CN106981638A - The method for depositing Nanometer Copper on iron phosphate lithium positive pole surface using magnetron sputtering technique - Google Patents
The method for depositing Nanometer Copper on iron phosphate lithium positive pole surface using magnetron sputtering technique Download PDFInfo
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Abstract
The present invention relates to a kind of method that utilization magnetron sputtering deposits Nanometer Copper on iron phosphate lithium positive pole surface, belong to the technical field of lithium ion battery electrode material, it is characterised in that：Predecessor containing lithium, iron, phosphorus and carbon is mixed and ball milling is carried out, after being pressed into button shape after the slurry drying after ball milling, and is carried out heat treatment in sections under argon atmosphere, finally gives the lithium iron phosphate positive material of carbon coating.The Kynoar of the LiFePO4, the conductive black of 10 ~ 20 parts by weight and 5 ~ 10 parts by weight of 70 ~ 80 parts by weight is weighed respectively, sequentially pour into the mortar containing N methyl pyrrolidones, it is fully ground uniformly, slurry is coated on aluminium foil, vacuum drying obtains iron phosphate lithium electrode piece.Using magnetron sputtering technique, the electrode slice for being coated with completion is placed in sputtering chamber, by Nanometer Copper modification on the positive plate of LiFePO4.Using method of the present invention, the rate charge-discharge performance and cyclical stability of battery are significantly improved, and improvement is not influenceed by carbon coating.
Description
Technical field
Patent of the present invention belongs to lithium rechargeable battery field of material technology, and in particular to one kind is using magnetron sputtering in phosphorus
The method that sour iron lithium positive electrode surface deposits Nanometer Copper.
Technical background
Since 21 century, global energy crisis and environmental problem become increasingly conspicuous, the traditional energy such as oil coal
Deng not adapt to world today's green energy resource theme, so far various novel energies be exploited and people production with
Huge effect is played in life.And be exactly in such overall background as the lithium ion battery of the superior energy storage device of a new generation
Under arise at the historic moment.Have the advantages that operating voltage is high, energy density is high, pollution-free and good cycle, lithium rechargeable battery
It is widely used in portable digital equipment, electric car（EVs）, hybrid electric vehicle (PHEVs) and the arms mobile electron such as equipment
Field of terminal equipment.
The positive electrode of lithium rechargeable battery has a variety of, for example LiCoO2、LiMn2O4、LiNi1/3Co1/3Mn1/3、
LiNi0.5Mn1.5O4And LiFeSiO4Etc..The LiFePO of olivine-type4Because it has very high specific capacity（170mAhg-1）、
Abundant raw material, the cheap market price and it is environmentally friendly the advantages of, increasingly paid close attention to by people.The especially material
The intrinsic safety and stability sexual satisfaction electric car of material（EVs）, hybrid electric vehicle（PHEVs）The strict requirements proposed to lithium battery.
Cause the LiFePO of olivine-type4Widely studied and rapid development is obtained.
Yet with the limitation of lattice structure, LiFePO4Show low electronic conductivity（10-9 S cm-2）And lithium ion
Diffusivity（10-14 ~ 10-16 S-1 cm2）, under powerful charging or discharging current, LiFePO4Produce the damage of big irreversible capacity
Lose.In order to improve the chemical property of LiFePO4, modified method is mainly manifested in carbon coating, metal oxide bag at present
Cover, transition metal mix and the effective means such as nanosizing on.The nanosizing of LiFePO4 can effectively shorten lithium ion
Diffusion path, considerably improves the high rate performance of material.And carbon coating and the common cladding of oxide, not only improve precursor granule
Between electric conductivity, and can suppress the erosion of hydrofluoric acid in electrolyte, improve the cyclical stability of battery.The ginseng of metal ion
It is miscellaneous, improved in root in LiFePO4 electric conductivity, promote the chemical property of material.In Chinese invention patent
Specification（A kind of " preparation method of nano-grade lithium iron phosphate " application number: CN103647044A）In, using in microwave field with
500-800 degrees Celsius of reaction temperature calcining precursor and the mixture of charcoal, successfully prepares the superior nanometer of chemical property
LiFePO4.Chinese invention patent specification（" preparation method of carbon coating hierarchical organization LiFePO4 " application number:
CN103956493A）, using lithium source, source of iron, phosphorus source and chelating agent as reaction source, by traditional hydro-thermal reaction, prepare carbon bag
The LiFePO4 of hierarchical organization is covered, excellent chemical property is not only shown, and prepares repeatability height, reality is fully met
Produce the requirement to high energy storage device.Chinese invention patent specification（" a kind of doped iron lithium phosphate and preparation method " applies
Number：201410764158.6）, by the method for ball milling, there is provided a kind of excellent anode material doped titanium phosphoric acid of electric conductivity
Iron lithium.In a word, surface modification is mixed with ion can effectively improve the chemical property of electrode material.
In recent years, metal oxide is directly modified to be considered to be in electrode surface and improves having for battery performance row
One of means of effect.And with it is easy to operate, prepare the controllable magnetron sputtering technique of film thickness, be expected to be used in electrode table
In the modification of face.In addition, selection of the magnetron sputtering technique to sputtering source is unrestricted, the material of choosing multiple enters to electrode surface
Row modification.This applies to battery surface modification for magnetron sputtering nothing but and provides strong chip.On modification electrode surface, phase
For metal oxide, introduce for the Nanometer Copper with higher electric conductivity, this is rich for the electric property for improving battery
There is great possibility.This patent discloses a kind of method that utilization magnetron sputtering deposits Nanometer Copper on iron phosphate lithium positive pole surface
And improve battery high-rate charge-discharge capability, in particular for improving the charge-discharge performance of LiFePO4.
The content of the invention
It is an object of the invention to by magnetron sputtering technique on the positive electrode surface even application of LiFePO4 copper nanometer
Layer, LiFePO4 is solved with this in powerful charge-discharge performance and cyclical stability.
In order to reach the purpose of the present invention use technical scheme be：
（1）The LiFePO4 of carbon coating is obtained using high-temperature solid phase reaction method
1）By predecessor lithium acetates of the component A containing lithium or lithium carbonate, component B phosphorous predecessor ammonium dihydrogen phosphate or phosphoric acid hydrogen two
Ammonium, component C predecessor sucrose or glucose containing charcoal, with ferrous oxalate in absolute ethyl alcohol or acetone ball milling 12 ~ 24 hours, turn
Speed is 180 ~ 350 turns per minute.Wherein component A, component B, the molal weight ratio of component C and ferrous oxalate are 1.03：1~1.08：
0.05~0.07：0.92~1.08.
2）Pulpous state predecessor after ball milling is dried 12 ~ 24 hours in 60 ~ 80 DEG C of drying box, yellowish toner is formed
End, pale yellow powder is ground after 30 ~ 120 minutes in agate mortar, is pressed into button shape, and pressure size is 10Mpa ~ 20Mpa.
3）Button shape presoma is placed in atmosphere furnace, some charcoals are placed in tube furnace axial direction precursor front and rear sides,
Calcined in two steps under protective gas nitrogen or argon atmosphere：
The first step：Calcining heat is 350 ~ 400 DEG C, and calcination time is 3 ~ 6 hours, and the heating rate of sintering temperature is raised to from room temperature
For 3 ~ 5 DEG C per minute, first step sintering is down to room temperature under protection atmosphere after finishing together with stove, obtains the fluffy phosphorus of black
Sour iron lithium block.It is placed in after being ground 30 ~ 60 minutes in agate mortar, is pressed into button shape, pressure size is 10Mpa ~ 20Mpa；
Second step：Calcining heat is 650 ~ 750 DEG C, and calcination time is 10 ~ 12 hours, and the heating speed of sintering temperature is raised to from room temperature
Rate is 3 ~ 5 DEG C per minute, and sintering is down to room temperature under protection atmosphere after finishing together with stove, obtains the phosphoric acid of black carbon coating
Iron lithium powder.
（2）The preparation of iron phosphate lithium positive pole piece
1）Difference ratio 70 ~ 80 by weight：10~20：5 ~ 10 weigh LiFePO4 or LiFePO4/ C, conductive black（SP）With
Kynoar (PVDF).PVDF is placed in agate mortar first, 1-METHYLPYRROLIDONE is poured into, treats that PVDF is dissolved in N- first
After base pyrrolidones, SP and LiFePO are separately added into4Or LiFePO4One of/C, is fully ground uniformly, grinds to form thin mud
It is coated on after shape on aluminium foil, is heated up again after predrying 3 ~ 6 hours in 60 DEG C of vacuum drying chamber and dry 12 as 100 ~ 110 DEG C
~ 24 hours, obtain iron phosphate lithium positive pole piece.Iron phosphate lithium positive pole piece phosphoric acid iron lithium or LiFePO every square centimeter during coating4/
3.0 ~ 6.0 milligrams of C.
（3）Nano copper particle is sputtered on lithium iron phosphate positive material surface
1）Iron phosphate lithium positive pole piece is positioned in sputtering chamber as sputtering substrate, is evacuated to 10-4Pa, intracavitary bottom-heated
Device temperature setting is between 70 ~ 100 DEG C.
2）Pure argon is passed through in toward sputtering chamber, control gas flow rate is between 20 ~ 40sccm, regulation breather valve control sputtering
The operating air pressure of intracavitary is between 0.1 ~ 2Pa.Set operating power between 60 ~ 80W during sputtering, start RF device, intracavitary is opened
Brightness；The operating distance of target and sputtering substrate is 10 ~ 15cm；By regulating and controlling sputtering time parameter, by the nanometer Copper thin film of sputtering
Thickness control is between 5 nanometers ~ 20 nanometers.
3）The LiFePO4 or LiFePO for having Nanometer Copper will be sputtered4/ C positive plate is placed in 80 ~ 100 DEG C of vacuum drying chambers
Dry 8 ~ 12 hours, obtain utilization magnetron sputtering of the present invention and deposit the ferric phosphate of Nanometer Copper on iron phosphate lithium positive pole surface
Lithium positive plate.
Nanometer Copper of the present invention grinds target pioneer purchased from wide light crystalline substance.
Using method of the present invention, step is simple, after iron phosphate lithium positive pole piece surface sputtering Nanometer Copper, battery
High power charging-discharging and stable circulation performance significantly improve, improvement is not had carbon coating to be influenceed by LiFePO4, this hair
The bright electrode surface nanometer copper method provided as detailed above, its application highly significant.
Brief description of the drawings
Fig. 1 is the iron phosphate lithium positive pole piece SEM figures of Nanometer Copper modification.
Fig. 2 is the discharge platform that Nanometer Copper modifies LiFePO4.
Embodiment
In order to illustrate influence of the magnetron sputtering Nanometer Copper to the chemical property of LiFePO4, assembled using traditional technique
It is electrolyte, EC (carbonic acid that R2025 simulated batteries, wherein electrolyte, which choose the LiPF6/EC/DEC/DMC that concentration is 1.0mol/L,
Vinyl acetate)/DEC (diethyl carbonate)/DMC (dimethyl carbonate) be double solvents, the volume ratio of three（EC:DEC:DMC）For
1：1：1, LiPF6 is conducting salt.Using LiFePO4 as test electrode, from metal lithium sheet be reference electrode, polypropylene screen
For battery diaphragm.At room temperature, charge-discharge battery is come with 0.5C, 1C, 3C, 5C current density, wherein 1 C=170 milliampere
When/gram, test voltage scope 2.5V-4.3V.
Embodiment 1
1st, the LiFePO4 of carbon coating is obtained using high-temperature solid phase reaction method
1.6500g lithium acetates, 2.8758g ammonium dihydrogen phosphates, 0.6565g sucrose and 4.4974g ferrous oxalates are mixed in ball grinder
In, add ethanol and do not had medicine just, ball milling 24 hours, rotating speed is 200 turns per minute, obtains flaxen slurry；By slurry
It is placed in 80 DEG C of drying box and dries 12 hours, forms pale yellow powder；Pale yellow powder is ground 60 points in agate mortar
Zhong Hou, is pressed into button shape, and pressure size is 20Mpa.Button shape presoma is placed in atmosphere furnace, high-purity argon gas, first is passed through
Walk calcining heat be 350 DEG C, calcination time 6 hours, heating rate be 3 DEG C/it is per minute；Calcination finish after protection atmosphere under with
Stove is down to room temperature together, obtains the fluffy LiFePO4 block of black.The fluffy LiFePO4 block of black is placed in agate
Grinding was shaken up after 30 minutes in mortar, was pressed into button shape, pressure size is 20Mpa.This button shape medicine is placed through height again
Carrying out second in the atmosphere furnace of pure argon to calcine, temperature is 750 DEG C, calcination time is 12 hours, heating rate is 3 DEG C/it is every
Minute, sintering is down to room temperature under protection atmosphere after finishing together with stove, obtains the iron phosphate powder of black carbon coating.
2nd, the preparation of iron phosphate lithium positive pole piece
Ratio weighs 0.14g respectively by weight has the iron phosphate powder of carbon coating, 0.04g carbon blacks (SP) and 0.02g poly- inclined
PVDF, is placed in agate mortar, pours into 1-METHYLPYRROLIDONE by PVF (PVDF) first, treats that PVDF is dissolved in N- methyl
After pyrrolidones, SP and LiFePO are separately added into4, it is fully ground uniformly, is coated on after grinding to form sposh pulpous state on aluminium foil,
Heat up and dried 12 hours as 110 DEG C again after predrying 3 hours in 60 DEG C of vacuum drying chamber, obtain iron phosphate lithium positive pole piece.
Using magnetron sputtering technique, Nanometer Copper modification is carried out to iron phosphate lithium positive pole piece, pole piece is placed in sputtering chamber,
10 are evacuated in cavity-4Pa, the temperature setting of substrate heater is 100 DEG C, and the operating distance of target and pole piece is 10cm.Connect
Get off, toward sputtering chamber in be passed through pure argon, setting gas flow rate is the work gas in 30sccm, regulation breather valve control sputtering chamber
Press as 0.7Pa.Under 80W operating power, start RF device, intracavitary starter, the sputtering of progress one minute.It is to be sputtered to terminate
Afterwards, the positive plate of LiFePO4 is placed in 80 DEG C of vacuum drying chambers and dried 12 hours.The LiFePO4 of Nanometer Copper modification is just
Pole piece SEM figures are as shown in Figure 1.
The iron phosphate lithium positive pole piece that there is Nanometer Copper on surface is cut into the disk of 1.25 centimetres of diameter with mould and with 3MP power
By iron phosphate lithium positive pole piece surface flatten, by 80 DEG C dry 5 hours after be put into the glove box full of high-purity argon gas, water,
Oxygen index, which is respectively less than under 1 ppm environment, is assembled into R2025 type simulated batteries, has been encapsulated in glove box and 12 are stood after simulated battery
Hour, proceed by electrochemical property test.At room temperature, battery, test voltage are tested with 0.5C, 1C, 3C, 5C multiplying power
Scope 2.5V-4.3V.Charge-discharge test result shows that under the conditions of 0.5C rate charge-discharges, surface does not sputter Nanometer Copper
The specific discharge capacity of LiFePO4 be 140mAh/g, and the specific discharge capacity of LiFePO4 that surface sputtering has Nanometer Copper is
139mAh/g；Under the conditions of 1C rate charge-discharges, surface does not have the specific discharge capacity of the LiFePO4 of Nanometer Copper to be 129mAh/
G, and the specific discharge capacity that surface sputtering has the LiFePO4 of Nanometer Copper is 133mAh/g；Under the conditions of 3C rate charge-discharges, table
Face does not have the specific discharge capacity of the LiFePO4 of Nanometer Copper to be 74mAh/g, and surface sputtering has putting for the LiFePO4 of Nanometer Copper
Electric specific capacity is 115mAh/g；Under the conditions of 5C rate charge-discharges, surface does not have the electric discharge ratio of the LiFePO4 of Nanometer Copper modification
Capacity is 57mAh/g, and the specific discharge capacity that surface modification has the LiFePO4 of Nanometer Copper is 101mAh/g.Nanometer Copper modifies phosphorus
The discharge platform of sour iron lithium is as shown in Figure 2.Even if illustrating LiFePO4 has a carbon coating, the electricity of the modification of Nanometer Copper to LiFePO4
Chemical property tool improves.
Embodiment 2
1st, the LiFePO4 of carbon coating is obtained using high-temperature solid phase reaction method
1.1550g lithium carbonates, 3.5961g ammonium dihydrogen phosphates, 0.5354g glucose and 4.4974g ferrous oxalates are mixed in ball milling
In tank, add ethanol and do not had medicine just, ball milling 12 hours, rotating speed is 350 turns per minute, obtains flaxen slurry；Will slurry
Material is placed in 60 DEG C of drying box and dried 12 hours, forms pale yellow powder；Pale yellow powder is ground 120 in agate mortar
After minute, button shape is pressed into, pressure size is 15Mpa.Button shape presoma is placed in atmosphere furnace, high-purity argon gas is passed through, the
One-step calcination temperature be 350 DEG C, calcination time 3 hours, heating rate be 5 DEG C/it is per minute；It is calcined after finishing under protection atmosphere
Room temperature is down to together with stove, the fluffy LiFePO4 block of black is obtained.The fluffy LiFePO4 block of black is placed in agate
Grinding was shaken up after 30 minutes in Nao mortars, was pressed into button shape, pressure size is 10Mpa.This button shape medicine is placed through again
Carrying out second in the atmosphere furnace of high-purity argon gas to calcine, temperature is 650 DEG C, calcination time is 12 hours, heating rate is 3 DEG C/
Per minute, sintering is down to room temperature under protection atmosphere after finishing together with stove, obtains the iron phosphate powder of black carbon coating.
2nd, the preparation of iron phosphate lithium positive pole piece
Ratio weighs 0.14g respectively by weight has the iron phosphate powder of carbon coating, 0.04g carbon blacks (SP) and 0.02g poly- inclined
PVDF, is placed in agate mortar, pours into 1-METHYLPYRROLIDONE by PVF (PVDF) first, treats that PVDF is dissolved in N- methyl
After pyrrolidones, SP and LiFePO are separately added into4, it is fully ground uniformly, is coated on after grinding to form sposh pulpous state on aluminium foil,
Heat up and dried 12 hours as 110 DEG C again after predrying 3 hours in 60 DEG C of vacuum drying chamber, obtain iron phosphate lithium positive pole piece.
Using magnetron sputtering technique, Nanometer Copper modification is carried out to iron phosphate lithium positive pole piece, pole piece is placed in sputtering chamber,
10 are evacuated in cavity-4Pa, the temperature setting of substrate heater is 100 DEG C, and the operating distance of target and pole piece is 10cm.Connect
Get off, toward sputtering chamber in be passed through pure argon, setting gas flow rate is the work gas in 30sccm, regulation breather valve control sputtering chamber
Press as 0.7Pa.Under 60W operating power, start RF device, intracavitary starter, the sputtering of progress one minute.It is to be sputtered to terminate
Afterwards, the positive plate of LiFePO4 is placed in 100 DEG C of vacuum drying chambers and dried 12 hours.
The iron phosphate lithium positive pole piece that there is Nanometer Copper on surface is cut into the disk of 1.25 centimetres of diameter with mould and with 3MP power
By iron phosphate lithium positive pole piece surface flatten, by 80 DEG C dry 5 hours after be put into the glove box full of high-purity argon gas, water,
Oxygen index, which is respectively less than under 1 ppm environment, is assembled into R2025 type simulated batteries, has been encapsulated in glove box and 12 are stood after simulated battery
Hour, proceed by electrochemical property test.At room temperature, battery, test voltage are tested with 0.5C, 1C, 3C, 5C multiplying power
Scope 2.5V-4.3V.Charge-discharge test result shows that under the conditions of 0.5C rate charge-discharges, surface does not sputter Nanometer Copper
The specific discharge capacity of LiFePO4 be 138mAh/g, and the specific discharge capacity of LiFePO4 that surface sputtering has Nanometer Copper is
141mAh/g；Under the conditions of 1C rate charge-discharges, surface does not have the specific discharge capacity of the LiFePO4 of Nanometer Copper to be 132mAh/
G, and the specific discharge capacity that surface sputtering has the LiFePO4 of Nanometer Copper is 136mAh/g；Under the conditions of 3C rate charge-discharges, table
Face does not have the specific discharge capacity of the LiFePO4 of Nanometer Copper to be 75.5mAh/g, and surface sputtering has the LiFePO4 of Nanometer Copper
Specific discharge capacity is 113mAh/g；Under the conditions of 5C rate charge-discharges, surface does not have the electric discharge of the LiFePO4 of Nanometer Copper modification
Specific capacity is 58.5mAh/g, and the specific discharge capacity that surface modification has the LiFePO4 of Nanometer Copper is 103mAh/g.
In summary, Nanometer Copper is deposited on iron phosphate lithium positive pole surface using magnetron sputtering technique the invention discloses one kind
Method, realize the lifting to electrochemical performances of lithium iron phosphate.
The object, technical solutions and advantages of the present invention are further described by above-listed preferred embodiment, are answered
Understand, within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc. should be included in
Within protection scope of the present invention.
Claims (5)
1. a kind of method that utilization magnetron sputtering technique deposits Nanometer Copper on iron phosphate lithium positive pole surface, it is characterised in that：
1）By predecessor lithium acetates of the component A containing lithium or lithium carbonate, component B phosphorous predecessor ammonium dihydrogen phosphate or phosphoric acid hydrogen two
Ammonium, component C predecessor sucrose or glucose containing charcoal, with ferrous oxalate in absolute ethyl alcohol or acetone ball milling 12 ~ 24 hours, turn
Speed is 180 ~ 350 turns per minute；Wherein component A, component B, the molal weight ratio of component C and ferrous oxalate are 1.03：1~1.08：
0.05~0.07：0.92~1.08；
2）Pulpous state predecessor after ball milling is dried 12 ~ 24 hours in 60 ~ 80 DEG C of drying box, pale yellow powder is formed, will
Pale yellow powder is ground after 30 ~ 120 minutes in agate mortar, is pressed into button shape, and pressure size is 10Mpa ~ 20Mpa；
3）Button shape presoma is placed in atmosphere furnace, some charcoals are placed in tube furnace axial direction precursor front and rear sides, protected
Calcined in two steps under shield gas nitrogen or argon atmosphere, obtain the iron phosphate powder of black carbon coating；
4）Difference ratio 70 ~ 80 by weight：10~20：5 ~ 10 weigh LiFePO4 or LiFePO4/ C, conductive black and poly- inclined fluorine
Kynoar, is placed in agate mortar by ethene first, pours into 1-METHYLPYRROLIDONE, treats that PVDF is dissolved in N- methylpyrroles
After alkanone, conductive black and LiFePO are separately added into4Or LiFePO4One of/C, is fully ground uniformly, grinds to form thin mud
It is coated on after shape on aluminium foil, iron phosphate lithium positive pole piece is obtained after drying；
5）Iron phosphate lithium positive pole piece is positioned in sputtering chamber as sputtering substrate, is evacuated to 10-4Pa, intracavitary bottom heater
Temperature setting is between 70 ~ 100 DEG C；
6）Pure argon is passed through in toward sputtering chamber, control gas flow rate is between 20 ~ 40sccm, in regulation breather valve control sputtering chamber
Operating air pressure sputtered between 0.1 ~ 2Pa；
7）The LiFePO4 or LiFePO for having Nanometer Copper will be sputtered4/ C positive plate, which is placed in 80 ~ 100 DEG C of vacuum drying chambers, dries 8
~ 12 hours, obtain described utilization magnetron sputtering and deposit the iron phosphate lithium positive pole piece of Nanometer Copper on iron phosphate lithium positive pole surface.
2. a kind of utilization magnetron sputtering technique according to claim 1 deposits the side of Nanometer Copper on iron phosphate lithium positive pole surface
Method, it is characterised in that described calcining in two steps, be specially：
The first step：Calcining heat is 350 ~ 400 DEG C, and calcination time is 3 ~ 6 hours, and the heating rate of sintering temperature is raised to from room temperature
For 3 ~ 5 DEG C per minute, first step sintering is down to room temperature under protection atmosphere after finishing together with stove, obtains the fluffy phosphorus of black
Sour iron lithium block；LiFePO4 block be placed in agate mortar grind 30 ~ 60 minutes after, be pressed into button shape, pressure size is
10Mpa~20Mpa；
Second step：Calcining heat is 650 ~ 750 DEG C, and calcination time is 10 ~ 12 hours, and the heating speed of sintering temperature is raised to from room temperature
Rate is 3 ~ 5 DEG C per minute, and sintering is down to room temperature under protection atmosphere after finishing together with stove.
3. a kind of utilization magnetron sputtering technique according to claim 1 deposits the side of Nanometer Copper on iron phosphate lithium positive pole surface
Method, it is characterised in that the coating, iron phosphate lithium positive pole piece phosphoric acid iron lithium or LiFePO every square centimeter during coating4/C 3.0
~ 6.0 milligrams.
4. a kind of utilization magnetron sputtering technique according to claim 1 deposits the side of Nanometer Copper on iron phosphate lithium positive pole surface
Method, it is characterised in that described sputtering, sets operating power between 60 ~ 80W, and the operating distance of target and sputtering substrate is 10
~ 15cm, the Nanometer Copper plastics thickness control after sputtering is between 5 nanometers ~ 20 nanometers.
5. a kind of utilization magnetron sputtering technique according to claim 1 deposits the side of Nanometer Copper on iron phosphate lithium positive pole surface
Method, it is characterised in that the drying, its process be heated up again after predrying 3 ~ 6 hours in 60 DEG C of vacuum drying chamber as
100 ~ 110 DEG C of dryings 12 ~ 24 hours.
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| CN (1) | CN106981638A (en) |
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| CN108172813A (en) * | 2018-02-01 | 2018-06-15 | 广东工业大学 | A kind of composite positive pole and preparation method thereof |
| CN108539179A (en) * | 2018-04-28 | 2018-09-14 | 河南工业大学 | Phosphoric acid vanadium lithium combination electrode material and the preparation method and application thereof |
| CN108923019A (en) * | 2018-06-30 | 2018-11-30 | 宁波革创新材料科技有限公司 | The preparation method of anode material for lithium-ion batteries based on magnetically controlled sputter method |
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| CN108923019A (en) * | 2018-06-30 | 2018-11-30 | 宁波革创新材料科技有限公司 | The preparation method of anode material for lithium-ion batteries based on magnetically controlled sputter method |
| CN114094084A (en) * | 2021-11-24 | 2022-02-25 | 昆明理工大学 | Preparation method and application of metal oxalate-graphite composite electrode material |
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