CN110265640A - A method of preparing electrode of lithium cell carbon coating porous silica material - Google Patents
A method of preparing electrode of lithium cell carbon coating porous silica material Download PDFInfo
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- CN110265640A CN110265640A CN201910502926.3A CN201910502926A CN110265640A CN 110265640 A CN110265640 A CN 110265640A CN 201910502926 A CN201910502926 A CN 201910502926A CN 110265640 A CN110265640 A CN 110265640A
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- silicon
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- silica material
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- porous silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000011248 coating agent Substances 0.000 title claims abstract description 35
- 238000000576 coating method Methods 0.000 title claims abstract description 35
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 35
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002210 silicon-based material Substances 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 15
- 239000010703 silicon Substances 0.000 claims abstract description 15
- 229910021426 porous silicon Inorganic materials 0.000 claims description 83
- 239000011863 silicon-based powder Substances 0.000 claims description 51
- 229920001661 Chitosan Polymers 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 27
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 22
- 238000002604 ultrasonography Methods 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims description 21
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 20
- 239000011856 silicon-based particle Substances 0.000 claims description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000003638 chemical reducing agent Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 230000004087 circulation Effects 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 230000002441 reversible effect Effects 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- VZOPRCCTKLAGPN-ZFJVMAEJSA-L potassium;sodium;(2r,3r)-2,3-dihydroxybutanedioate;tetrahydrate Chemical compound O.O.O.O.[Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O VZOPRCCTKLAGPN-ZFJVMAEJSA-L 0.000 claims description 5
- 229940074446 sodium potassium tartrate tetrahydrate Drugs 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 claims description 3
- 238000004544 sputter deposition Methods 0.000 claims description 3
- 239000007772 electrode material Substances 0.000 abstract description 4
- 235000013339 cereals Nutrition 0.000 description 15
- 229960004756 ethanol Drugs 0.000 description 11
- -1 stir 3~5 hours Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000002153 silicon-carbon composite material Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000012686 silicon precursor Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000002194 amorphous carbon material Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention discloses a kind of method for preparing electrode of lithium cell carbon coating porous silica material, present invention incorporates forming porous structure on silicon materials and carbon coating silicon both effective methods are prepared for a kind of carbon coating porous silica material, effective solution silicon electrode material problem encountered.
Description
Technical field
The present invention relates to a kind of methods for preparing electrode of lithium cell carbon coating porous silica material.
Background technique
Currently, lithium ion battery is considered as the energy-storage system for being most commercialized value, have extended cycle life because it has,
Light weight, memory-less effect, it is environmental-friendly the features such as.But with large-scale energy storage facility, the quick hair in electric car field
Exhibition, the demand of more height ratio capacity, the more excellent lithium ion battery of battery performance are also increasing.The main composition of lithium ion battery
Part includes anode, cathode, electrolyte, diaphragm etc..Wherein, negative electrode material is also an important factor for influencing performance of lithium ion battery
One of.
In existing negative electrode material, it is existing frequently-used that silicon materials, which have highest theoretical specific capacity (4200mAh/g),
Ten times of specific capacity (372mAh/g) for being commercialized graphite material is more.Silica-base material is abundant due to saving in nature, environment
The advantages that friendly and height ratio capacity, it is considered to be the most lithium ion battery negative material of application prospect.However, by silicon substrate
Material large-scale commercial application also faces several serious problems.On the one hand, in charge and discharge process, a large amount of lithium ion batteries
Insertion and abjection silica-base material, cause silica-base material that huge volume change (> 300%), volume change constantly repeatedly occurs
So that generating crack between electrode material, or even fall off from collector, so as to cause between electrode material and electrode material
Electrical contact is lost between collector.Eventually lead to the fast decay of battery capacity.On the other hand, the electric conductivity of silicon materials is not
It is good, it is not able to satisfy the requirement of relatively high power battery.
Application No. is 201610901161.7, entitled " a kind of electrode of lithium cell of high capacity high stability is used
In silicon-carbon composite nano materials ", disclosed this composite nano materials are made of porous silicon and amorphous carbon material.Specific steps
Are as follows: the preparation of first step porous silicon matrix: ethyl alcohol and organosilicon are uniformly mixed, and it is water-soluble that inorganic acid is added under stirring
Liquid, reaction obtain mixed liquor A, prepare aqueous silicate solution and inorganic base is added, obtain mixed liquid B after reaction.A, B are mixed respectively
It is centrifuged after conjunction liquid aging, washs, is dried to obtain silicon precursor A, B, be finally uniformly mixed A, B silicon precursor, peptizing agent is added
Molding is dried and obtains porous silicon matrix after calcining.It is molten to be dissolved in dehydrated alcohol/water mixing by second step for carbon source and ferrocene
In agent, then the porous silicon matrix that the first step obtains is added thereto, is put into reaction kettle and reacts after ultrasonic treatment, by product from
Reaction kiln roasting is placed into after the heart, washing, drying, finally obtains silicon-carbon composite nano materials.The material that this method obtains
Although the performance for that can be got well in lithium battery, reaction process is complicated, and condition requires height to be not easy to industrial production.
Application No. is 201610214428.5, a kind of entitled " porous Si-C composite material and preparation method thereof
With application " in, open specific steps are as follows: the preparation of first step porous silicon: preparing the solution of the salt containing transiting state metal, and ammonium hydroxide is added
PH is adjusted, simple substance silica flour is then added, glucose solution is added and stirs 24 hours, obtaining to surface has transition metal particles deposition
Silicon powder, then be dispersed in the mixed liquor of hydrofluoric acid containing and hydrogen peroxide, stir 3~5 hours, product is redispersed in dilute nitre
It cleaned after being reacted in acid, be dried to obtain porous silicon powder.Step 2: phenylenediamine is dissolved in dilute hydrochloric acid, the first step is added
Obtained porous silicon powder is added sodium nitrite after ultrasonic and reacts 4~12 hours, places into instead after reaction product cleaning, drying
Sintering in furnace is answered to obtain porous Si-C composite material.This method is although fairly simple, but obtained material is applied to lithium ion
Battery cathode performance improvement is unobvious, and be also greatly improved space.
So the battery being assembled into using silicon materials as negative electrode of lithium ion battery, mainly faces two problems, one is lithium
Ion is constantly embedded in abjection silicon particle, so that its volume change is huge, the other is the problem of silicon materials poorly conductive.Often at present
The method for preparing silicon materials mainly passes through ball milling, and the methods of magnesium reduction process prepares nanoscale silicon, but such
Method is at high cost, and nano silicone is oxidizable so preparation condition is harsh, while not solving still the problem of the poorly conductive of silicon
Certainly.
Summary of the invention
Above of the existing technology to solve the problems, such as, the invention proposes a kind of easy to operate, at low cost prepares lithium
The problems such as battery electrode improves silicon materials poorly conductive with the method for carbon coating porous silica material, and volume expansion is serious, and
Obtain the good lithium ion cell electrode negative electrode material of height ratio capacity, cyclicity.
The present invention can be achieved by the following technical programs:
1. a kind of method for preparing electrode of lithium cell carbon coating porous silica material, which comprises the following steps:
1) it using the silicon powder of 1~20um of partial size as raw material, is first pre-processed, then ultrasonic, last drying for standby；
2) porous silicon is prepared, comprising: the first step is prepared and contains 0.2~15mol/L hydrofluoric acid and 0.005~0.50mol/L nitre
The mixed solution of sour silver, the silicon powder that the step 1) obtains is added thereto and is reacted, is washed with deionized water after the reaction was completed
It washs and filters or the first step, the method for chemical plating plates Ag or the first step in silicon powder surface, with magnetron sputtering method in silicon powder table
Face sputters upper Ag, obtains the silicon particle that surface is modified by Ag particle after dry；The silicon particle that Ag particle is modified is put by second step
The mixed solution etching of the hydrofluoric acid composition of the hydrogen peroxide and 0.1~5.0mol/L of 0.1~8.0mol/L, then uses deionization
Water is rinsed and is filtered, and obtains three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 0.5~10% and chitosan solution is made,
The three-dimensional porous silicon materials are put into deionized water, then to take 10~80ml chitosan solution to be put into the three-dimensional porous silicon water-soluble
In liquid, and mixed solution pH value is adjusted with hydrochloric acid and reaches 2~5, the positively charged chitosan solution absorption after electrostatic attraction
It is centrifuged after 60~90 DEG C are stirred 4~15 hours on electronegative three-dimensional porous silicon particle surface and dries or directly stir baking
It is dry, porous silicon chitosan complexes are obtained after freeze-drying, obtained porous silicon chitosan complexes are warm in nitrogen atmosphere
2~4 hours are handled to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment display its reversible capacity is 2005~2450mAh/g for the first time, after 200 circulations there are also 600~
800mAh/g。
Show fabulous specific capacity and cyclical stability.
Ultrasound described in step 1) of the present invention include first by Si powder be put into ethyl alcohol or acetone soln ultrasound 30~
Ultrasound 30~80 minutes in deionized water are put into after 80 minutes again.
Pretreatment includes the greasy dirt and impurity on removal Si powder surface in step 1) of the present invention.
Dry in step 1) of the present invention is 5~10 hours dry in an oven.
Reaction is stirred to react 1~10 minute under the conditions of being 20~30 DEG C in step 2) of the present invention.
Etching is to etch 10~50 minutes under the conditions of 20~30 DEG C in step 2) of the present invention.
The method of chemical plating of the present invention includes: to plate Ag in silicon face, prepares reducing agent first, first by 1~15g/L
Glucose and the mixing of 0.5~10g/L sodium potassium tartrate tetrahydrate are boiled, and 2~30ml/L ethyl alcohol and 1~12ml/L polyethylene glycol system are added
Reducing agent, then by 0.1~8g/L silver nitrate and 1~25ml/L ammonium hydroxide, 0.2~15ml/L ethylenediamine, 0.5~10g/L hydrogen-oxygen
Change potassium and be mixed to prepare main salt, Si powder is added after main salt and reducing agent are mixed, reaction obtains Ag particle after 10~30 minutes and repairs
The silicon particle of decorations.
Magnetron sputtering method of the present invention includes: uniformly to be laid in silicon powder on specimen rotating holder, using high-purity Ag as target
Material opens instrument switch, and the silicon materials of Ag particle modification are obtained after sputtering.
Carbon source can be chitosan, polyacrylamide or diallyl dimethyl ammoniumchloride in step 3) of the present invention
One of them.
Beneficial effects of the present invention: operation of the present invention is simple, raw material is cheap, step is controllable, it is raw to be conducive to large-scale industry
It produces.Material produced by the present invention is used in lithium ion battery simultaneously, obtains good battery performance, it is negative that silicon substrate has been effectively relieved
The shortcomings that pole volume expansion is serious and poorly conductive.
Detailed description of the invention
Fig. 1 is flow chart of the invention
Specific embodiment
Illustrate embodiments of the present invention below by way of particular specific embodiment, those skilled in the art can be by this theory
The bright revealed content of book is understood other advantages and efficacy of the present invention easily.
Embodiment 1
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) using the silicon powder of average grain diameter 15um as raw material, first pre-processed, remove Si powder surface greasy dirt and
Then Si powder is first put into ethanol solution after ultrasound 30 minutes and is put into ultrasound 30 minutes in deionized water, finally by impurity
In an oven dry 5 hours it is spare；
2) porous silicon is prepared, comprising: the first step prepares the mixing of hydrofluoric acid containing 10mol/L and 0.005mol/L silver nitrate
The silicon powder that the step 1) obtains is added thereto by solution, and 10min is stirred to react under the conditions of 20 DEG C, spend after the reaction was completed from
Sub- water washing simultaneously filters, and obtains the silicon particle that surface is modified by Ag particle after dry；Second step, the silicon particle that Ag particle is modified
It is put into the mixed solution of the hydrogen peroxide of 3mol/L and the hydrofluoric acid composition of 1mol/L, at 20 °C etching 10 minutes, so
It is rinsed and is filtered with deionized water afterwards, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 1% and chitosan solution is made, it will be described
Three-dimensional porous silicon materials are put into deionized water, then 10ml chitosan solution is taken to be put into porous silicon aqueous solution, and with hydrochloric acid tune
Section mixed solution pH value reaches 2, and positively charged chitosan solution is adsorbed on electronegative porous silicon after electrostatic attraction
Grain surface is centrifuged and obtains after drying porous silicon chitosan complexes, the porous silicon shell that will be obtained after 70 DEG C are stirred 4 hours
Glycan compound is heat-treated 2 hours in nitrogen atmosphere to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2025mAh/g for the first time for it, and there are also 710mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 2
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) it using the silicon powder of average grain diameter 5um as raw material, is first pre-processed, removes the greasy dirt on Si powder surface and miscellaneous
Then Si powder is first put into acetone soln after ultrasound 80 minutes and is put into ultrasound 80 minutes in deionized water, finally exists by matter
In baking oven dry 10 hours it is spare；
2) porous silicon is prepared, comprising: the first step plates Ag in silicon face, prepares reducing agent first, first by 15g/L grape
Sugar and the mixing of 8g/L sodium potassium tartrate tetrahydrate are boiled, and are added 30ml/L ethyl alcohol and 12ml/L polyethylene glycol and are made reducing agent, then by 3g/
L silver nitrate and 25ml/L ammonium hydroxide, 10ml/L ethylenediamine, 10g/L potassium hydroxide are mixed to prepare main salt, and main salt and reducing agent are mixed
After be added Si powder, reaction after ten minutes, is dried to obtain the silicon particle of Ag particle modification；Second step, the silicon that Ag particle is modified
Particle is put into the mixed solution of the hydrogen peroxide of 0.6mol/L and the hydrofluoric acid composition of 0.1mol/L, etches 10 under the conditions of 25 DEG C
Minute, it is then rinsed and is filtered with deionized water, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 5% and chitosan solution is made, it will be described
Three-dimensional porous silicon materials are put into deionized water, then 15ml chitosan solution is taken to be put into porous silicon aqueous solution, and with hydrochloric acid tune
Section mixed solution pH value reaches 3, and positively charged chitosan solution is adsorbed on electronegative porous silicon after electrostatic attraction
Grain surface is centrifuged and obtains after drying porous silicon chitosan complexes, the porous silicon shell that will be obtained after 70 DEG C are stirred 6 hours
Glycan compound is heat-treated 2.5 hours in nitrogen atmosphere to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2250mAh/g for the first time for it, and there are also 720mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 3
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) using the silicon powder of average grain diameter 10um as raw material, first pre-processed, remove Si powder surface greasy dirt and
Then Si powder is first put into ethanol solution after ultrasound 50 minutes and is put into ultrasound 30 minutes in deionized water, finally by impurity
In an oven dry 10 hours it is spare；
2) porous silicon is prepared, comprising: silicon powder is uniformly laid on specimen rotating holder, using high-purity Ag as target by the first step
Material opens instrument switch, and the silicon materials of Ag particle modification are obtained after sputtering；The silicon particle that Ag particle is modified is put by second step
The mixed solution of the hydrofluoric acid of the hydrogen peroxide of 0.6mol/L and 0.8mol/L composition, etches 30 minutes under the conditions of 25 DEG C, so
It is rinsed and is filtered with deionized water afterwards, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 4% and chitosan solution is made, it will be described
Three-dimensional porous silicon materials are put into deionized water, then 35ml chitosan solution is taken to be put into porous silicon aqueous solution, and with hydrochloric acid tune
Section mixed solution pH value reaches 3.5, and positively charged chitosan solution is adsorbed on electronegative porous silicon after electrostatic attraction
Particle surface obtains porous silicon chitosan complexes, obtained porous silicon shell is gathered after 90 DEG C are stirred 7 hours after freeze-drying
Saccharide complex is heat-treated 4 hours in nitrogen atmosphere to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2450mAh/g for the first time for it, and there are also 780mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 4
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) it using the silicon powder of average grain diameter 1um as raw material, is first pre-processed, removes the greasy dirt on Si powder surface and miscellaneous
Then Si powder is first put into ultrasound in ethanol solution and is put into ultrasound 30 minutes in deionized water again after sixty minutes, finally existed by matter
In baking oven dry 5 hours it is spare；
2) porous silicon is prepared, comprising: the first step, the mixing for preparing hydrofluoric acid containing 15mol/L and 0.5mol/L silver nitrate are molten
The silicon powder that the step 1) obtains is added thereto by liquid, and 1min is stirred to react under the conditions of 30 DEG C, uses deionized water after the reaction was completed
It washs and filters, obtain the silicon particle that surface is modified by Ag particle after dry；The silicon particle that Ag particle is modified is put by second step
The mixed solution of the hydrofluoric acid of the hydrogen peroxide of 6.0mol/L and 5mol/L composition, etches 50 minutes under the conditions of 30 DEG C, then
It is rinsed and is filtered with deionized water, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 5% and chitosan solution is made, it will be described
Three-dimensional porous silicon materials are put into deionized water, then 50ml chitosan solution is taken to be put into porous silicon aqueous solution, and with hydrochloric acid tune
Section mixed solution pH value reaches 5, and positively charged chitosan solution is adsorbed on electronegative porous silicon after electrostatic attraction
Grain surface obtains porous silicon chitosan complexes, the porous silicon that will be obtained after 80 DEG C are stirred 4 hours after direct stirring and drying
Chitosan complexes are heat-treated 4 hours in nitrogen atmosphere to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2250mAh/g for the first time for it, and there are also 610mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 5
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) using the silicon powder of average grain diameter 20um as raw material, first pre-processed, remove Si powder surface greasy dirt and
Then Si powder is first put into ethyl alcohol or acetone soln after ultrasound 30 minutes and is put into 30 points of ultrasound in deionized water by impurity
Clock, finally in an oven dry 10 hours it is spare；
2) porous silicon is prepared, comprising: the first step, the mixing for preparing hydrofluoric acid containing 5mol/L and 0.02mol/L silver nitrate are molten
The silicon powder that the step 1) obtains is added thereto by liquid, and 5min is stirred to react under the conditions of 20 DEG C, uses deionized water after the reaction was completed
It washs and filters, obtain the silicon particle that surface is modified by Ag particle after dry；The silicon particle that Ag particle is modified is put by second step
The mixed solution of the hydrofluoric acid of the hydrogen peroxide of 0.8mol/L and 0.5mol/L composition, etches 30 minutes at 20 °C, so
It is rinsed and is filtered with deionized water afterwards, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 8% and chitosan solution is made, it will be described
Three-dimensional porous silicon materials are put into deionized water, then 80ml chitosan solution is taken to be put into porous silicon aqueous solution, and with hydrochloric acid tune
Section mixed solution pH value reaches 2.5, and positively charged chitosan solution is adsorbed on electronegative porous silicon after electrostatic attraction
Particle surface is centrifuged and obtains after drying porous silicon chitosan complexes, the porous silicon that will be obtained after 70 DEG C are stirred 10 hours
Chitosan complexes are heat-treated 3 hours in nitrogen atmosphere to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2120mAh/g for the first time for it, and there are also 800mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 6
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) using the silicon powder of average grain diameter 10um as raw material, first pre-processed, remove Si powder surface greasy dirt and
Then Si powder is first put into acetone soln after ultrasound 50 minutes and is put into ultrasound 50 minutes in deionized water, finally by impurity
In an oven dry 7 hours it is spare；
2) porous silicon is prepared, comprising: the first step plates Ag in silicon face, prepares reducing agent first, first by 1g/L glucose
It is boiled with the mixing of 0.5g/L sodium potassium tartrate tetrahydrate, adds 3ml/L ethyl alcohol and 2ml/L polyethylene glycol and be made reducing agent, then by 0.1g/
L silver nitrate and 5ml/L ammonium hydroxide, 2ml/L ethylenediamine, 1g/L potassium hydroxide are mixed to prepare main salt, after main salt and reducing agent are mixed
Si powder is added and is dried to obtain the silicon particle of Ag particle modification after reaction 30 minutes；Second step, the silicon that Ag particle is modified
Grain is put into the mixed solution of the hydrogen peroxide of 1.2mol/L and the hydrofluoric acid composition of 0.3mol/L, and 30 points are etched under the conditions of 25 DEG C
Then clock is rinsed and is filtered with deionized water, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 1% and chitosan solution is made, it will be described
Three-dimensional porous silicon materials are put into deionized water, then 55ml chitosan solution is taken to be put into porous silicon aqueous solution, and with hydrochloric acid tune
Section mixed solution pH value reaches 5, and positively charged chitosan solution is adsorbed on electronegative porous silicon after electrostatic attraction
Grain surface is centrifuged and dries or direct stirring and drying, porous silicon chitosan is obtained after freeze-drying after 60 DEG C are stirred 15 hours
Obtained porous silicon chitosan complexes are heat-treated 4 hours to get carbon-coated porous silicon is arrived by compound in nitrogen atmosphere
Composite material；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2005mAh/g for the first time for it, and there are also 680mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 7
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) using the silicon powder of average grain diameter 15um as raw material, first pre-processed, remove Si powder surface greasy dirt and
Then Si powder is first put into ethyl alcohol or acetone soln after ultrasound 80 minutes and is put into 80 points of ultrasound in deionized water by impurity
Clock, finally in an oven dry 8 hours it is spare；
2) porous silicon is prepared, comprising: the first step, preparation hydrofluoric acid containing 0.20mol/L and 0.005mol/L silver nitrate mix
Solution is closed, the silicon powder that the step 1) obtains is added thereto, 10min is stirred to react under the conditions of 25 DEG C, is spent after the reaction was completed
Ion water washing simultaneously filters, and obtains the silicon particle that surface is modified by Ag particle after dry；Second step, the silicon that Ag particle is modified
Grain is put into the mixed solution of the hydrogen peroxide of 8mol/L and the hydrofluoric acid composition of 2mol/L, etches 50 minutes under the conditions of 25 DEG C,
Then it is rinsed and is filtered with deionized water, obtain three-dimensional porous silicon after dry；
3) Polyacrylamide Powder as carbon source is dissolved in 50ml deionized water, by the three-dimensional porous silicon materials
It is put into the ionized water containing carbon source, and adjusts mixed solution pH value with hydrochloric acid and reach 5, after 70 DEG C are stirred 4 hours, freezing
Porous silicon polyacrylamide amine compound is obtained after drying, obtained porous silicon polyacrylamide amine compound is warm in nitrogen atmosphere
3 hours are handled to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2145mAh/g for the first time for it, and there are also 750mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
Embodiment 8
A method of preparing electrode of lithium cell carbon coating porous silica material, comprising the following steps:
1) using the silicon powder of average grain diameter 10um as raw material, first pre-processed, remove Si powder surface greasy dirt and
Then Si powder is first put into acetone soln after ultrasound 50 minutes and is put into ultrasound 80 minutes in deionized water, finally by impurity
In an oven dry 5 hours it is spare；
2) porous silicon is prepared, comprising: the first step plates Ag in silicon face, prepares reducing agent first, first by 5g/L glucose
It is boiled with the mixing of 4g/L sodium potassium tartrate tetrahydrate, adds 2ml/L ethyl alcohol and 1ml/L polyethylene glycol and be made reducing agent, then by 0.5g/L
Silver nitrate and 15ml/L ammonium hydroxide, 6ml/L ethylenediamine, 5g/L potassium hydroxide are mixed to prepare main salt, after main salt and reducing agent are mixed
Si powder is added, reaction after ten minutes, is dried to obtain the silicon particle of Ag particle modification；Second step, the silicon that Ag particle is modified
Grain is put into the mixed solution of the hydrogen peroxide of 0.1mol/L and the hydrofluoric acid composition of 1.5mol/L, and 30 points are etched under the conditions of 30 DEG C
Then clock is rinsed and is filtered with deionized water, obtain three-dimensional porous silicon after dry；
3) the diallyl dimethyl ammoniumchloride powder as carbon source is dissolved in 50ml deionized water solution, it will be described
Three-dimensional porous silicon materials are put into the ionized water containing carbon source, and are adjusted mixed solution pH value with hydrochloric acid and reached 2, are stirred at 80 DEG C
After mixing 10 hours, it is centrifuged and obtains porous silicon diallyl dimethyl ammoniumchloride compound, the porous silicon that will be obtained after drying
Diallyl dimethyl ammoniumchloride compound is heat-treated 3 hours in nitrogen atmosphere to get compound to carbon-coated porous silicon
Material；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, is filled later
Discharge test, experiment show that reversible capacity is 2145mAh/g for the first time for it, and there are also 670mAh/g later for 200 circulations, show pole
Good specific capacity and cyclical stability.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of method for preparing electrode of lithium cell carbon coating porous silica material, which comprises the following steps:
1) it using the silicon powder of 1~20um of partial size as raw material, is first pre-processed, then ultrasonic, last drying for standby；
2) porous silicon is prepared, comprising: the first step is prepared and contains 0.2~15mol/L hydrofluoric acid and 0.005~0.50mol/L silver nitrate
Mixed solution, the silicon powder that the step 1) obtains is added thereto and is reacted, is washed with deionized after the reaction was completed simultaneously
It filters or the first step, the method for chemical plating plates Ag or the first step in silicon powder surface, splashed with magnetron sputtering method in silicon powder surface
Ag is penetrated, obtains the silicon particle that surface is modified by Ag particle after dry；The silicon particle that Ag particle is modified is put into 0.1 by second step
The mixed solution etching of the hydrofluoric acid composition of the hydrogen peroxide and 0.1~5.0mol/L of~8.0mol/L, then uses deionized water
It rinses and filters, obtain three-dimensional porous silicon after dry；
3) Chitosan powder as carbon source is dissolved in the acetum containing 0.5~10% and chitosan solution is made, by institute
It states three-dimensional porous silicon materials to be put into deionized water, then 10~80ml chitosan solution is taken to be put into the three-dimensional porous silicon aqueous solution
In, and adjust mixed solution pH value with hydrochloric acid and reach 2~5, positively charged chitosan solution is adsorbed on after electrostatic attraction
Electronegative three-dimensional porous silicon particle surface is centrifuged after 60~90 DEG C are stirred 4~15 hours and dries or directly stir baking
It is dry, porous silicon chitosan complexes are obtained after freeze-drying, obtained porous silicon chitosan complexes are warm in nitrogen atmosphere
2~4 hours are handled to get carbon-coated porous silicon composite material is arrived；
4) assembled battery is carried out using obtained carbon coating porous silica material as the cathode of lithium ion battery, carries out charge and discharge later
Experiment tests and shows that reversible capacity is 2005~2450mAh/g, also 600~800mAh/g after 200 circulations for the first time for it.
2. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
Stating ultrasound described in step 1) includes that first Si powder is put into ethyl alcohol or acetone soln after ultrasound 30~80 minutes and is put into
Ultrasound 30~80 minutes in ionized water.
3. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
State the greasy dirt and impurity that pretreatment in step 1) includes removal Si powder surface.
4. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
It is 5~10 hours dry in an oven for stating dry in step 1).
5. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
It states under the conditions of reaction in step 2) is 20~30 DEG C and is stirred to react 1~10 minute.
6. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
Stating etching in step 2) is to etch 10~50 minutes under the conditions of 20~30 DEG C.
7. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
The method for stating chemical plating includes: to plate Ag in silicon face, prepares reducing agent first, first by 1~15g/L glucose and 0.5~
The mixing of 10g/L sodium potassium tartrate tetrahydrate is boiled, and adds 2~30ml/L ethyl alcohol and reducing agent is made in 1~12ml/L polyethylene glycol, then will
0.1~8g/L silver nitrate and 1~25ml/L ammonium hydroxide, 0.2~15ml/L ethylenediamine, 0.5~10g/L potassium hydroxide are mixed to prepare master
Salt, is added Si powder after main salt and reducing agent are mixed, reaction obtains the silicon particle of Ag particle modification after 10~30 minutes.
8. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
Stating magnetron sputtering method includes: uniformly to be laid in silicon powder on specimen rotating holder, using high-purity Ag as target, opens instrument switch,
The silicon materials of Ag particle modification are obtained after sputtering.
9. the method according to claim 1 for preparing electrode of lithium cell carbon coating porous silica material, which is characterized in that institute
Stating carbon source in step 3) can be one of chitosan, polyacrylamide or diallyl dimethyl ammoniumchloride.
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Application publication date: 20190920 |