CN108878823A - A kind of preparation method of metal olivine cladding nano-silicon - Google Patents
A kind of preparation method of metal olivine cladding nano-silicon Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of metal olivine cladding nano-silicon.This method comprises the following steps：1) under conditions of oxygen content is lower than 1000ppm, by metal oxide powder and SiOxPowder is uniformly mixed, and obtains mixture；2) starvation calcines mixture, obtains compound；3) compound is carried out ball milling by starvation, obtains metal olivine cladding nano-silicon.Preparation method of the invention is simple, easily operated and control, and organic solvent used in simultaneously synthesizing process is seldom; be conducive to protect environment, and cladding raw material is cheap, favorably there is saving cost; it is suitble to industrialization large-scale production, there is chemical property outstanding in silicium cathode material.
Description
Technical field
The present invention relates to field of nanometer material technology, and in particular to a kind of preparation method of metal olivine cladding nano-silicon.
Background technique
There is operating voltage height, ratio as the lithium ion battery of positive electrode using cobalt acid lithium, LiFePO4, nickel cobalt manganese etc.
Energy is big, pollution-free, light-weight, small in size, memory-less effect, can be quickly charged and discharged with the service life it is long the advantages that, be widely used in
The portable electronic products such as mobile phone, while becoming 21 century also by large-scale application on electric vehicle and hybrid electric vehicle
Most there is one of the energy storage device of application value.
Currently, carbon negative pole material it is conductive it is good, intercalation potential is low, cycle performance is excellent, resourceful, price is low
The advantages that honest and clean, nontoxic and pollution-free is comparatively ideal lithium ion battery negative material.However, the carbon negative pole material being widely used is deposited
Specific capacity low (theoretical capacity 372mAh/g) the problem of.It is not able to satisfy the demand for development of high capacity, high power secondary battery,
The promotion of lithium battery performance is restrict, thus develops novel cell negative electrode material to become one of current important research direction.
Silicon has biggish lithium storage content (4200mAh/g), and the rich content in the earth is the ideal of lithium ion battery
Negative electrode material, but, silicon materials can generate huge volume change (300%) during lithium ion embedding de- lithium, so that negative
Structure broken, dusting in cyclic process in pole causes the forfeiture of removal lithium embedded ability, and negative electrode material falls off from collector and caused
Collect the deterioration of properties of flow.Meanwhile the SEI film that volume expansion also causes surface to be formed is very unstable, leads to lower coulombic efficiency.
To constrain application of the silicon as negative electrode material.
Currently, improving the method for silicon materials stable circulation performance has very much, such as：Using nano-silicon as negative electrode material, when
Silicon particle size be less than 150nm after, Volumetric expansion begins to reduce, thus nano-silicon as active material initial
Preferable chemical property can be shown in circulation, but as the cycle progresses, agglomeration can occur for nano-silicon, thus
Capacity attenuation is very fast during following cycle.And it is expensive as negative electrode material directly to prepare nano-silicon, large-scale commercial applications
A possibility that change, is also little, and CN106784762A provides the preparation method and applications of a kind of nanometer of silicon array negative electrode material,
Although nanometer silicon array alleviates volume expansion to a certain extent, cyclical stability is improved, the method step is various, it is difficult to
Scale application.
In addition, the coating modification for silicon materials is also more universal, CN106784763A discloses a kind of porous oxide
It is living to control silica-base material surface by being passivated processing to silicon substrate pole material surface for the preparation method for wrapping up battery silicium cathode
Property species number, recycle gas phase technique for atomic layer deposition to silica-base material surface carry out different-thickness nanoporous grade oxygen
The package of compound, CN106159215A disclose a kind of silicium cathode material and preparation method thereof and including the silicium cathode materials
Cathode and lithium ion battery carry out two layers of carbon coating to 1~100 μm of silicon powder using liquid phase method, and CN107845800A is then using splashing
It penetrates deposition technique and nano silicon nitride tin cladding is carried out to the silicon base of load silicon array, although the silicon materials after above-mentioned cladding are certain
The chemical property of battery is improved in degree, but the method for coating being related to is extremely complex, and wherein there are also using graphene or
It is nitride as clad, cost is very high, and condition requirement is also harsher, in addition, the gas phase atomic layer deposition being related to
Technology and sputter-deposition technology are only limited to laboratory preparation at present, thus, it is unfavorable for industrialization large-scale production.
How using the modified silica-base material of the synthetic method being simple and efficient, to effectively improve using silica-base material as cathode
The chemical property of lithium ion battery, further to develop silicon based anode material and realizing large-scale industrial production with important
Realistic meaning.
Summary of the invention
It is an object of the invention to a kind of preparation methods of metal olivine cladding nano-silicon.The preparation method is simple, easily
In operation and control, raw material is cheap, favorably there is saving cost, is suitble to industrialization large-scale production.
The technical solution adopted by the present invention is that：
A kind of preparation method of metal olivine cladding nano-silicon, includes the following steps：
1) under conditions of oxygen content is lower than 1000ppm, by metal oxide powder and SiOxPowder is uniformly mixed, and is obtained
Mixture；
2) starvation calcines mixture, obtains compound；
3) compound is carried out ball milling by starvation, obtains metal olivine cladding nano-silicon；
Wherein, 0.2≤x≤1.5.Preferably, 0.8≤x≤1.2.
Preferably, the metal oxide powder and SiO in step 1)xThe mass ratio of powder is (0.1~10)：1.
Preferably, the metal oxide powder and SiO in step 1)xThe mass ratio of powder is (0.5~4)：1.
It is highly preferred that metal oxide powder and SiO in step 1)xThe mass ratio of powder is (0.5~2.5)：1.
Wherein, excessive metal oxide can reduce the volumetric properties of material, less metal oxide to product for the first time
The raising of coulombic efficiency is unobvious.
Preferably, the partial size D50 of metal oxide powder is 0.02~20 μm in step 1).
Preferably, the partial size D50 of metal oxide powder is 0.1~10 μm in step 1).
It is highly preferred that the partial size D50 of metal oxide powder is 1~5 μm in step 1).
Preferably, SiO in step 1)xThe partial size D50 of powder is 0.1~20 μm.
Preferably, SiO in step 1)xThe partial size D50 of powder is 0.5~10 μm.
It is highly preferred that SiO in step 1)xThe partial size D50 of powder is 1~8 μm.
Too small metal oxide and SiOxThe partial size of powder will increase cost, and will increase SiOxExposure is in air by oxygen
The risk of change, and partial size is excessive, improves the subsequent energy consumption that technique is sanded, and is unfavorable for material and comes into full contact with mixing.
Preferably, in step 1) metal oxide in magnesia, calcium oxide, lithia, iron oxide, aluminium oxide extremely
Few one kind.
Preferably, in step 1) mixture partial size D50≤150nm.
Sufficiently small mixture partial size facilitates being sufficiently mixed between different raw material.
Preferably, the metal olivine clad to form crystal structure is fired in step 2).
It wherein, is the calcining effect for reaching step 2), calcination condition can be：700~1400 DEG C of calcination temperature, calcining
Time is 0.2~10h, it is highly preferred that calcination condition can be：900~1400 DEG C of calcination temperature, calcination time is 0.5~6h.
Preferably, the rotational speed of ball-mill in step 3) is 400~450r/min, and Ball-milling Time is 8~16h.
Preferably, the partial size D50 of the resulting metal olivine cladding nano-silicon of step 3) is 50~200nm.
It is highly preferred that the partial size D50 of the resulting metal olivine cladding nano-silicon of step 3) is 80~180nm.
Sufficiently small particle improves stability of the material in circulating battery.
Wherein, above-mentioned nano-silicon is the nano-silicon of crystal structure, and D50 is indicated：Partial size is greater than its particle and accounts for 50%, small
Particle in it also accounts for 50%, is expressed as average grain diameter；D90 is expressed as partial size and accounts for 90% less than its particle.
The beneficial effects of the invention are as follows：
1, by being coated with metal olivine clad as main component in nanometer silicon face, nano-silicon has been effectively relieved
Volume expansion problem be conducive to improve its cyclical stability in charge and discharge process when it is as silicium cathode material, protect
The stability and high efficiency for having demonstrate,proved its chemical property plays.
2, preparation method of the invention is simple, easily operated and control, and organic solvent used in simultaneously synthesizing process is very
It is few, be conducive to protect environment, and cladding raw material is cheap, favorably there is saving cost, is suitble to industrialization large-scale production.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of material prepared by the embodiment of the present invention 1；
Fig. 2 is the first charge-discharge curve graph of the material of comparative example preparation of the present invention；
Fig. 3 is the first charge-discharge curve graph of material prepared by the embodiment of the present invention 1.
Specific embodiment
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art are according to the present invention
Some nonessential modifications and adaptations that the principle of elaboration is made all belong to the scope of protection of the present invention.Following specific works of example
Skill parameter etc. is also only an example in OK range, i.e. those skilled in the art can do suitable model by the explanation of this paper
Interior selection is enclosed, and does not really want to be defined in hereafter exemplary specific data.
Embodiment 1
A kind of preparation method of the nano-silicon of metal olivine cladding, includes the following steps：
1) under nitrogen or argon gas protection, by the light magnesium oxide powder and partial size of the partial size D50 purity 99% for being 2 μm
D50 is that 5 μm oxidation Asia silicon (SiO) powder is 3 in mass ratio：2 weigh, and are put into ball grinder after mixing, and are added anhydrous
Ethyl alcohol makes solution solid content reach 30%, and the ball milling 20h in high energy ball mill, rotational speed of ball-mill 450r/min, after in 100~
It is heated in 150 DEG C of vacuum ovens, removes dehydrated alcohol, obtain the mixture that D50 is 150nm；
2) mixture is placed in tube furnace and is warming up to 1150 DEG C with the rate of 5 DEG C/min, 2h is calcined in nitrogen atmosphere,
Obtain the compound of silicon forsterite cladding；
3) the resulting compound of step 2) is mixed with dehydrated alcohol, the solution that solid content is 30% is obtained, in nitrogen atmosphere
Lower high-energy ball milling 12h is enclosed, rotational speed of ball-mill is set as 450r/min, obtains receiving for the silicon magnesia olivine cladding that partial size D50 is 150nm
Rice silicon.
Embodiment 2~7
For operating procedure with embodiment 1, raw material and reaction condition setting see the table below 1, table 1 it is unmentioned then with embodiment 1 one
It causes：
Table 1
Comparative example
A kind of preparation method of nano silicon material, includes the following steps：
1) 5kg is weighed, the amorphous silicon that partial size D50 is 5 μm is added after 17kg dehydrated alcohol in high energy ball mill ball milling
20h, rotational speed of ball-mill 450r/min, after heated in 100~150 DEG C of vacuum ovens, remove dehydrated alcohol, obtain partial size
D50 is the unformed silicon of 150nm；
2) the unformed silicon for obtaining step 1), which is placed in tube furnace, is warming up to 1150 DEG C with the rate of 5 DEG C/min, in nitrogen
2h is calcined in gas atmosphere；
3) the resulting substance of step 2) is mixed with dehydrated alcohol, the solution that solid content is 30% is obtained, in nitrogen atmosphere
Lower high-energy ball milling 12h, rotational speed of ball-mill are set as 450r/min, obtain the nano silicon material that partial size D50 is 150nm.
1, morphology characterization：
Fig. 1 is the scanning electron microscope (SEM) photograph of material prepared by the embodiment of the present invention 1.As seen from Figure 1, the material of the application preparation
Expect that the particle size of the patch unit is different, and partial size is about by the layer structure of the flat crystal element stack of compound with regular structure
50~200nm.
2, electric performance test：
Respectively using embodiment 1 and comparative example as positive electrode, lithium metal is cathode, makes half-cell test material performance,
PVDF is binder, and active carbon is conductive agent, and the mass percent of three is 50：30：20, using NMP as solvent, done by stirring
At slurry, slurry is uniformly coated on aluminium foil using coating machine, positive plate is made after drying, electrolyte is 1M LiPF6It is dissolved in
EC/DMC(1：1, v/v), using lithium metal as cathode, it is assembled into CR2016 battery respectively in the glove box full of argon gas,
In the voltage range of 0.01~3V, constant current charge-discharge test is carried out to battery with the current density of 150mA/g, test result is shown in
Fig. 2 and Fig. 3.
From Fig. 2 and Fig. 3：The chemical property of embodiment and comparative example has huge difference, and comparative example is for the first time
Specific discharge capacity is only 700mAh/g or so, and the first discharge specific capacity of embodiment is 1700mAh/g or so, is comparative example
2.43 times, specific capacity when comparative example charges to 2V is only 260mAh/g, and the specific capacity of embodiment is 1290mAh/g or so,
About 5 times of comparative example, this illustrates that the nano silicon material of the metal olivine cladding of the application preparation is received compared to common
Rice silicon materials have superior chemical property.
Claims (10)
1. a kind of preparation method of metal olivine cladding nano-silicon, it is characterised in that：Include the following steps：
1) under conditions of oxygen content is lower than 1000ppm, by metal oxide powder and SiOxPowder is uniformly mixed, and must be mixed
Object；
2) starvation calcines mixture, obtains compound；
3) compound is carried out ball milling by starvation, obtains metal olivine cladding nano-silicon；
Wherein, 0.2≤x≤1.5.
2. preparation method according to claim 1, it is characterised in that：Metal oxide powder and SiO in step 1)xPowder
The mass ratio at end is (0.1~10)：1.
3. preparation method according to claim 2, it is characterised in that：Metal oxide powder and SiO in step 1)xPowder
The mass ratio at end is (0.5~4)：1.
4. preparation method according to claim 1, it is characterised in that：The partial size D50 of metal oxide powder in step 1)
It is 0.02~20 μm.
5. preparation method according to claim 1, it is characterised in that：SiO in step 1)xThe partial size D50 of powder be 0.1~
20μm。
6. preparation method according to claim 5, it is characterised in that：SiO in step 1)xThe partial size D50 of powder be 0.5~
10μm。
7. preparation method according to claim 1, it is characterised in that：Metal oxide is selected from magnesia, oxygen in step 1)
Change at least one of calcium, lithia, iron oxide, aluminium oxide.
8. preparation method according to claim 1, it is characterised in that：Partial size D50≤150nm of mixture in step 1).
9. preparation method according to claim 1, it is characterised in that：Step 2) is fired to the metal olive to form crystal structure
Olive stone clad.
10. preparation method according to claim 1, it is characterised in that：The resulting metal olivine of step 3) coats nanometer
The partial size D50 of silicon is 50~200nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111900368A (en) * | 2020-07-24 | 2020-11-06 | 陕西煤业化工技术研究院有限责任公司 | Lithium ion battery-grade silicon monoxide negative electrode material, and preparation method and application thereof |
| CN114927675A (en) * | 2022-06-30 | 2022-08-19 | 宜春瑞富特新能源材料技术有限公司 | Composite metal-coated silicon carbide-based negative electrode material and preparation method and application thereof |
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| CN111900368A (en) * | 2020-07-24 | 2020-11-06 | 陕西煤业化工技术研究院有限责任公司 | Lithium ion battery-grade silicon monoxide negative electrode material, and preparation method and application thereof |
| CN114927675A (en) * | 2022-06-30 | 2022-08-19 | 宜春瑞富特新能源材料技术有限公司 | Composite metal-coated silicon carbide-based negative electrode material and preparation method and application thereof |
| CN114927675B (en) * | 2022-06-30 | 2024-06-07 | 宜春瑞富特新能源材料技术有限公司 | Composite metal coated silicon carbide-based negative electrode material and preparation method and application thereof |
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