CN110371940A - A kind of LiMnPO4Presoma template Li3PO4Tiny balloon and its preparation method and application - Google Patents
A kind of LiMnPO4Presoma template Li3PO4Tiny balloon and its preparation method and application Download PDFInfo
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- CN110371940A CN110371940A CN201910831328.0A CN201910831328A CN110371940A CN 110371940 A CN110371940 A CN 110371940A CN 201910831328 A CN201910831328 A CN 201910831328A CN 110371940 A CN110371940 A CN 110371940A
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
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- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/00—Electrodes
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Abstract
The invention discloses a kind of LiMnPO4Presoma template Li3PO4Tiny balloon and its preparation method and application, belong to the positive electrode technical field of lithium ion battery, method: sodium hydroxide, lithium salts, phosphate are added to diethylene glycol (DEG) and sufficiently reacted with the in the mixed solvent of deionized water, reaction product is successively separated by solid-liquid separation, washs, dry, obtains target product Li3PO4Tiny balloon adjusts the dosage of diethylene glycol (DEG) or sodium hydroxide in reaction, can obtain diameter in the Li of 100nm ~ 5 μm3PO4Tiny balloon also discloses application of the tiny balloon of preparation in high performance lithium ion battery anode material.The present invention, synthesis technology is simple and convenient to operate, raw material is cheap and easily-available, equipment requirement is low, is suitable for industrialized production.
Description
Technical field
The present invention relates to the positive electrode technical field of lithium ion battery, specifically a kind of LiMnPO4Presoma template
Li3PO4Tiny balloon and its preparation method and application.
Background technique
Lithium ion battery is relative to other secondary cells such as lead storage, ni-Cd with operating temperature is wide, output voltage is high, puts certainly
The advantages that rate is low, specific power is high, specific energy is big.With the continuous promotion of people's demand, lithium ion battery just towards it is lighter, more pacify
Entirely, specific energy is bigger, the higher direction of specific power is developed.Positive electrode is the important component of lithium ion battery, it grinds
Study carefully with exploitation play the role of to the performance of lithium ion battery overall performance it is vital.Positive electrode can be divided into layer by structure
Shape structure, spinel structure etc., the wherein LiMnPO of forsterite type structure4Positive electrode has at low cost, highly-safe, knot
The features such as structure is stable, environmental-friendly, is one of the hot spot positive electrode studied at present.However its ion and electronic conductivity is but
It is very low, cause it forthright very poor again.Currently, passing through the nanosizing of material grains size, to shorten the migration distance of ion, in turn
Improve the high rate performance of material.But nanosizing crystal grain, it will lead to the reduction of positive electrode tap density, the volume energy of battery
Density reduces.The crystal grain of nanosizing has very high specific surface area, side reaction easily occurs when with electrolyte contacts, so as to cause
Capacitance loss and safety problem.In addition, the crystal grain of nanosizing, hardly possible is uniformly mixed with conductive agent, binder, is added in battery preparation
Work craftsmanship is poor.These lead to the problem of with crystallite dimension nanosizing, seriously hinder LiMnPO4The quotient of positive electrode
With exploitation and practical application.
There is high tap density, moderate specific surface area and good by the Hollow Microspheres Structure of nanocrystal assembling
The features such as processing technology got well, the dimensional effect of nanocrystal can either be played, and can be avoided the appearance of the above problem,
It is widely used in the numerous areas such as energy storage, biological medicine and chemical catalysis.Currently, the positive electrode of tiny balloon pattern
Preparation method has hard template method, this special Grindelwald curing method etc., wherein from template is sacrificed with high-efficient, simple process, knot
The advantages that structure controllability is strong.Using the LiMnPO for preparing tiny balloon pattern from sacrifice template method4When positive electrode, also deposit at present
Regulate and control difficulty in the size of tiny balloon, this affects LiMnPO4The adjusting of positive electrode tap density and volume energy are close
The optimization of degree, therefore there is an urgent need to a kind of size regulation and control schemes of tiny balloon pattern presoma template.
Summary of the invention
It is an object of the present invention to be directed to LiMnPO4The low tap density of nano anode material, provides a kind of LiMnPO4Before
Drive body template Li3PO4Tiny balloon and its preparation method and application comes by adjusting the dosage of diethylene glycol (DEG) solvent or sodium hydroxide
Regulate and control Li3PO4The size of tiny balloon, to improve the tap density of material, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of LiMnPO4Presoma template Li3PO4The preparation method of tiny balloon, is specifically realized by the following steps:
S1: by diethylene glycol (DEG) and deionized water mixed preparing mixed solvent；
S2: being added sequentially in the mixed solvent for sodium hydroxide, lithium salts and phosphate at 800 ~ 1200rpm of low whipping speed,
So that it is 0.1 ~ 5mol/L, lithium that hydroxide ion concentration, which is 1 ~ 10mol/L, lithium ion and phosphorus acid ion concentration, in mixed solution
Ion and phosphate anion molar ratio are 3:(0.9 ~ 1.1)；
S3: 5 ~ 60min is reacted under stirring；
S4: reaction product is successively separated by solid-liquid separation, washs, dry, obtains the Li of diameter 100nm ~ 5 μm3PO4It is hollow micro-
Ball.
As a further solution of the present invention: lithium salts described in step S2 is acetic acid dihydrate lithium, sulfuric acid monohydrate lithium, chlorine
Change lithium, lithium lactate or Lithium formate hydrate, phosphate is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or tertiary sodium phosphate.
As a further solution of the present invention: the concrete operations of separation of solid and liquid described in step S4 are as follows: using filtering side
Method separates product, obtains the solid precipitating in product.
As a further solution of the present invention: the concrete operations of washing described in step S4 are as follows: using deionization first
The solid precipitating that water washing is separated by solid-liquid separation, is washed 3 ~ 5 times, then washed 1 ~ 2 time using dehydrated alcohol, solid after being washed
Precipitating.
As further scheme of the invention: dry concrete operations described in step S4 are as follows: by solid after washing
Precipitating is placed in a vacuum drying oven, and 8 ~ 16h is dried in vacuo at 50 ~ 70 DEG C.
As presoma template Li3PO4Tiny balloon can prepare LiMnPO4Positive electrode, and in high-performance lithium ion electricity
It is applied in pond.
Compared with prior art, the beneficial effects of the present invention are:The use of diethylene glycol (DEG) or sodium hydroxide is adjusted in the reaction
Amount, can be achieved with Li3PO4The regulation of tiny balloon size.Simple process, easy to operate, raw material is cheap and easily-available, equipment requirement is low,
Suitable for industrialized production.Prepared Li3PO4Tiny balloon size adjustable regular shape, is evenly distributed, better crystallinity degree.
Detailed description of the invention
Fig. 1 is Li prepared in the embodiment of the present invention 13PO4Tiny balloon and LiMnPO4The XRD spectrum of tiny balloon.
Fig. 2 ~ 6 are Li prepared in the embodiment of the present invention 13PO4Tiny balloon and LiMnPO4Tiny balloon is at different times
SEM figure under several.
Fig. 7 ~ 8 are Li prepared in the embodiment of the present invention 13PO4Tiny balloon and LiMnPO4The TEM of tiny balloon schemes.
Fig. 9 is Li prepared in the embodiment of the present invention 23PO4The XRD spectrum of tiny balloon.
Figure 10 ~ 12 are Li prepared in the embodiment of the present invention 23PO4SEM figure of the tiny balloon under different multiples.
Figure 13 is Li prepared in the embodiment of the present invention 33PO4The XRD spectrum of tiny balloon.
Figure 14 ~ 16 are Li prepared in the embodiment of the present invention 33PO4SEM figure of the tiny balloon under different multiples.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1: diameter is about 3 μm of Li3PO4The preparation method of tiny balloon, and sky is prepared as presoma template
The LiMnPO of heart microballoon pattern4Positive electrode is specifically realized by the following steps:
5ml diethylene glycol (DEG) and 35ml deionized water are prepared into mixed solvent.By 100mmol under low whipping speed 1000rpm
Sodium hydroxide, 21mmol acetic acid dihydrate lithium and 7mmol ammonium dihydrogen phosphate are added sequentially in the mixed solvent.In stirring shape
30min is reacted under state.Product is separated using filter method, obtains the solid precipitating in product, then use deionization
Water washing solid precipitates 4 times, dehydrated alcohol washing 1 time, and solid precipitating is dried in vacuo 12h at 60 DEG C again after being washed, and obtains
To about 3 μm of Li of diameter3PO4Tiny balloon.
By prepared 5mmolLi3PO4Tiny balloon, tetra- acetate hydrate Asia manganese of 5mmol and 5mmol ammonium sulfate are added to
20ml ethylene glycol and 20ml deionized water prepare in the mixed solvent, and the stainless steel reaction of polytetrafluoroethyllining lining is sealed in after stirring
In kettle, it is cooled to room temperature after 180 DEG C of heat preservation 4h.Obtained solid is precipitated, is washed through deionized water washing 4 times, dehydrated alcohol
It washs 1 time, be dried in vacuo 12h at 60 DEG C, obtain about 3 μm of diameter of LiMnPO4Tiny balloon.
The Li that this test is prepared is detected using X-ray diffractometer3PO4Tiny balloon and LiMnPO4Tiny balloon, inspection
It is as shown in Figure 1 to survey result.As shown in Figure 1, the product that this test is prepared is respectively pure Li3PO4Object phase and pure
LiMnPO4Object phase.
The tiny balloon that this test is prepared is observed using scanning electron microscope, as shown in Fig. 2 ~ 6.Fig. 2 ~ 3 are
Li3PO4SEM figure under tiny balloon different multiples, by figure as can be seen that the Li that this test is prepared3PO4Tiny balloon
Diameter is about 3 μm, regular shape, is evenly distributed；Fig. 4 ~ 6 are LiMnPO4SEM figure under tiny balloon different multiples, passes through figure
It can be seen that LiMnPO4Inherit Li3PO4The appearance structure of tiny balloon, diameter are about 3 μm.
The tiny balloon being prepared using transmission electron microscope observation this test, as shown in Fig. 7 ~ 8.Fig. 7 is Li3PO4
Tiny balloon TEM figure is tiny balloon by the microballoon that experiment known to light and shade contrast comparison in Fig. 7 is prepared；Fig. 8 is
LiMnPO4Microballoon TEM schemes, as shown in Figure 8 LiMnPO4Microballoon has hollow structure.
Embodiment 2: diameter is about 1.5 μm of Li3PO4The preparation method of tiny balloon, is specifically realized by the following steps
:
8ml diethylene glycol (DEG) and 32ml deionized water are prepared into mixed solvent.By 100mmol under low whipping speed 1000rpm
Sodium hydroxide, 21mmol acetic acid dihydrate lithium and 7mmol ammonium dihydrogen phosphate are added sequentially in the mixed solvent.In stirring shape
30min is reacted under state.Product is separated using filter method, obtains the solid precipitating in product, then use deionization
Water washing solid precipitates 4 times, dehydrated alcohol washing 1 time, and solid precipitating is dried in vacuo 12h at 60 DEG C again after being washed, and obtains
To about 3 μm of Li of diameter3PO4Tiny balloon.
The Li that this test is prepared is detected using X-ray diffractometer3PO4Tiny balloon, testing result are as shown in Figure 9.It is logical
Fig. 9 is crossed it is found that the product that this test is prepared is pure Li3PO4Object phase.
The Li that this test is prepared is observed using scanning electron microscope3PO4Tiny balloon, the difference as shown in Figure 10 ~ 12
SEM figure under multiple.By figure as can be seen that the Li that this test is prepared3PO4Tiny balloon diameter is about 1.5 μm, shape
Rule is evenly distributed.
Embodiment 3: the Li that diameter is about 750nm3PO4The preparation method of tiny balloon, is specifically realized by the following steps
:
8ml diethylene glycol (DEG) and 32ml deionized water are prepared into mixed solvent.By 120mmol under low whipping speed 1000rpm
Sodium hydroxide, 21mmol acetic acid dihydrate lithium and 7mmol ammonium dihydrogen phosphate are added sequentially in the mixed solvent.In stirring shape
30min is reacted under state.Product is separated using filter method, obtains the solid precipitating in product, then use deionization
Water washing solid precipitates 4 times, dehydrated alcohol washing 1 time, and solid precipitating is dried in vacuo 12h at 60 DEG C again after being washed, and obtains
To about 3 μm of Li of diameter3PO4Tiny balloon.
The Li that this test is prepared is detected using X-ray diffractometer3PO4Tiny balloon, testing result are as shown in figure 13.
As shown in Figure 13, the product that this test is prepared is pure Li3PO4Object phase.
The Li that this test is prepared is observed using scanning electron microscope3PO4Tiny balloon, the difference as shown in Figure 14 ~ 16
SEM figure under multiple.By figure as can be seen that the Li that this test is prepared3PO4Tiny balloon diameter is about 750nm, shape
Rule is evenly distributed.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. a kind of LiMnPO4Presoma template Li3PO4The preparation method of tiny balloon, which comprises the steps of:
S1: by diethylene glycol (DEG) and deionized water mixed preparing mixed solvent；
S2: being added sequentially in the mixed solvent for sodium hydroxide, lithium salts and phosphate under certain mixing speed, so that mixing is molten
It is 0.1 ~ 5mol/L, lithium ion and phosphoric acid that hydroxide ion concentration, which is 1 ~ 10mol/L, lithium ion and phosphorus acid ion concentration, in liquid
Radical ion molar ratio is 3:(0.9 ~ 1.1)；
S3: 5 ~ 60min is reacted under stirring；
S4: reaction product is successively separated by solid-liquid separation, washs, dry, obtains the Li of diameter 100nm ~ 5 μm3PO4Tiny balloon.
2. a kind of LiMnPO according to claim 14Presoma template Li3PO4The preparation method of tiny balloon, feature
Be, lithium salts described in step S2 be acetic acid dihydrate lithium, sulfuric acid monohydrate lithium, lithium chloride, lithium lactate or Lithium formate hydrate,
Phosphate is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or tertiary sodium phosphate.
3. a kind of LiMnPO according to claim 24Presoma template Li3PO4The preparation method of tiny balloon, feature
It is, mixing speed is 800 ~ 1200rpm in step S2.
4. a kind of LiMnPO according to claim 14Presoma template Li3PO4The preparation method of tiny balloon, feature
It is, the concrete operations of separation of solid and liquid described in step S4 are as follows: product is separated using filter method, is obtained in product
Solid precipitating.
5. a kind of LiMnPO according to claim 1 or 44Presoma template Li3PO4The preparation method of tiny balloon, it is special
Sign is that the concrete operations of washing described in step S4 are as follows: adopting the solid for being washed with deionized and being separated by solid-liquid separation and obtaining first
Precipitating is washed 3 ~ 5 times, then is washed 1 ~ 2 time using dehydrated alcohol, and solid precipitates after being washed.
6. a kind of LiMnPO according to claim 54Presoma template Li3PO4The preparation method of tiny balloon, feature
It is, dry concrete operations described in step S4 are as follows: solid precipitating after washing is placed in a vacuum drying oven, and 50 ~
8 ~ 16h is dried in vacuo at 70 DEG C.
7. a kind of LiMnPO4Presoma template Li3PO4Tiny balloon, which is characterized in that be as described in claim any one of 1-6
Method be prepared.
8. a kind of LiMnPO according to claim 74Presoma template Li3PO4Tiny balloon is in high performance lithium ion battery
Positive electrode in application.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113540455A (en) * | 2021-05-31 | 2021-10-22 | 佛山市德方纳米科技有限公司 | Hollow carbon-coated lithium iron phosphate particles and preparation method and application thereof |
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| CN101296863A (en) * | 2005-10-28 | 2008-10-29 | 丰田自动车株式会社 | Method for manufacturing LiMnPO4 |
| US20090117464A1 (en) * | 2007-11-07 | 2009-05-07 | Korea Institute Of Science And Technology | Fabrication method for electrode active material and lithium battery comprising electrode active material fabricated therefrom |
| CN101506094A (en) * | 2006-08-21 | 2009-08-12 | 株式会社Lg化学 | Method for preparing lithium metal phosphate |
| CN102629687A (en) * | 2012-05-03 | 2012-08-08 | 哈尔滨工业大学 | Shape control synthesis method of LiMnPO4 electrode materials |
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2019
- 2019-09-04 CN CN201910831328.0A patent/CN110371940A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101296863A (en) * | 2005-10-28 | 2008-10-29 | 丰田自动车株式会社 | Method for manufacturing LiMnPO4 |
| CN101506094A (en) * | 2006-08-21 | 2009-08-12 | 株式会社Lg化学 | Method for preparing lithium metal phosphate |
| US20090117464A1 (en) * | 2007-11-07 | 2009-05-07 | Korea Institute Of Science And Technology | Fabrication method for electrode active material and lithium battery comprising electrode active material fabricated therefrom |
| CN102629687A (en) * | 2012-05-03 | 2012-08-08 | 哈尔滨工业大学 | Shape control synthesis method of LiMnPO4 electrode materials |
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| XIAOLIANG PAN, ET AL: "Self-templating preparation and electrochemical performance of LiMnPO4 hollow microspheres", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113540455A (en) * | 2021-05-31 | 2021-10-22 | 佛山市德方纳米科技有限公司 | Hollow carbon-coated lithium iron phosphate particles and preparation method and application thereof |
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