CN109192955A - A kind of preparation method of LiFePO4/graphene in-situ composite - Google Patents
A kind of preparation method of LiFePO4/graphene in-situ composite Download PDFInfo
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- CN109192955A CN109192955A CN201811050593.7A CN201811050593A CN109192955A CN 109192955 A CN109192955 A CN 109192955A CN 201811050593 A CN201811050593 A CN 201811050593A CN 109192955 A CN109192955 A CN 109192955A
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Abstract
This field is related to technical field of function materials, the preparation method of especially a kind of LiFePO4/graphene in-situ composite.The graphene that the present invention prepares full liquid water phase physics stripping method carries out the method that weak oxide is modified, then combines by rheology phase-carbon thermal reduction, keeps LiFePO4 and graphene growth in situ formula compound, forms LiFePO4/graphene in-situ composite.LiFePO4 prepared by the present invention/graphene in-situ composite charge/discharge capacity height, good cycle, electric conductivity be good, electrochemical performance, and required processing step is simple, low raw-material cost, is suitable for industrialized production.
Description
Technical field
This field is related to technical field of function materials, the system of especially a kind of LiFePO4/graphene in-situ composite
Preparation Method.
Background technique
LiFePO4 is a kind of positive electrode of lithium battery, has the characteristics that at low cost, safety and service life are long.However, phosphorus
The electric conductivity of sour iron lithium material is poor, specific discharge capacity is low, is not able to satisfy the positive electrode of high-capacity lithium-ion power battery
Needs.
Graphene is a kind of novel two-dimension nano materials, has good electric conductivity.By grapheme material with it is existing
Positive electrode progress is compound, can effectively improve the chemical property of material.Currently, LiFePO 4 material and grapheme material
Complex method mainly passes through simple dry powder ball milling or wet ball grinding.These modes are difficult to LiFePO 4 material and stone
Black alkene material is uniformly dispersed, and causes existing grapheme material to promote the chemical property of LiFePO 4 material limited.
Summary of the invention
The deficiencies in the prior art are directed to, the present invention provides a kind of LiFePO4/graphene in-situ composite systems
Preparation Method.LiFePO4 prepared by the present invention/graphene in-situ composite has charge/discharge capacity height, good cycle, leads
The characteristics of electrical property is good, electrochemical performance.
The invention adopts the following technical scheme:
A kind of preparation method of LiFePO4/graphene in-situ composite, comprising the following steps:
(1) by FeSO4、H3PO4, LiOH be added in distilled water, citric acid is then added, be uniformly mixed, mixed
Liquid；FeSO4、H3PO4, LiOH molar ratio be 1:1:3；The quality of citric acid is LiFePO4Theoretical generate the 45% of quality；
Distilled water and the mass ratio for the substance total amount being added are 30-50:1；
(2) graphene is carried out weak oxide to be modified, obtains modified graphene；
(3) by modified graphene, ultrasonic disperse is uniform in deionized water, and ultrasonic time 3-5h obtains graphene dispersion
Liquid；The mass fraction of modified graphene is 5-10% in graphene dispersing solution；
(4) graphene dispersing solution is added in the mixed liquor that step (1) obtains, stirs 3- at 90-100 DEG C of temperature
4h obtains fluid；
(5) dry fluid, then fluid is ground, obtain presoma；
(6) presoma is pre-sintered, is then formally sintered, obtain LiFePO4/graphene In-situ reaction material
Material.
Preferably, the graphene is prepared by full liquid physics stripping method, and the number of plies of graphene is 3-6.
Preferably, the weak oxide it is modified the following steps are included:
(a) graphene, potassium permanganate are sequentially added in the concentrated sulfuric acid, react 4-5h at 90-100 DEG C of temperature；The concentrated sulfuric acid, stone
The mass ratio that black alkene, potassium permanganate are added is 3:5:1；
(b) it collects graphene and is washed to pH value to be neutral to get to modified graphene.
Preferably, the drying is vacuum drying, and temperature is 100-120 DEG C, time 10-15h.
Preferably, the pre-sintering carries out in hydrogen reducing atmosphere, and the temperature of pre-sintering is 400-500 DEG C, and the time is
3-5h。
Preferably, the temperature being formally sintered is 700-800 DEG C, time 10-12h.
A kind of LiFePO4/graphene in-situ composite that above-mentioned method is prepared.
Graphene of the invention is prepared by full liquid physics stripping method.
More specifically, the method that full liquid water phase physics removing prepares graphene, comprising the following steps:
(1) using ultrapure water to impregnate carbon content is 99.99%, and dilation is 200 times of expanded graphite, carries out wetting immersion
Processing, for 8-15mL:1g, the time for soaking immersion treatment is 18- for the volume of the ultrapure water used and the mass ratio of expanded graphite
25h；
(2) expanded graphite after wetting immersion treatment in step (1) is put into sand mill stirring, placed at colloid mill
Reason, obtains expanded graphite soak, wherein the concrete operations of milled processed are as follows: puts the expanded graphite after wetting immersion treatment
Entering stir process 1.5-4h in the sand mill equipped with a small amount of zirconium pearl, the revolving speed of sand mill is set as 1000-2000rad/min, then
It is put into milling treatment of colloid 3-6h, the power of colloid mill is 1-2kW, treating capacity 18-25L/h；
(3) the expanded graphite soak in step (2) is put into high pressure homogenizer and carries out high-pressure homogeneous processing, then with height
The processing of emulsification pretreatment pump, then handled with super-pressure critical assembly, obtain graphene dispersing solution, wherein the item of high-pressure homogeneous processing
Part are as follows: time 1.5-3h, pressure 50-100MPa, the time of emulsification treatment are 2.5-5h, the condition of the critical processing of super-pressure
Are as follows: time 2.5-5h, pressure 120-180MPa；
(4) step (3) are handled to obtained graphene dispersing solution stratification, are done by spraying at being 180-250 DEG C in temperature
It is dry to get arrive graphene.
The graphene lattice structure being prepared using full liquid physics stripping method is complete, simultaneously containing a small amount of-OH etc.
Hydrophilic radical, specific surface area 679m2/ g, graphene carbon content are 99.99wt%, and metal ion content≤100ppm is led
Hot coefficient is 3800W/ (mK).
Graphene of the invention is removed by full liquid physics and is prepared, and since its surface functional group is less, is not easily dispersed in
In water, therefore weak oxide being carried out to it and is modified, modified graphene has good dispersion performance, can be uniform by ultrasound
It is scattered in deionized water.Sulfuric acid used in this process and potassium permanganate, dosage is few, and processing can be recycled, and not will cause environment dirt
Dye.Graphene sheet layer structural integrity prepared by the present invention, the number of plies facilitate the growth in situ of LiFePO4 between 3-6 layers.
The mass ratio of graphene and LiFePO4 is 1:15-20 in the present invention.
The present invention prepares LiFePO4, the LiFePO4 crystallinity height of synthesis, uniform particle sizes, and technique letter by hydro-thermal method
Single, low energy consumption, the period is short；By FeSO4、H3PO4, LiOH in molar ratio 1:1:3 be added in distilled water, add a certain amount of
Citric acid provides carbon source, after mixing, graphene mixed liquor is added, LiFePO4 can be made to be attached directly in nucleation process
Graphene film layer surface.The method combined by rheology phase-carbon thermal reduction keeps LiFePO4 and graphene growth in situ formula multiple
It closes, forms LiFePO4/graphene in-situ composite.Average grain diameter is that the lithium iron phosphate nano particle of 50nm-150nm is uniform
It is distributed in graphene film layer surface or is inserted into the interlayer of graphene, overcome dry powder ball milling or wet ball grinding method is difficult to phosphoric acid
The shortcomings that iron lithium material and grapheme material are uniformly dispersed.
Beneficial effects of the present invention:
(1) LiFePO4 prepared by the present invention/graphene in-situ composite has good charging and discharging capacity, is filling
Under conditions of discharge-rate is 20C, electric discharge gram volume is 115mAh/g；Under conditions of 10C, the capacity that circulation is 1500 times is kept
Rate still 95%, has excellent cycle performance；Compared with traditional lithium iron phosphate positive material, LiFePO4/graphene is in situ
The gram volume of composite material improves 20%, sufficiently solves the problems, such as that traditional lithium iron phosphate positive material charging capacity is low；
(2) LiFePO4 in the present invention and graphene are compound by growth in situ formula, since graphene is with good
Electric conductivity can fundamentally promote the electric conductivity of LiFePO4 itself, obtained LiFePO4/graphene In-situ reaction
The conductivity of material is up to 1.41 × 10-3S/cm；
(3) preparation method through the invention, lithium iron phosphate nano particle are evenly distributed on graphene film layer surface or insert
The interlayer for entering graphene forms numerous compound interfaces, so that lithium ion is easier to be enriched with, it is higher to become electro-chemical activity
Site substantially improves the chemical property of composite material；
(4) preparation process of the invention is simple, the low raw-material cost of use, is suitable for industrialized production.
Detailed description of the invention
Fig. 1 is LiFePO4/graphene in-situ composite electron microscope.
Specific embodiment
Below by embodiment, the present invention will be described in detail.
Embodiment 1
(1) by 0.5molFeSO4、0.5molH3PO4, 1.5molLiOH be added in 8L distilled water, 35.6g is then added
Citric acid is uniformly mixed, obtains mixed liquor；
(2) graphene is prepared by full liquid physics stripping method, 5g graphene, 1g is then sequentially added in the 3g concentrated sulfuric acid
Potassium permanganate, reacts 4h at 90 DEG C of temperature, collects graphene and is washed to pH value to be neutral to get to modified graphite
Alkene；
(3) by 5g modified graphene, ultrasonic disperse is uniform in 95mL deionized water, and ultrasonic time 3h obtains graphene
Dispersion liquid；
(4) graphene dispersing solution is added in the mixed liquor that step (1) obtains, stirs 3h at 90 DEG C of temperature, obtains
Fluid；
(5) it is dried in vacuo fluid 10h at 100 DEG C, then fluid is ground, obtains presoma；
(6) presoma is pre-sintered 3h in hydrogen reducing atmosphere progress at 400 DEG C；Then it is carried out just at 700 DEG C
Formula is sintered 10h, obtains LiFePO4/graphene in-situ composite.
Embodiment 2
(1) by 1molFeSO4、1molH3PO4, 3molLiOH be added in 21L distilled water, then be added 71.1g lemon
Acid is uniformly mixed, obtains mixed liquor；
(2) graphene is prepared by full liquid physics stripping method, 5g graphene, 1g is then sequentially added in the 3g concentrated sulfuric acid
Potassium permanganate, reacts 5h at 90 DEG C of temperature, collects graphene and is washed to pH value to be neutral to get to modified graphite
Alkene；
(3) by 8g modified graphene, ultrasonic disperse is uniform in 92mL deionized water, and ultrasonic time 3h obtains graphene
Dispersion liquid；
(4) graphene dispersing solution is added in the mixed liquor that step (1) obtains, stirs 4h at 95 DEG C of temperature, obtains
Fluid；
(5) it is dried in vacuo fluid 12h at 110 DEG C, then fluid is ground, obtains presoma；
(6) presoma is pre-sintered 4h in hydrogen reducing atmosphere progress at 500 DEG C；Then it is carried out just at 750 DEG C
Formula is sintered 11h, obtains LiFePO4/graphene in-situ composite.
Embodiment 3
(1) by 0.3molFeSO4、0.3molH3PO4, 0.9molLiOH be added in 7L distilled water, 21.3g is then added
Citric acid is uniformly mixed, obtains mixed liquor；
(2) graphene is prepared by full liquid physics stripping method, 5g graphene, 1g is then sequentially added in the 3g concentrated sulfuric acid
Potassium permanganate, reacts 4h at 100 DEG C of temperature, collects graphene and is washed to pH value to be neutral to get to modified graphite
Alkene；
(3) by 3g modified graphene, ultrasonic disperse is uniform in 47mL deionized water, and ultrasonic time 5h obtains graphene
Dispersion liquid；
(4) graphene dispersing solution is added in the mixed liquor that step (1) obtains, stirs 4h at 98 DEG C of temperature, obtains
Fluid；
(5) it is dried in vacuo fluid 10h at 105 DEG C, then fluid is ground, obtains presoma；
(6) presoma is pre-sintered 5h in hydrogen reducing atmosphere progress at 450 DEG C；Then it is carried out just at 800 DEG C
Formula is sintered 12h, obtains LiFePO4/graphene in-situ composite.
LiFePO4 prepared by the present invention/graphene in-situ composite electron microscope is as shown in Figure 1.
Standard phosphate iron lithium and LiFePO4 prepared by the present invention/graphene in-situ composite performance are carried out pair
Than the results are shown in Table 1:
| Standard phosphate iron lithium | Graphene In-situ reaction LiFePO4 | |
| Carbon content | 4% | 8.5% |
| Conductivity | 0.65×10-5S/cm | 1.41×10-3S/cm |
| Specific surface area | 15m2/g | 45m2/g |
| 0.2C electric discharge gram volume | 150mAh/g | 180mAh/g |
| 1C electric discharge gram volume | 130mAh/g | 170mAh/g |
| 5C electric discharge gram volume | 110mAh/g | 150mAh/g |
| 10C electric discharge gram volume | 100mAh/g | 140mAh/g |
| 20C electric discharge gram volume | 70mAh/g | 115mAh/g |
| 10C recycles 1500 capacity retention ratios | 65% | 95% |
As shown in Table 1, LiFePO4 prepared by the present invention/graphene in-situ composite has good charge and discharge capacitor
Amount, under conditions of charge-discharge magnification is 20C, electric discharge gram volume is 115mAh/g；Under conditions of charge-discharge magnification is 10C,
The capacity retention ratio that circulation is 1500 times is about 95%, has excellent cycle performance；Compared with traditional lithium iron phosphate positive material,
LiFePO4 prepared by the present invention/graphene in-situ composite gram volume improves 20%, sufficiently solves traditional ferric phosphate
The low problem of lithium material charging capacity.LiFePO4 prepared by the present invention/graphene in-situ composite conductivity be 1.41 ×
10-3S/cm has good conductive property.
Claims (7)
1. a kind of LiFePO4/graphene in-situ composite preparation method, which comprises the following steps:
(1) by FeSO4、H3PO4, LiOH be added in distilled water, citric acid is then added, be uniformly mixed, obtain mixed liquor；
FeSO4、H3PO4, LiOH molar ratio be 1:1:3；The quality of citric acid is LiFePO4Theoretical generate the 45% of quality；Distillation
Water and the mass ratio for the substance total amount being added are 30-50:1；
(2) graphene is carried out weak oxide to be modified, obtains modified graphene；
(3) by modified graphene, ultrasonic disperse is uniform in deionized water, and ultrasonic time 3-5h obtains graphene dispersing solution；
The mass fraction of modified graphene is 5-10% in graphene dispersing solution；
(4) graphene dispersing solution is added in the mixed liquor that step (1) obtains, stirs 3-4h at 90-100 DEG C of temperature, obtains
To fluid；
(5) dry fluid, then fluid is ground, obtain presoma；
(6) presoma is pre-sintered, is then formally sintered, obtain LiFePO4/graphene in-situ composite.
2. LiFePO4 according to claim 1/graphene in-situ composite preparation method, which is characterized in that institute
The graphene stated is prepared by full liquid physics stripping method, and the number of plies of graphene is 3-6.
3. LiFePO4 according to claim 1/graphene in-situ composite preparation method, which is characterized in that institute
The weak oxide stated it is modified the following steps are included:
(a) graphene, potassium permanganate are sequentially added in the concentrated sulfuric acid, react 4-5h at 90-100 DEG C of temperature；The concentrated sulfuric acid, graphite
The mass ratio that alkene, potassium permanganate are added is 3:5:1；
(b) it collects graphene and is washed to pH value to be neutral to get to modified graphene.
4. LiFePO4 according to claim 1/graphene in-situ composite preparation method, which is characterized in that institute
Stating dry is vacuum drying, and temperature is 100-120 DEG C, time 10-15h.
5. LiFePO4 according to claim 1/graphene in-situ composite preparation method, which is characterized in that institute
It states pre-sintering to carry out in hydrogen reducing atmosphere, the temperature of pre-sintering is 400-500 DEG C, time 3-5h.
6. LiFePO4 according to claim 1/graphene in-situ composite preparation method, which is characterized in that institute
Stating the temperature being formally sintered is 700-800 DEG C, time 10-12h.
7. a kind of LiFePO4/graphene in-situ composite that method described in any one of claims 1-6 is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109686962A (en) * | 2019-01-21 | 2019-04-26 | 新奥石墨烯技术有限公司 | Prepare method, the anode, battery of iron phosphate compound anode material of lithium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109686962A (en) * | 2019-01-21 | 2019-04-26 | 新奥石墨烯技术有限公司 | Prepare method, the anode, battery of iron phosphate compound anode material of lithium |
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