CN103219504A - Silicon monoxide composite cathode material for lithium ion battery, and preparation method thereof - Google Patents
Silicon monoxide composite cathode material for lithium ion battery, and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon monoxide composite cathode material for a lithium ion battery, and a preparation method of the silicon monoxide composite cathode material, aiming at improving the cycle performance. The composite cathode material comprises the components by mass percent: 10-30% of composite particle material and 70-90% of natural graphite or artificial graphite, wherein the composite particle material is silicon monoxide covered by a carbon nano tube and an amorphous carbon coating layer. The method comprises the following steps of: forming the carbon nano tube and the amorphous carbon coating layer on the surface of silicon monoxide to obtain composite particles, and mixing the composite particles with the graphite. Compared with the prior art, the preparation method enables cracking carbon to be covered on the surfaces of silicon monoxide particles, so that the volume effect of the silicon monoxide particles can be effectively inhibited in the charge-discharge process of a battery, the cycle performance is good, the specific capacity is more than 500mAh/ g, and the capacity retention ratio is more than 85% after the circulation is carried out for 100 times; and the preparation method is simple in preparation technology, low in raw material cost and suitable for the cathode material for the high-capacity lithium ion battery.
Description
Technical field
The present invention relates to a kind of battery material and preparation method thereof, particularly a kind of lithium ion battery cathode material and its preparation method.
Background technology
In short supply day by day along with traditional energy materials such as global coal, oil, people just are being devoted to develop the new forms of energy that can replace traditional fossil energy, and advantage such as lithium ion battery is because of having that voltage height, energy density are big, memory-less effect, life-span length, green non-pollution, self discharge are little, and become the first-selected power supply unit of various portable type electronic products.
Lithium ion battery negative material is based on carbon-based material at present, and comprising native graphite and Delanium, but its lower theoretical capacity (372mAh/g) has no longer adapted to the demand for development of lithium ion battery to high power capacity, small size.Therefore, people press for a kind of high capacity type lithium ion battery negative material that can substitute graphite material of exploitation.In many alternative materials, silicon materials become a kind of material that has potentiality that substitutes native graphite and Delanium because of having than height ratio capacity (theoretical value is 4200mAh/g).Yet there is huge change in volume in the pure silicon material in battery charge and discharge process, the pole piece efflorescence that this huge change in volume causes preparing, comes off, and causes separating of electrode active material and collector, thereby has had a strong impact on the cycle performance of battery.The silicon monoxide material, though its theoretical specific capacity is littler than pure silicon material, its bulk effect in battery charge and discharge process is less relatively, therefore, the easier breakthrough restriction of silicon monoxide material realizes industrialization early.
In the prior art, Chinese patent application number inferior silicon composite cathode material of 201110275091.6 disclosed a kind of lithium ion battery oxidations and preparation method thereof, this material preparation may further comprise the steps: (1) generates silicon nanoparticle and amorphous silica with the inferior silicon of oxidation high temperature sintering under inert atmosphere; (2) accurately take by weighing inferior silicon of a certain amount of oxidation behind sintering and conductive agent, add in the planetary ball mill, mixing and ball milling promptly obtains the inferior silicon composite cathode material of oxidation.Chinese patent application number 201110333476.3 disclosed a kind of lithium ion battery cathode material and its preparation methods, this lithium ion battery negative material is mixed by the inferior silicon grain of oxidation, graphite granule, expanded graphite particles, the inferior silicon grain of oxidation, graphite granule, expanded graphite particles are coated by carbon, its preparation method comprises the steps: that (1) takes by weighing an amount of oxidation Asia silicon, graphite, expanded graphite and puts into planetary ball mill, under vacuum or inert atmosphere, grind and mix, obtain elementary composite material; (2) take by weighing an amount of carbon source precursor and put into above-mentioned planetary ball mill, under vacuum or inert atmosphere, grind and mix, obtain secondary composite material with elementary composite material with elementary composite material; (3) take out secondary composite material, sintering under inert atmosphere, and make the carbonization of carbon source precursor, promptly obtain lithium ion battery negative material.The prepared silicon monoxide negative material of above-mentioned art methods is generally pursued high power capacity, and generally at 1000mAh/g, but cycle performance is all relatively poor, and the 100 all capability retentions that circulate realize that only for original 50%～60% industrialization still has big difficulty.
Summary of the invention
The purpose of this invention is to provide a kind of lithium ion battery silicon monoxide composite negative pole material and preparation method thereof, the technical problem that solve is to improve the cycle performance of height ratio capacity silicon monoxide negative material.
The present invention compared with prior art, by evenly coating one deck cracking carbon at nanometer silicon monoxide particle surface, suppress the bulk effect that the silicon monoxide particle occurs effectively in battery charge and discharge process, improve the stable circulation performance, specific capacity is greater than 500mAh/g, and 100 capability retentions that circulate are more than 85%, and preparation technology is simple, cost of material is cheap, is applicable to the lithium ion battery negative material of high capacity type.
Description of drawings
Fig. 1 is the SEM photo of the silicon monoxide raw material of the embodiment of the invention 1.
Fig. 2 is the SEM photo () of the composite particulate material of the embodiment of the invention 1.
Fig. 3 is the SEM photo (two) of the composite particulate material of the embodiment of the invention 1.
Fig. 4 is the section SEM photo of the composite particulate material of the embodiment of the invention 1.
Fig. 5 is the XRD figure of the composite particulate material of the embodiment of the invention 1.
Fig. 6 is the charging and discharging curve figure of the lithium ion battery of the embodiment of the invention 1 with the silicon monoxide composite negative pole material.
Fig. 7 is the charging and discharging curve figure of the lithium ion battery of the embodiment of the invention 2 with the silicon monoxide composite negative pole material.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.Lithium ion battery of the present invention silicon monoxide composite negative pole material, by mass percentage, mix with 70～90% native graphites or Delanium by 10%～30% composite particulate material and to form, composite particulate material is the silicon monoxide that is coated with carbon nano-tube and agraphitic carbon coating layer, the granularity of silicon monoxide is 60～120nm, the thickness of coating layer is 2～5 μ m, the phosphorus content of native graphite or Delanium 〉=99%.
Carbon nano-tube is the cracking carbon of short-term shape structure, agraphitic carbon be block and or the cracking carbon of layer structure,
The lithium ion battery of the present invention preparation method of silicon monoxide composite negative pole material may further comprise the steps:
One, by mass percentage, catalyst precursor with 4～20% and 80～96% silicon monoxide mix by prior art and to be scattered in the organic solvent, obtain slurry; Organic solvent is 100ml:2～15g with the volume mass ratio of powder body material, and speed of agitator is 800～1500r/m, and jitter time is 2～5h.
The catalyst precursor is more than one in nickel acetate, nickel nitrate and the nickel chloride.
Organic solvent is more than one in acetone, ethanol and the oxolane.
The granularity of silicon monoxide is 60～120nm.
Two, adopt spray dryer that slurry is carried out spray drying, obtain the mixed powder material, inlet temperature is 150～200 ℃, and outlet temperature is 75～120 ℃, and the atomizing frequency is 15000～20000Hz, makes mass water content≤0.1% of mixed powder material.
Three, with the pulverizer of prior art the mixed powder material is pulverized, obtained the compound that particle diameter is 20～30 μ m.
Four, compound is heat-treated, programming rate is 1～5 ℃/min, and heat treatment temperature is 400～600 ℃, and heat treatment time is 1～4h, naturally cools to room temperature in the stove.
Five, being crushed to granularity is 15～25 μ m, obtains pulverizing material.
Six, will pulverize material and put into chemical vapour deposition (CVD) CVD stove; feed protective gas nitrogen or argon gas; flow is 0.5～1.5L/min; programming rate with 1～5 ℃/min; to 600～700 ℃ of depositing temperatures; feed carbon-source gas acetylene or liquefied petroleum gas (liquefied gas); flow is 2～3.5L/min; time 1～3h forms carbon nano-tube and agraphitic carbon coating layer to the silicon monoxide surface, and the thickness of coating layer is 2～5 μ m; stop to feed carbon-source gas; be cooled to room temperature in the stove, stop to feed protective gas, obtain composite particles.
Seven, composite particles is pulverized by prior art, obtained the composite material granular that particle diameter is 15～30 μ m.
Eight, adopt the mixer such as the general VC mixer of prior art, by mass percentage, 10%～30% composite material granular is mixed rotating speed 800～1300r/min with 70～90% graphite, time 1～3h obtains lithium ion battery silicon monoxide composite negative pole material.
Graphite is phosphorus content 〉=99%, and particle diameter is 5～15 μ m, and specific area is 5～10m
2The native graphite of/g or Delanium.
With the lithium ion battery silicon monoxide composite negative pole material that the inventive method prepares, adopt FDAC S4800 type ESEM to analyze and observe.Adopt Dutch Panalytical X'Pert PRO X-ray diffractometer analyzing crystal structure, lattice parameter, graphite monochromator, (λ=0.15406nm), sweep speed is 10 °/min to the Cu target, and sweep limits is 10～90 °.
Use the silicon monoxide composite negative pole material as negative active core-shell material the lithium ion battery that embodiment 1～10 prepares, G makes 2016 simulated batteries by the GB/T24533-2009 appendix.The LAND(indigo plant that adopts Wuhan Jin Nuo Electronics Co., Ltd. to produce) electrical property of battery test system test simulation battery.The test voltage scope of simulated battery is 0.01V～1.5V, and charge-discharge magnification is 0.2C.
Prescription, the technological parameter of embodiment 1～10 see Table 1, and electric performance test sees Table 2.
Comparative Examples 1 adopts single silica material as negative active core-shell material, makes simulated battery as stated above.The test of employing same procedure, electric performance test sees Table 2.
Comparative Examples 2, by mass percentage, coat 85% silicon monoxide with 15% pitch cracking carbon after, more by mass percentage, 20% above-mentioned clad material is mixed with 80% graphite, as negative active core-shell material, make simulated battery as stated above.The test of employing same procedure, electric performance test sees Table 2.
As shown in Figure 1, the raw material silicon monoxide powder granularity of embodiment 1 employing is 60～120nm.
As shown in Figures 2 and 3, the cracking carbon that silicon monoxide is produced in the CVD process coats, and this cracking carbon is amorphous or fibrous pattern, and this composite particulate material granularity is 15～30 μ m.
As shown in Figure 4, the post-depositional composite particulate material of CVD is carried out the test of section Electronic Speculum, and test result shows that this composite particulate material is made up of silicon monoxide kernel and coating layer, this coating layer promptly is the cracking carbon coating layer that forms in the CVD process, and the thickness of this coating layer is 2～5 μ m.
As shown in Figure 5,26.5 degree are the strong peak of graphite diffraction, and silicon monoxide is an amorphous substance, therefore can only see the diffraction maximum of native graphite in the drawings.
As shown in Figure 6, silicon monoxide content 15% sample specific capacity is brought into play greater than 500mAh/g, and the 100 all capability retentions that circulate illustrate that greater than 92% lithium ion battery of the present invention has good stable circulation performance with the silicon monoxide composite negative pole material.
As shown in Figure 7, silicone content 12% sample specific capacity is greater than 460mAh/g, and the 100 all capability retentions that circulate illustrate that greater than 95% lithium ion battery of the present invention has good stable circulation performance with the silicon monoxide composite negative pole material.
Lithium ion battery of the present invention silicon monoxide composite negative pole material, at nanometer silicon monoxide particle surface chemical deposition carbon, coat amorphous or fibrous (the short-term shape of formation on the silicon monoxide surface, bulk and stratiform) the cracking carbon-coating of structure, this cracking carbon-coating has favorable mechanical cushioning effect and good electrical conductivity, the bulk effect that can effectively suppress silicon monoxide, thereby effectively suppressed the bulk effect that the silicon monoxide particle occurs in battery charge and discharge process, so it has better cycle performance, higher specific capacity, have application promise in clinical practice in the lithium ion battery field, technology is simple, easily control, cost is low, is fit to suitability for industrialized production.The prescription of table 1 embodiment 1～10, technology
The electric performance test of table 2 embodiment 1～10 and Comparative Examples
| Embodiment or Comparative Examples | |
100 all capability retention % circulate |
| Embodiment 1 | 500mAh/g | 92.3% |
| Embodiment 2 | 468mAh/g | 95.6% |
| Embodiment 3 | 550mAh/g | 90.4% |
| Embodiment 4 | 450mAh/g | 96.2% |
| Embodiment 5 | 451mAh/g | 96.0% |
| Embodiment 6 | 500mAh/g | 93.0% |
| Embodiment 7 | 461mAh/g | 94.7% |
| Embodiment 8 | 455mAh/g | 95.4% |
| Embodiment 9 | 470mAh/g | 94.6% |
| |
443mAh/g | 95.2% |
| Comparative Examples 1 | 1175mAh/g | 41.6%(10 week circulation) |
| Comparative Examples 2 | 850mAh/g | 57.3%(10 week circulation) |
Claims (10)
1. lithium ion battery silicon monoxide composite negative pole material, it is characterized in that: described lithium ion battery with the silicon monoxide composite negative pole material by mass percentage, mix with 70～90% native graphites or Delanium by 10%～30% composite particulate material and to form, composite particulate material is the silicon monoxide that is coated with carbon nano-tube and agraphitic carbon, the thickness of coating layer is 2～5 μ m, the phosphorus content of native graphite or Delanium 〉=99%.
2. lithium ion battery silicon monoxide composite negative pole material according to claim 1 is characterized in that: described carbon nano-tube is the cracking carbon of short-term shape; Described agraphitic carbon is block and or the cracking carbon of layer structure.
3. according to the described lithium ion battery of claim 1 silicon monoxide composite negative pole material, it is characterized in that: the granularity of described native graphite or Delanium is 5～15 μ m, and specific area is 5～10m
2/ g.
4. a lithium ion battery may further comprise the steps with the preparation method of silicon monoxide composite negative pole material:
One, silicon monoxide is put into chemical vapor deposition stove, feed protective gas, programming rate with 1～5 ℃/min, to 600～700 ℃ of depositing temperatures, feed carbon-source gas, form carbon nano-tube and agraphitic carbon coating layer to the silicon monoxide surface, stop to feed carbon-source gas, be cooled to room temperature in the stove, stop to feed protective gas, obtain composite particles;
Two, composite particles is pulverized, obtained composite material granular;
Three, by mass percentage, 10%～30% composite material granular is mixed with 70～90% graphite, rotating speed is 800～1300r/min, and incorporation time is 1～3h, obtains lithium ion battery silicon monoxide composite negative pole material.
5. preparation method according to claim 4 is characterized in that: protective gas is nitrogen or argon gas in the described step 1, and flow is 0.5～1.5L/min, and carbon-source gas is acetylene or liquefied petroleum gas, and flow is 2～3.5L/min.
6. preparation method according to claim 4 is characterized in that: the particle diameter of pulverizing the back composite material granular in the step 2 is 15～30 μ m.
7. preparation method according to claim 4 is characterized in that: described silicon monoxide is put into chemical vapor deposition stove before, handle according to the following steps:
One, by mass percentage, catalyst precursor with 20～4% and 80～96% silicon monoxide are scattered in the organic solvent, obtain slurry; Organic solvent is 100ml:2～15g, dispersed with stirring rotating speed 800～1500r/m, jitter time 2～5h with the volume mass ratio of powder body material;
Two, slurry is carried out spray drying, obtain the mixed powder material; The inlet temperature of described spray dryer is 150～200 ℃, and outlet temperature is 75～120 ℃, and the atomizing frequency is 15000～20000rpm;
Three, the mixed powder material is pulverized, obtained the compound that particle diameter is 20～30 μ m;
Four, compound is heat-treated, programming rate is 1～5 ℃/min, and heat treatment temperature is 400～600 ℃, and heat treatment time is 1～4h, naturally cools to room temperature in the stove;
Five, being crushed to granularity is 15～25 μ m, obtains pulverizing material.
8. preparation method according to claim 7 is characterized in that: the granularity of silicon monoxide is 60～120nm in the described step 1.
9. preparation method according to claim 7 is characterized in that: described catalyst precursor is more than one in nickel acetate, nickel nitrate and the nickel chloride; Described organic solvent is more than one in acetone, ethanol and the oxolane.
10. preparation method according to claim 7 is characterized in that: mass water content≤0.1% that obtains the mixed powder material in the described step 2.
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| CN104022257A (en) * | 2014-06-16 | 2014-09-03 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon dioxide composite anode material for lithium ion battery, as well as preparation method and application of silicon dioxide composite anode material |
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