and chemical formula is Li [Fe0.9Cu0.1Li0.1]PO4Cu is positive monovalence in/C, formula.The doping of cuprous ion is carried out to LiFePO 4 using the method for carbon thermal reduction first, lithium source, source of iron, copper source and phosphorus source are stoichiometrically well mixed, wet ball grinding is simultaneously spray-dried.The calcining of two steps and natural cooling, that is, obtain the LiFePO 4 electrode material that described cuprous ion is modified in a nitrogen atmosphere.Contained organic acid can reduce ferric iron and bivalent cupric ion as reducing agent in first calcination process in raw material；Hydrogen phosphate is easily decomposed into gas at high temperature, effectively reduces the generation of impurity.The cuprous ion modified phosphate ferrous lithium electrode material that the present invention is provided improves lithium ion diffuser efficiency and charge/discharge capacity, guarantee is provided with the accumulation of energy of battery for electric automobile etc. is high-power while improved structure and crystal grain thinning.
Description
Technical field
The present invention relates to electrochemical energy field of material technology, more particularly to a kind of cuprous ion modified phosphate ferrous lithium electricity
Pole material and preparation method thereof.
Background technology
Since proposing ferrous phosphate lithium battery from Radhi in 1997 etc., thousands of related research conclusions are delivered, and are caused
The extensive concern of all trades and professions stakeholder.Compared to nickel, manganese, chromium, cobalt power plasma battery, ferrous phosphate lithium battery is with its cost
Lower, the life-span is longer, theoretical capacity (170mAh g-1) higher and pollution is smaller and has more obvious advantage.
But, the practical application of ferrous phosphate lithium battery still has difficulties, essentially consist in the diffusion of its lithium ion it is difficult and
Electronic conductivity it is low so that its at room temperature multiplying power it is not high.For these shortcomings, researchers propose that different methods are entered to it
Row study on the modification, mainly there is carbon coating, metal ion or oxide-doped, crystal grain thinning etc..So far, it is a variety of different
Carbon is used to do covering, such as acetylene black, CNT, graphene and glucose.Wherein glucose can be as stable
Agent carrys out crystal grain thinning, prevent from reuniting influences little to its pH simultaneously.
Because current theoretical research is still immature and lacks substantial progress, correlative study more sight invest in
LiFePO4/FePO4Reaction mechanism and phase in version.Lithium ion can only be of equal value by one-dimensional bending and anisotropic channel transfer
Or aliovalent substitution can cause the lattice defect of lithium ion position, have scholar to think that lattice defect can accelerate the transmission of lithium ion,
Some scholars think the inner exchanging in view of lithium ion and iron ion, and aliovalent substitution may improve the energy of lithium ion transport
Amount.Cuprous ion is doped into LiFePO 4 particle internal structure by the present invention first, is improved by triggering lattice defect
Its lithium ion transport speed.
The content of the invention
A kind of cuprous ion modified phosphate ferrous lithium electrode material that the present invention is provided is a kind of Surface coating 3-4nm carbon-coatings
Sub-micron grade single-size, chemical formula be Li [Fe0.9Cu0.1Li0.1]PO4Cu is positive monovalence in/C, formula.
Li[Fe0.9Cu0.1Li0.1]PO4/ C is positive electrode, and lithium ion battery is in charging process, the Li in its molecule+Enter
Enter electrolyte, Fe3+It is reduced to Fe2+, to keep the electroneutral of positive electrode.A small amount of cuprous ion is doped into ferrous phosphate
In lithium structure, lithium ion position can be made to occur lattice defect, so as to accelerate lithium ion diffuser efficiency, improve electrical conductivity and phase turns
Variable Rate.
To achieve the above object, a kind of the step of preparation method of cuprous ion modified phosphate ferrous lithium electrode material is such as
Under：
(1) lithium source, source of iron, copper source and phosphorus source are mixed by a certain percentage, adds a certain amount of glucose and surface-active
Agent.Using absolute ethyl alcohol as grinding aid, uniform ore pulp is made in ball milling 10h.What raw material and absolute ethyl alcohol were formed uniform mixes
Formation with respect to final product is particularly important.
Described lithium source is lithium acetate, lithium formate, the one or several kinds of lithium citrate；Described source of iron is ferric phosphate, three
Aoxidize two iron, the one or several kinds of iron hydroxide；Described copper source is copper acetate, the one or several kinds of copper citrate；Described
Phosphorus source is the one or several kinds of diammonium hydrogen phosphate or ammonium dihydrogen phosphate.
Described surfactant is cetyl trimethylammonium bromide (CTMAB).
Described glucose and CTMAB addition are respectively the 5-30% and 0.2-10% of product theory yield.
In described step (1), to keep electroneutral, lithium source, Tong Yuan, source of iron and phosphorus source are mixed by a certain percentage makes Li:
Cu:Fe:P is 1+x:x:1-x:1, wherein, x is the ratio between amount of material of copper ion and product LiFePO 4, and scope is 0.01-
0.5。
It is further preferred that the ratio between amount of material of described copper ion and product LiFePO 4 scope is 0.01-
0.1, effect of now adulterating is preferable.If the accounting of copper ion is excessive, the arrangement of LiFePO 4 particle inner ion is irregular, holds
It is also easy to produce impurity；If the accounting of copper ion is too small, adulterate DeGrain, it is impossible to triggers LiFePO 4 particle internal crystal framework
Defect.
Its circulation volume of the quality and thickness effect of carbon coating and inactive Fe3+The ratio of phase.Carbon-coating is excessively thin to cause electricity
Conductance is low, although blocked up can improve its electrical conductivity, can reduce its volume energy density and tap density, therefore surface covering carbon
The thickness of layer is very big to the performance impact of battery material.Equally, surfactant, which is dissolved in water, can significantly reduce the surface energy of water,
But only suitable addition metering could obtain the expected uniform submicron-scale of LiFePO 4 electrode material and distribution.
It is further preferred that described glucose and CTMAB contents is respectively the 10-15% and 1.5- of product theory yield
2.5%.Breakdown of glucose is that the thick carbon-coatings of 3-4nm are covered in its surface.
(2) gained ore pulp is spray-dried at 150 DEG C to 260 DEG C, is dried, even-grained powder；
Spray drying can make formed ore pulp fast dewatering and dry, and obtain the uniform powder of composition.In spray drying
During, CTMAB plays surfactant, can effectively suppress particle agglomeration.
(3) by above-mentioned well mixed powder pressing forming, secondary clacining, naturally cools to room temperature in a nitrogen atmosphere,
Products therefrom is the lithium iron phosphate cathode material that cuprous ion is modified.
Preferably, secondary clacining process is 300 DEG C of insulation 2h, 650 DEG C of insulation 4h are warming up to.Calcined for the first time at 300 DEG C
During, organic acid and hydrophosphate are decomposed into gas, can effectively reduce the generation of impurity.Meanwhile, it is contained in raw material to have
Machine acid group can reduce ferric iron and bivalent cupric ion as reducing agent in first calcination process.
A kind of cuprous ion modified phosphate ferrous lithium electrode material proposed by the present invention and preparation method thereof, first using carbon
The method of thermal reduction carries out the doping of cuprous ion to LiFePO 4, and method is improving its structure and refining the same of its crystal grain
When, lithium ion diffuser efficiency and charge/discharge capacity are improved, guarantee is provided with the accumulation of energy of battery for electric automobile etc. is high-power.
Preferably, a kind of the step of preparation method of cuprous ion modified phosphate ferrous lithium electrode material is as follows：
(1) mixing lithium acetate, copper acetate, ferric phosphate and ammonium dihydrogen phosphate by a certain percentage makes Li:Cu:Fe:P is 1+x:
x:1-x:1, it is separately added into electrode material theoretical yield 10-15% glucose and 1.5-2.5% CTMAB.With absolute ethyl alcohol
As grinding aid, uniform ore pulp is made in ball milling 10h, and x is the ratio between amount of material of copper ion and product LiFePO 4, model
Enclose for 0.01-0.1..
(2) gained ore pulp is spray-dried at 150 DEG C to 260 DEG C, is dried, even-grained powder；
(3) by above-mentioned well mixed powder pressing forming, secondary clacining, naturally cools to room temperature in a nitrogen atmosphere,
Products therefrom is the lithium iron phosphate cathode material of cuprous ion doping.
Secondary clacining is 300 DEG C of insulation 2h, is warming up to 650 DEG C of insulation 4h.At 300 DEG C in first calcination process, organic acid
Root and hydrophosphate be decomposed at gas, 650 DEG C second calcination process reaction example just like：
90FePO4+110LiCH3COO+10Cu(CH3COO)2+10NH4H2PO4→100Li1.1Cu0.1Fe0.9PO4
Use the preparation method can obtained cuprous ion ferrous phosphate doping lithium anode material carbon layer on surface thickness for
3-4nm, particle diameter distribution is 50-500nm, and the lithium ion transport speed order of magnitude is 10-14With 10-12Between, specific discharge capacity is
140-170mAh/g。
Embodiment
The present invention is further elaborated and illustrated with reference to specific embodiment.The number of component in following each embodiments
It is molar part.
Embodiment 1
The present embodiment is prepared for the cuprous ion modified phosphate ferrous lithium electrode material and its preparation that a kind of carbon-coating is 3.2nm
Method, specific preparation method is comprised the following steps：
(1) 101 parts of lithium acetate, 1 part of copper acetate, 99 parts of ferric phosphate, 1 part of ammonium dihydrogen phosphate, and 10 parts of anhydrous second are weighed
Alcohol, 10 parts of glucose, and 1.5 parts of CTMAB, are placed in ball mill, ball milling 10 hours；
(2) gained ore pulp is spray-dried at 150 DEG C, is dried, even-grained powder；
(3) by above-mentioned well mixed powder pressing forming, 300 DEG C of insulation 2h, are warming up to 650 DEG C of guarantors in a nitrogen atmosphere
Warm 4h, naturally cools to room temperature, and products therefrom is the ferrous lithium phosphate cathode material that the cuprous ion that carbon-coating is 3.2nm adulterates
Material.
Electrochemical property test, its lithium are carried out to cuprous ion ferrous phosphate doping lithium anode material prepared by embodiment 1
The ion diffuser efficiency order of magnitude is 10-14, specific discharge capacity is 141mAh/g, is declined slightly after circulating 50 times.
Embodiment 2
The present embodiment is prepared for the cuprous ion modified phosphate ferrous lithium electrode material and its preparation that a kind of carbon-coating is 3.3nm
Method, specific preparation method is comprised the following steps：
(1) 104 parts of lithium acetate, 4 parts of copper acetate, 96 parts of ferric phosphate, 4 parts of ammonium dihydrogen phosphate, and 10 parts of anhydrous second are weighed
Alcohol, 12 parts of glucose, and 1.5 parts of CTMAB, are placed in ball mill, ball milling 10 hours；
(2) gained ore pulp is spray-dried at 200 DEG C, is dried, even-grained powder；
(3) by above-mentioned well mixed powder pressing forming, 300 DEG C of insulation 2h, are warming up to 650 DEG C of guarantors in a nitrogen atmosphere
Warm 4h, naturally cools to room temperature, and products therefrom is the ferrous lithium phosphate cathode material that the cuprous ion that carbon-coating is 3.3nm adulterates
Material.
Electrochemical property test, its lithium are carried out to cuprous ion ferrous phosphate doping lithium anode material prepared by embodiment 2
The ion diffuser efficiency order of magnitude is 10-14, specific discharge capacity is 155mAh/g, and about 2mAh/g is risen after circulating 50 times.
Embodiment 3
The present embodiment is prepared for the cuprous ion modified phosphate ferrous lithium electrode material and its preparation that a kind of carbon-coating is 3.4nm
Method, specific preparation method is comprised the following steps：
(1) 106 parts of lithium acetate, 6 parts of copper acetate, 94 parts of ferric phosphate, 6 parts of ammonium dihydrogen phosphate, and 10 parts of anhydrous second are weighed
Alcohol, 13 parts of glucose, and 1.8 parts of CTMAB, are placed in ball mill, ball milling 10 hours；
(2) gained ore pulp is spray-dried at 260 DEG C, is dried, even-grained powder；
(3) by above-mentioned well mixed powder pressing forming, 300 DEG C of insulation 2h, are warming up to 650 DEG C of guarantors in a nitrogen atmosphere
Warm 4h, naturally cools to room temperature, and products therefrom is that carbon-coating is the lithium iron phosphate cathode material that 3.4nm cuprous ions adulterate.
Electrochemical property test, its lithium are carried out to cuprous ion ferrous phosphate doping lithium anode material prepared by embodiment 3
The ion diffuser efficiency order of magnitude is 10-12, specific discharge capacity is 160mAh/g, and about 1mAh/g is risen after circulating 50 times.
Embodiment 4
The present embodiment is prepared for the cuprous ion modified phosphate ferrous lithium electrode material and its preparation that a kind of carbon-coating is 3.8nm
Method, specific preparation method is comprised the following steps：
(1) 108 parts of lithium acetate, 8 parts of copper acetate, 92 parts of ferric phosphate, 8 parts of ammonium dihydrogen phosphate, and 10 parts of anhydrous second are weighed
Alcohol, 15 parts of glucose, and 2.5 parts of CTMAB, are placed in ball mill, ball milling 10 hours；
(2) gained ore pulp is spray-dried at 180 DEG C, is dried, even-grained powder.
(3) by above-mentioned well mixed powder pressing forming, 300 DEG C of insulation 2h, are warming up to 650 DEG C of guarantors in a nitrogen atmosphere
Warm 4h, naturally cools to room temperature, and products therefrom is the ferrous lithium phosphate cathode material that the cuprous ion that carbon-coating is 3.8nm adulterates
Material.
Electrochemical property test, its lithium are carried out to cuprous ion ferrous phosphate doping lithium anode material prepared by embodiment 4
The ion diffuser efficiency order of magnitude is 10-12, specific discharge capacity is 166mAh/g, and about 2mAh/g is risen after circulating 50 times.
Embodiment 5
The present embodiment is prepared for the cuprous ion modified phosphate ferrous lithium electrode material and its preparation that a kind of carbon-coating is 3.5nm
Method, specific preparation method is comprised the following steps：
(1) 110 parts of lithium acetate is weighed, 10 parts of copper acetate, 90 parts of ferric phosphate, 10 parts of ammonium dihydrogen phosphate, and 10 parts anhydrous
Ethanol, 14 parts of glucose, and 2.5 parts of CTMAB, are placed in ball mill, ball milling 10 hours；
(2) gained ore pulp is spray-dried at 220 DEG C, is dried, even-grained powder.
(3) by above-mentioned well mixed powder pressing forming, 300 DEG C of insulation 2h, are warming up to 650 DEG C of guarantors in a nitrogen atmosphere
Warm 4h, naturally cools to room temperature, and products therefrom is the ferrous lithium phosphate cathode material that the cuprous ion that carbon-coating is 3.5nm adulterates
Material.
Electrochemical property test, its lithium are carried out to cuprous ion ferrous phosphate doping lithium anode material prepared by embodiment 4
The ion diffuser efficiency order of magnitude is 10-14, specific discharge capacity is 159mAh/g, and about 1mAh/g is risen after circulating 50 times.
Claims (7)
1. a kind of cuprous ion modified phosphate ferrous lithium electrode material, it is characterised in that it is a kind of Surface coating 3-4nm carbon-coatings
Sub-micron grade single-size, chemical formula be Li [Fe0.9Cu0.1Li0.1]PO4Cu is positive monovalence in/C, formula.
2. a kind of preparation method of cuprous ion modified phosphate ferrous lithium electrode material as claimed in claim 1, its feature
Be, it the step of it is as follows：
(1) lithium source, source of iron, copper source and phosphorus source are mixed by a certain percentage, adds a certain amount of glucose and surfactant, with
Uniform ore pulp is made as grinding aid, ball milling 10h in absolute ethyl alcohol；
(2) gained ore pulp is spray-dried at 150 DEG C to 260 DEG C, is dried, even-grained powder；
(3) by above-mentioned well mixed powder pressing forming, secondary clacining, naturally cools to room temperature, gained in a nitrogen atmosphere
Product is the lithium iron phosphate cathode material of cuprous ion doping.
3. the preparation method of cuprous ion modified phosphate ferrous lithium electrode material according to claim 2, its feature exists
In described lithium source is lithium acetate, lithium formate, the one or several kinds of lithium citrate；Described source of iron is ferric phosphate, three oxidations two
Iron, the one or several kinds of iron hydroxide；Described copper source is copper acetate, the one or several kinds of copper citrate；Described phosphorus source is
One or both of diammonium hydrogen phosphate and ammonium dihydrogen phosphate.
4. the preparation method of cuprous ion modified phosphate ferrous lithium electrode material according to claim 2, its feature exists
In described surfactant is cetyl trimethylammonium bromide.
5. the preparation method of cuprous ion modified phosphate ferrous lithium electrode material according to claim 4, its feature exists
In, described glucose and the addition of cetyl trimethylammonium bromide be respectively the 5-30% and 0.2- of product theory yield
10%.
6. the preparation method of cuprous ion modified phosphate ferrous lithium electrode material according to claim 2, its feature exists
In in described step (1), to keep electroneutral, lithium source, Tong Yuan, source of iron and phosphorus source are mixed by a certain percentage makes Li:Cu:Fe:
P is 1+x:x:1-x:1, wherein, x is the ratio between amount of material of copper ion and product LiFePO 4, and scope is 0.01-0.5.
7. the preparation method of cuprous ion modified phosphate ferrous lithium electrode material according to claim 2, its feature exists
In secondary clacining process is 300 DEG C of insulation 2h, is warming up to 650 DEG C of insulation 4h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746742A (en) * | 2008-12-11 | 2010-06-23 | 中国电子科技集团公司第十八研究所 | Method for preparing lithium ion battery anode material spherical LiFePO4 |
| CN103165886A (en) * | 2012-11-23 | 2013-06-19 | 杭州金马能源科技有限公司 | Preparation method for lithium iron phosphate materials with high tap density |
-
2017
- 2017-04-12 CN CN201710237490.0A patent/CN107093715A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746742A (en) * | 2008-12-11 | 2010-06-23 | 中国电子科技集团公司第十八研究所 | Method for preparing lithium ion battery anode material spherical LiFePO4 |
| CN103165886A (en) * | 2012-11-23 | 2013-06-19 | 杭州金马能源科技有限公司 | Preparation method for lithium iron phosphate materials with high tap density |
Non-Patent Citations (1)
| Title |
|---|
| JIAN-MIN ZHU等: ""A novel Cu+-doped Li[Fe0.9Cu0.1Li0.1]PO4/C cathode material with enhanced electrochemical roperties"", 《RSC ADVANCES》 * |
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Application publication date: 20170825 |