CN107195896A - A kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle - Google Patents
A kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle, it is characterised in that:Using conducting metal nano particle as carrier, organosilicon hydrolyzation deposition silica, then mix with metal, low melting point salt, thermal reduction, coated polymer, washing and drying, acquisition silicium cathode material;Conducting metal nano particle is Nanometer Copper, Nano Silver, Nanoscale Iron, nanometer bismuth, nanometer tin, nano nickel, nanometer cobalt, nanometer indium, the one or more of nano-titanium;Reducing metal is the one or more in the alloy of lithium, potassium, calcium, rubidium, sodium, strontium, barium, lanthanum and above-mentioned metal;Low melting point salt is the one or more in gallium, germanium, tin, aluminium, the villaumite of magnesium, bromide and villiaumite;Polymer is the one or more in the derivative of polyaniline, polypyrrole, polythiophene and above-mentioned polymer;The mol ratio (1~5) of silicon and conducting metal: 1;Silicon:Reducing metal:The mol ratio of low melting point salt is 1: (2~5): (1~20);The mol ratio of silicon and polymer precursor is (5~30): 1.The negative material has good chemical property, has good application prospect in field of lithium ion battery.
Description
Technical field
The invention belongs to field of lithium ion battery material, and in particular to one kind is using conducting metal nano particle as carrier low temperature
Synthesize the preparation method of silicium cathode material.
Background technology
The advantages of elemental silicon has storage lithium energy density height (theoretical capacity is up to 3580mA h/g), rich reserves, right and wrong
Often there is the lithium ion battery negative material of application prospect.But Volume Changes are big during silicon has simple substance poorly conductive, removal lithium embedded
Etc. defect, cause silicon can not extensive use because of chemical property difference.At present, scientific research personnel uses nano material, loose structure
Alleviate alleviations Volume Changes, the conduction of increase silicon materials of the silicon in charge and discharge process with the method such as the carbon for being introduced into high conductivity
Property, so as to improve the cycle performance of silicon materials.But nanosizing and loose structure result in the reduction of material volume specific energy density, and
Its preparation method is generally complicated, and cost is high, limits its commercial applications.
SiOx materials are a kind of silicium cathode materials of better performances, are also a kind of current most widely used silicon materials.Reason
Found by research, Li is embedded into SiOx, can form multiple compounds, these lithium silicon compounds turn into Si negative electrode volume expansions
Buffer strip, suppresses the volumetric expansion of silicium cathode, so as to improve the cycle performance of SiOx materials.Patent 1 (CN105789577A,
A kind of preparation method of lithium ion battery silicium cathode material and the silicium cathode material) to aoxidize sub- silicon as raw material, hydroxylating, mixed
Close graphite, high-temperature calcination and obtain silicium cathode material, effectively increase the chemical property of silicium cathode material.Patent 2
(CN105406050A, one kind meets silicium cathode material, preparation method and purposes), using nano-silicon as raw material, passes through high temperature coated Si
Oxide and metal composite layer, again high temperature coated with conductive carbon-coating;The silicium cathode material capacity is higher than 1500mAh/g, 300 circulations
Capacity is maintained at more than 90% afterwards.
Obviously, the electrochemistry capacitance and cycle performance for improving SiOx are the passes for realizing SiOx electrode material commercial applications
Key, current research also obtains gratifying achievement.But high-temperature calcination energy consumption is big and produces large quantity of exhaust gas pollution environment, virtually
Add the preparation cost of SiOx electrode materials.
The content of the invention
Present invention aims at provide a kind of system that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle
Preparation Method, overcomes the defect of existing technology of preparing, improves the chemical property of silicium cathode material.For achieving the above object,
The technical scheme is that:A kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle,
It is characterized in that:Using conducting metal nano particle as carrier, organosilicon hydrolyzation deposition silica, then with metal, low melting point salt
Mixing, thermal reduction, coated polymer, washing and drying obtain silicium cathode material;Conducting metal nano particle is Nanometer Copper, nanometer
Silver, Nanoscale Iron, nanometer bismuth, nanometer tin, nano nickel, nanometer cobalt, nanometer indium, the one or more of nano-titanium;Reducing metal be lithium,
One or more in potassium, calcium, rubidium, sodium, strontium, barium, the alloy of lanthanum and above-mentioned metal;Low melting point salt is gallium, germanium, tin, aluminium, magnesium
Villaumite, bromide and villiaumite in one or more;Polymer is polyaniline, polypyrrole, polythiophene and above-mentioned polymer
One or more in derivative;The mol ratio (1~5) of silicon and conducting metal: 1;Silicon: reducing metal: mole of low melting point salt
Than for 1: (2~5): (1~20);The mol ratio of silicon and polymer is (5~20): 1;One kind is using conducting metal nano particle as load
The preparation method of body hypothermia synthesis silicium cathode material includes:
1) conductive nano-particles for weighing certain mass are dispersed in aqueous solutions of organic solvent, add surfactant, are surpassed
1~20h of sound;
Wherein, one kind or several of aldehydes, carboxylic acids, alcohols and above-mentioned organic matter derivative that organic solvent is C1~C8
Kind;The volume ratio of organic matter and water is (0.1~10): 1;
2) ethanol solution of organosilicon is instilled into step 1) product, stir 1~40h;Temperature control is at 10~100 DEG C;
Wherein, organosilicon is the one or more of esters of silicon acis, silane, silicon chloride, silicon bromide and above-mentioned organic matter derivative;
3) by step 2) product separation, drying, mixed with metal and low melting point salt, be put into container, vacuumize, close,
2~40h is placed at 200~500 DEG C;
4) by step 3) product input hydrochloric acid solution, impregnate 5~60h;Separation, deionized water washing, drying;
5) by step 4) product input alcohol water blend, add a certain amount of polymeric precursor, at the uniform velocity stir 2~5h;
Then initiator is added, stirring, standing, filtering, vacuum drying obtain silicium cathode material.
Compared with other silicium cathode materials, patent of the present invention has the following advantages that:
1) silicium cathode material technology of the present invention is simple and convenient to operate, and is conducive to industrialized production.
2) silicium cathode material preparation condition of the present invention is gentle, and energy consumption is low.
3) present invention uses metal nanoparticle for carrier deposit Si oxide, improves the electric conductivity of silicon, network-like to lead
Electric polymer provides enough spaces for silicium cathode expansion, so silicium cathode material prepared by the present invention has good electrochemistry
Performance, 50mA electric currents, the charge/discharge capacity of material is more than 700mAh/g.
Embodiment
In order to further understand the content, features and effects of the present invention, it is as follows hereby to lift following examples detailed description:
Embodiment 1
A kind of composition design of silicium cathode material:
1) Nanometer Copper, 0.01mol;Tetraethyl orthosilicate, 0.02mol;Lithium metal, 0.04mol;Aluminium chloride, 0.04mol;Benzene
Amine, 0.002mol;
2) Nano Silver, 0.01mol;Silicon tetrachloride, 0.02mol;Magnesium metal, 0.04mol;Lithium chloride, 0.06mol;Pyrroles,
0.003mol;
3) nanometer tin, 0.01mol;Dichlorosilane, 0.02mol;Metallic aluminium, 0.04mol;Calcirm-fluoride, 0.06mol;Pyrroles,
0.003mol;
A kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle:
1) nano-metal particle for weighing certain mass is dispersed in ethanol water, adds Surfactant CTAB, is surpassed
Sound 5h;The volume ratio of ethanol and water is 9: 1;
2) ethanol solution of organosilicon is instilled into step 1) product, stir 10h;Temperature control is at 40 DEG C;
3) by step 2) product separation, drying, mixed with metal and low melting point salt, be put into container, vacuumize, close,
15h is placed at 250 DEG C;
4) by step 3) product input hydrochloric acid solution, impregnate 5h;Separation, deionized water washing, drying, obtain SiOx/
Nano metal negative material;
5) by step 4) product input alcohol water blend, add a certain amount of polymeric precursor, at the uniform velocity stir 2~5h;
Then initiator is added, stirring, standing, filtering, vacuum drying obtain silicium cathode material.
The silica-base material particle size is tiny, and loose structure is presented;During for negative electrode of lithium ion battery;After 100 circulations,
50mA discharge capacities are more than 700mAh/g.
Embodiment 2
A kind of composition design of silicium cathode material:
4) Nanometer Copper, 0.01mol;Silicon tetrachloride, 0.01mol;Lithium metal, 0.02mol;Aluminium chloride, 0.04mol;Aniline,
0.001mol;
5) Nanometer Copper, 0.01mol;Silicon tetrachloride, 0.03mol;Magnesium metal, 0.07mol;Lithium chloride, 0.06mol;Pyrroles,
0.002mol;
6) Nanometer Copper, 0.01mol;Silicon tetrachloride, 0.04mol;Metallic aluminium, 0.12mol;Magnesium bromide, 0.06mol;Aniline,
0.0015mol;
A kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle:
1) nano-metal particle for weighing certain mass is dispersed in ethanol water, adds Surfactant CTAB, is surpassed
Sound 10h;The volume ratio of ethanol and water is 5: 1;
2) ethanol solution of organosilicon is instilled into step 1) product, stir 5h;Temperature control is at 60 DEG C;
3) by step 2) product separation, drying, mixed with metal and low melting point salt, be put into container, vacuumize, close,
5h is placed at 300 DEG C;
4) by step 3) product input hydrochloric acid solution, impregnate 10h;Separation, deionized water washing, drying, obtain SiOx/
Nano metal negative material;
5) by step 4) product input alcohol water blend, add a certain amount of polymeric precursor, at the uniform velocity stir 2~5h;
Then initiator is added, stirring, standing, filtering, vacuum drying obtain silicium cathode material.
The silica-base material particle size is tiny, and loose structure is presented;During for negative electrode of lithium ion battery;After 100 circulations,
50mA discharge capacities are more than 700mAh/g.
Embodiment 3
Be the same as Example 1 operates
A kind of composition design of silicium cathode material:
7) Nanoscale Iron, 0.01mol;Silicon tetrachloride, 0.01mol;Lithium metal, 0.02mol;Aluminium chloride, 0.04mol;Aniline,
0.001mol;
8) nano-titanium, 0.01mol;Silicon tetrachloride, 0.03mol;Magnesium metal, 0.07mol;Lithium chloride, 0.06mol;Pyrroles,
0.001mol;
9) Nanometer Copper, 0.01mol;Silicon tetrachloride, 0.04mol;Metal rubidium, 0.12mol;Magnesium bromide, 0.06mol;Poly- pair
Chloroaniline, 0.001mol;
10) nano nickel, 0.01mol;Silicon tetrachloride, 0.01mol;Lithium metal, 0.02mol;Aluminium chloride, 0.04mol;Poly- neighbour
Methylaniline, 0.001mol;
11) nanometer cobalt, 0.01mol;Silicon tetrachloride, 0.03mol;Magnesium metal, 0.07mol;Lithium chloride, 0.06mol;Between poly-
5-trifluoromethylaniline, 0.002mol;
12) nanometer indium, 0.01mol;Silicon tetrachloride, 0.04mol;Lanthanoid metal, 0.12mol;Magnesium bromide, 0.06mol;It is poly-
(1- methylene -2- methyl naphthalenes)-N- pyrroles, 0.0015mol;
13) nanometer bismuth, 0.01mol;Silicon tetrachloride, 0.04mol;Metal rubidium, 0.12mol;Magnesium bromide, 0.06mol;Poly- 4-
(N- ethyls -1,8- naphthalimide) N- pyrroles,
The silica-base material particle size is tiny, and loose structure is presented;During for negative electrode of lithium ion battery;After 100 circulations,
50mA discharge capacities are more than 700mAh/g.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (1)
1. a kind of preparation method that silicium cathode material is synthesized by carrier low temperature of conducting metal nano particle, it is characterised in that:With
Conducting metal nano particle is carrier, organosilicon hydrolyzation deposition silica, then mix with metal, low melting point salt, thermal reduction, wrap
Polymer is covered, washing and drying obtains silicium cathode material;Conducting metal nano particle is Nanometer Copper, Nano Silver, Nanoscale Iron, nanometer
Bismuth, nanometer tin, nano nickel, nanometer cobalt, nanometer indium, the one or more of nano-titanium;Reducing metal be lithium, potassium, calcium, rubidium, sodium,
One or more in strontium, barium, the alloy of lanthanum and above-mentioned metal;Low melting point salt is gallium, germanium, tin, aluminium, the villaumite of magnesium, bromide
With the one or more in villiaumite;Polymer is one in the derivative of polyaniline, polypyrrole, polythiophene and above-mentioned polymer
Plant or a variety of;The mol ratio (1~5) of silicon and conducting metal: 1;Silicon: reducing metal: the mol ratio of low melting point salt is 1: (2~5):
(1~20);The mol ratio of silicon and polymer precursor is (5~30): 1;One kind is using conducting metal nano particle as carrier low temperature
The preparation method of synthesis silicium cathode material includes:
1) conductive nano-particles for weighing certain mass are dispersed in aqueous solutions of organic solvent, addition surfactant, and ultrasound 1~
20h;Wherein, the one or more of aldehydes, carboxylic acids, alcohols and above-mentioned organic matter derivative that organic solvent is C1~C8;Have
The volume ratio of machine thing and water is (0.1~10): 1;
2) ethanol solution of organosilicon is instilled into step 1) product, stir 1~40h;Temperature control is at 10~100 DEG C;Wherein,
Organosilicon is the one or more of esters of silicon acis, silane, silicon chloride, silicon bromide and above-mentioned organic matter derivative;
3) by step 2) product separation, drying, mixed with metal and low melting point salt, be put into container, vacuumize, close, 200
~500 DEG C of 2~40h of placement;
4) by step 3) product input hydrochloric acid solution, impregnate 5~60h;Separation, deionized water washing, drying;
5) by step 4) product input alcohol water blend, add a certain amount of polymeric precursor, at the uniform velocity stir 2~5h;Then
Initiator is added, stirring, standing, filtering, vacuum drying obtain silicium cathode material.
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CN108847478A (en) * | 2018-06-04 | 2018-11-20 | 安徽潜川动力锂电科技有限公司 | A kind of lithium battery silicon-carbon nano composite anode material and preparation method thereof |
CN109817925A (en) * | 2019-01-24 | 2019-05-28 | 广东凯金新能源科技股份有限公司 | Lithium ion secondary battery Si oxide composite negative pole material and preparation method |
CN109860507A (en) * | 2018-12-03 | 2019-06-07 | 中国计量大学 | A kind of foam conductive net/silica preparation facilities and control method |
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CN111952591B (en) * | 2018-05-04 | 2023-08-29 | 浙理氢能(杭州)科技有限公司 | Aerogel doped polythiophene battery additive and preparation method thereof |
CN108847478A (en) * | 2018-06-04 | 2018-11-20 | 安徽潜川动力锂电科技有限公司 | A kind of lithium battery silicon-carbon nano composite anode material and preparation method thereof |
CN111085186A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Regular carrier catalyst with desulfurization effect and preparation and application thereof |
CN111085197A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Regular carrier catalyst with desulfurization effect and preparation and application thereof |
CN111085256A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Regular carrier catalyst with desulfurization effect and preparation and application thereof |
CN109860507A (en) * | 2018-12-03 | 2019-06-07 | 中国计量大学 | A kind of foam conductive net/silica preparation facilities and control method |
CN109860507B (en) * | 2018-12-03 | 2022-01-28 | 中国计量大学 | Foam conductive net/silicon dioxide preparation device and control method |
CN109817925A (en) * | 2019-01-24 | 2019-05-28 | 广东凯金新能源科技股份有限公司 | Lithium ion secondary battery Si oxide composite negative pole material and preparation method |
CN112234183A (en) * | 2020-10-14 | 2021-01-15 | 中国计量大学 | Preparation method for in-situ synthesis of conductive metal/silicon/polymer-based negative electrode material |
CN115863660A (en) * | 2022-12-09 | 2023-03-28 | 江苏正力新能电池技术有限公司 | Negative current collector of negative-electrode-free lithium battery and preparation method and application thereof |
CN115863660B (en) * | 2022-12-09 | 2024-05-17 | 江苏正力新能电池技术有限公司 | Negative electrode current collector of non-negative electrode lithium battery and preparation method and application thereof |
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