CN107959019A - A kind of preparation of graphene tinbase silicon based cells negative material - Google Patents
A kind of preparation of graphene tinbase silicon based cells negative material Download PDFInfo
- Publication number
- CN107959019A CN107959019A CN201711323881.0A CN201711323881A CN107959019A CN 107959019 A CN107959019 A CN 107959019A CN 201711323881 A CN201711323881 A CN 201711323881A CN 107959019 A CN107959019 A CN 107959019A
- Authority
- CN
- China
- Prior art keywords
- reactor
- solution
- suspension
- graphene
- silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- H01M4/36—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
- H01M4/36—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
- H01M4/387—Tin or alloys based on tin
-
- 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
Abstract
The present invention proposes a kind of preparation of graphene tinbase silicon based cells negative material,First at ambient temperature,Then a certain amount of powdered native graphite is weighed by weighing apparatus,Potassium permanganate and sodium nitrate,Then powdered native graphite is put into reactor,Then sodium nitrate is added in reactor again,Reactor is put into cryostat pond again,Then certain concentrated sulfuric acid is measured by graduated cylinder,Then the concentrated sulfuric acid is placed into reactor,Then potassium permanganate is divided into more parts to be added separately in reactor,Fully reactor is taken out from cryostat pond after reaction,Obtain the suspension of brown viscous,The new method for preparing graphene negative material,Step is simple,It is easy to operate,Not only obtained lithium cell cathode material excellent performance,And preparation method is simple,So that the storage battery produced is more durable,Better quality,Provide a convenient,It is adapted to industrialized production.
Description
Technical field
The present invention relates to cell negative electrode material preparing technical field, is specially a kind of graphene tinbase silicon based cells anode material
The preparation of material.
Background technology
In recent years, lithium ion battery is widely used in portable power, electric automobile, hybrid-electric car and wind energy, too
Positive energy energy storage.But its security is bad, theoretical specific capacity is relatively low and high rate capability is poor, has been difficult to meet the development of the national economy
The requirement growing day by day to lithium ion battery, graphene have very high theoretical specific surface area with social development.It is in the world most
Thin is also most hard nano material, and thermal conductivity ratio carbon nanotubes and diamond are taller, its electron mobility also compares nano-sized carbon
Pipe or silicon crystal are high, and resistivity only has about 10-6Ω cm, are the materials of world resistivity minimum.Due to graphene these
Excellent property, it has very big potential application in field of batteries, and due to tin, silicon is considered as before one kind has very much all the time
The negative material on way, but there are serious problems in actual lithium ion battery applications, mainly due to its undesirable battery
Caused by recycling the significantly volume change caused by performance and electrode charge discharge process, therefore using not
Just.
The content of the invention
The technical problem to be solved in the present invention is overcome the defects of existing, there is provided a kind of graphene tinbase silicon based cells anode
The preparation of material, step is simple, easy to operate, not only obtained lithium cell cathode material excellent performance, and preparation method letter
It is single, it is adapted to industrialized production, can effectively solves the problems, such as in background technology.
To achieve the above object, the present invention proposes：A kind of preparation of graphene tinbase silicon based cells negative material, including with
Lower step：
S1) yellowish-brown graphene oxide solid is produced：First at ambient temperature, then weighed by weighing apparatus a certain amount of
Powdered native graphite, potassium permanganate and sodium nitrate, then powdered native graphite is put into reactor, then again will
Sodium nitrate is added in reactor, then reactor is put into cryostat pond, and certain concentrated sulfuric acid is then measured by graduated cylinder,
Then the concentrated sulfuric acid is placed into reactor, potassium permanganate then is divided into more parts is added separately in reactor, fully reaction
Reactor is taken out from cryostat pond afterwards, obtains the suspension of brown viscous, then measuring a certain amount of water using graduated cylinder instills
Into brown suspension, reacted diluting constantly temperature to suspension and being maintained at 80-100 DEG C, then suspension is stood, and makes to hang
The temperature of supernatant liquid adds the mixed liquor of certain proportion hydrogen peroxide and distilled water when being down to 40-60 DEG C, glassy yellow oxidation is obtained with this
Glassy yellow graphite oxide dispersion, is then put into centrifugal separator by graphite dispersing solution, by centrifugal separator by suspension
In supernatant remove, solid is obtained with this, obtained solid is washed using distilled water, then using 30% hydrochloric acid and second
Alcohol washs fixation respectively, and finally, using petroleum ether precipitation, then general teflon membrane filter filtering, then passes through
Solid is dried in drying machine, and yellowish-brown graphene oxide solid is obtained with this；
S2) Primary product is produced：Take a certain amount of chlorination tin-salt solution to be put into reactor first, then pass through stirring
Device is stirred, and the graphene oxide produced is added in solution after stirring, and then solution is shaken by ultrasonic oscillator
Swing 1-3 it is small when, then add a certain amount of 37% hydrochloric acid solution, then by magnetic stirring apparatus to solution stir 6-10 it is small when,
Then be then added to hydrazine hydrate, then by reactor be put into sea water bath stirring 8 it is small when, after reaction, then will hold liquid
Filtered after standing room temperature, then washed, make the liquid PH after washing be equal to 7, then by reactant be put into from
In scheming, by obtaining product after centrifuge, then by product by vacuum drier dry 5-18 it is small when, obtained with this
Primary product；
S3) silicon nanoparticle suspension is produced：A certain amount of nano silicon particles are weighed by weigher, so by 20%
The solution and nano silicon particles of HF/ ethanol will be placed into reactor, and certain time is stood at room temperature after reaction, then will be mixed
Compound hair puts drying in vacuum drying oven, obtains a nanometer silicon ion with this, then nanometer silicon ion is put into ethanol solution,
Suspension is obtained with this, then suspension is put into centrifuge, is handled by centrifuge, with this to nanometer silicon ion
Collect, disperseed with what this was repeated, centrifugation, drying process, silicon nanoparticle suspension is obtained with this；
S4) graphene/Sn/Si composite materials：Primary product is added in ethanol solution again, then silicon nanoparticle is suspended
Liquid is added dropwise in solution, is then shaken certain time to solution by ultrasonic oscillator, is then coated, and in high temperature
Under the conditions of hydrogen/argon gas calcine some hours, graphene/Sn/Si composite materials are obtained with this.
As a preferred technical solution of the present invention：After reactor is taken out from cryostat pond, then reaction is held
Device is heated between 30-40 DEG C, then by blender machine to solution stir 1-3 it is small when.
As a preferred technical solution of the present invention：After the solution reaction of nano silicon particles and the 20%HF/ ethanol,
It is multiple by ethanol washing, HF excessive in solution is removed with this.
Compared with prior art, the beneficial effects of the invention are as follows：The new method for preparing graphene negative material, step
Simply, it is easy to operate, not only obtained lithium cell cathode material excellent performance, and preparation method is simple so that produce
Storage battery is more durable, and better quality, provides a convenient, and is adapted to industrialized production.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all
Belong to the scope of protection of the invention.
The present invention provides following technical scheme：A kind of preparation of graphene tinbase silicon based cells negative material, including it is following
Step：
S1) yellowish-brown graphene oxide solid is produced：First at ambient temperature, then weighed by weighing apparatus a certain amount of
Powdered native graphite, potassium permanganate and sodium nitrate, then powdered native graphite is put into reactor, then again will
Sodium nitrate is added in reactor, then reactor is put into cryostat pond, and certain concentrated sulfuric acid is then measured by graduated cylinder,
Then the concentrated sulfuric acid is placed into reactor, potassium permanganate then is divided into more parts is added separately in reactor, fully reaction
Reactor is taken out from cryostat pond afterwards, after reactor is taken out from cryostat pond, reaction vessel is then heated to 30-40
Between DEG C, then by blender machine to solution stir 1-3 it is small when, the suspension of brown viscous is obtained, then using graduated cylinder amount
Take a certain amount of water to be added dropwise in brown suspension, reacted diluting constantly temperature to suspension and being maintained at 80-100 DEG C, so
Rear suspension liquid is stood, and the mixed liquor of certain proportion hydrogen peroxide and distilled water is added when the temperature of suspension is down to 40-60 DEG C, with
This obtains glassy yellow graphite oxide dispersion, and then glassy yellow graphite oxide dispersion is put into centrifugal separator, by from
Centrifugal separator removes the supernatant in suspension, obtains solid with this, obtained solid is washed using distilled water, then
Fixation is washed respectively using 30% hydrochloric acid and ethanol, finally, using petroleum ether precipitation, then general polytetrafluoroethylene (PTFE)
Membrane filtration, is then dried solid by drying machine, and yellowish-brown graphene oxide solid is obtained with this；
S2) Primary product is produced：Take a certain amount of chlorination tin-salt solution to be put into reactor first, then pass through stirring
Device is stirred, and the graphene oxide produced is added in solution after stirring, and then solution is shaken by ultrasonic oscillator
Swing 1-3 it is small when, then add a certain amount of 37% hydrochloric acid solution, then by magnetic stirring apparatus to solution stir 6-10 it is small when,
Then be then added to hydrazine hydrate, then by reactor be put into sea water bath stirring 8 it is small when, after reaction, then will hold liquid
Filtered after standing room temperature, then washed, make the liquid PH after washing be equal to 7, then by reactant be put into from
In scheming, by obtaining product after centrifuge, then by product by vacuum drier dry 5-18 it is small when, obtained with this
Primary product；
S3) silicon nanoparticle suspension is produced：A certain amount of nano silicon particles are weighed by weigher, so by 20%
The solution and nano silicon particles of HF/ ethanol will be placed into reactor, and certain time is stood at room temperature after reaction, silicon nanometer
After the solution reaction of grain and 20%HF/ ethanol, washed repeatedly by ethanol, removed HF excessive in solution with this, then will
Mixture hair puts drying in vacuum drying oven, obtains a nanometer silicon ion with this, nanometer silicon ion then is put into ethanol solution
In, suspension is obtained with this, then suspension is put into centrifuge, is handled by centrifuge, with this to nano-silicon
Ioncollection, is disperseed, centrifugation, drying process, silicon nanoparticle suspension is obtained with this with what this was repeated；
S4) graphene/Sn/Si composite materials：Primary product is added in ethanol solution again, then silicon nanoparticle is suspended
Liquid is added dropwise in solution, is then shaken certain time to solution by ultrasonic oscillator, is then coated, and in high temperature
Under the conditions of hydrogen/argon gas calcine some hours, graphene/Sn/Si composite materials are obtained with this.
Benefit of the present invention：The new method for preparing graphene negative material, step is simple, easy to operate, is not only made
Lithium cell cathode material excellent performance, and preparation method is simple so that the storage battery produced is more durable, and quality is more
It is good, provide a convenient, be adapted to industrialized production.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of changes, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (3)
- A kind of 1. preparation of graphene tinbase silicon based cells negative material, it is characterised in that：Comprise the following steps：S1）Yellowish-brown graphene oxide solid is produced：First at ambient temperature, then a certain amount of powder is weighed by weighing apparatus Powdered native graphite, is then put into reactor by last shape native graphite, potassium permanganate and sodium nitrate, then again by nitric acid Sodium is added in reactor, then reactor is put into cryostat pond, certain concentrated sulfuric acid is then measured by graduated cylinder, then The concentrated sulfuric acid is placed into reactor, potassium permanganate then is divided into more parts is added separately in reactor, will fully after reaction Reactor takes out from cryostat pond, obtains the suspension of brown viscous, then using graduated cylinder measure a certain amount of water be added dropwise to it is brown In color suspension, reacted diluting constantly temperature to suspension and being maintained at 80-100 DEG C, then suspension is stood, and makes suspension Temperature the mixed liquor of certain proportion hydrogen peroxide and distilled water is added when being down to 40-60 DEG C, glassy yellow graphite oxide is obtained with this Glassy yellow graphite oxide dispersion, is then put into centrifugal separator by dispersion liquid, by centrifugal separator by suspension Supernatant removes, and obtains solid with this, obtained solid is washed using distilled water, then using 30% hydrochloric acid and ethanol pair Fixation is washed respectively, and finally, using petroleum ether precipitation, then general teflon membrane filter filtering, then passes through drying Solid is dried in machine, and yellowish-brown graphene oxide solid is obtained with this；S2）Primary product is produced：Take a certain amount of chlorination tin-salt solution to be put into reactor first, then by blender into The graphene oxide produced, is added in solution by row stirring after stirring, then shakes 1-3 to solution by ultrasonic oscillator Hour, then add a certain amount of 37% hydrochloric acid solution, then by magnetic stirring apparatus to solution stir 6-10 it is small when, Ran Houzai Be added to hydrazine hydrate, then by reactor be put into sea water bath stirring 8 it is small when, after reaction, then will hold liquid and stand and arrive Filtered after room temperature, then washed, the liquid PH after washing is equal to 7, then reactant is put into centrifuge, By obtaining product after centrifuge, then by product by vacuum drier dry 5-18 it is small when, primary production is obtained with this Thing；S3）Silicon nanoparticle suspension is produced：A certain amount of nano silicon particles are weighed by weigher, so by 20%HF/ ethanol Solution and nano silicon particles will be placed into reactor, stand certain time at room temperature after reaction, then send out mixture Drying in vacuum drying oven is put, a nanometer silicon ion is obtained with this, then nanometer silicon ion is put into ethanol solution, is obtained with this To suspension, then suspension is put into centrifuge, is handled by centrifuge, with this to nano-silicon ioncollection, Disperseed with what this was repeated, centrifugation, drying process, silicon nanoparticle suspension is obtained with this；S4）Graphene/Sn/Si composite materials：Primary product is added in ethanol solution again, then by the suspended drop of silicon nanoparticle Enter into solution, certain time is then shaken to solution by ultrasonic oscillator, is then coated, and in hot conditions Lower hydrogen/argon gas calcines some hours, and graphene/Sn/Si composite materials are obtained with this.
- A kind of 2. preparation of graphene tinbase silicon based cells negative material according to claim 1, it is characterised in that：By instead After answering device to be taken out from cryostat pond, between reaction vessel then is heated to 30-40 DEG C, then solution is stirred by blender machine Mix 1-3 it is small when.
- A kind of 3. preparation of graphene tinbase silicon based cells negative material according to claim 1, it is characterised in that：The silicon After the solution reaction of nano particle and 20%HF/ ethanol, washed repeatedly by ethanol, removed HF excessive in solution with this.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711323881.0A CN107959019A (en) | 2017-12-13 | 2017-12-13 | A kind of preparation of graphene tinbase silicon based cells negative material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711323881.0A CN107959019A (en) | 2017-12-13 | 2017-12-13 | A kind of preparation of graphene tinbase silicon based cells negative material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107959019A true CN107959019A (en) | 2018-04-24 |
Family
ID=61957778
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711323881.0A Pending CN107959019A (en) | 2017-12-13 | 2017-12-13 | A kind of preparation of graphene tinbase silicon based cells negative material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107959019A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109546115A (en) * | 2018-11-19 | 2019-03-29 | 安徽安凯汽车股份有限公司 | A kind of NCA ternary battery of nickelic rich lithium manganese base solid solution positive electrode |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102576859A (en) * | 2009-09-25 | 2012-07-11 | 株式会社丰田自动织机 | Negative electrode for lithium-ion secondary battery, and manufacturing process for the same |
| CN103189313A (en) * | 2010-09-03 | 2013-07-03 | 奈克松有限公司 | Electroactive material |
| CN104009205A (en) * | 2014-06-12 | 2014-08-27 | 上海中聚佳华电池科技有限公司 | Hollow graphene ball and preparation method and application thereof |
| CN104064739A (en) * | 2014-07-02 | 2014-09-24 | 长沙国容新能源有限公司 | Tin cobalt alloy/ graphene composite material and preparation method thereof |
| CN107359308A (en) * | 2017-07-25 | 2017-11-17 | 南京红太阳新能源有限公司 | A kind of Preparation equipment and method of graphene silicon lithium cell cathode material |
| CN107394165A (en) * | 2017-07-25 | 2017-11-24 | 南京红太阳新能源有限公司 | A kind of Preparation equipment and method of graphene tin cobalt lithium cell cathode material |
-
2017
- 2017-12-13 CN CN201711323881.0A patent/CN107959019A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102576859A (en) * | 2009-09-25 | 2012-07-11 | 株式会社丰田自动织机 | Negative electrode for lithium-ion secondary battery, and manufacturing process for the same |
| CN103189313A (en) * | 2010-09-03 | 2013-07-03 | 奈克松有限公司 | Electroactive material |
| CN104009205A (en) * | 2014-06-12 | 2014-08-27 | 上海中聚佳华电池科技有限公司 | Hollow graphene ball and preparation method and application thereof |
| CN104064739A (en) * | 2014-07-02 | 2014-09-24 | 长沙国容新能源有限公司 | Tin cobalt alloy/ graphene composite material and preparation method thereof |
| CN107359308A (en) * | 2017-07-25 | 2017-11-17 | 南京红太阳新能源有限公司 | A kind of Preparation equipment and method of graphene silicon lithium cell cathode material |
| CN107394165A (en) * | 2017-07-25 | 2017-11-24 | 南京红太阳新能源有限公司 | A kind of Preparation equipment and method of graphene tin cobalt lithium cell cathode material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109546115A (en) * | 2018-11-19 | 2019-03-29 | 安徽安凯汽车股份有限公司 | A kind of NCA ternary battery of nickelic rich lithium manganese base solid solution positive electrode |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105355877B (en) | A kind of graphene metal oxide composite cathode material and preparation method thereof | |
| CN110518251A (en) | A kind of three-dimensional grapheme powder body material and preparation method thereof | |
| CN105390687A (en) | High-performance three-dimensional carbon nanotube composite negative electrode material, preparation method therefor and application thereof | |
| CN108682833B (en) | Preparation method of lithium iron phosphate-based modified cathode material | |
| CN110838583B (en) | Carbon nanotube/M-phase vanadium dioxide composite structure, preparation method thereof and application thereof in water-based zinc ion battery | |
| CN109088064A (en) | A kind of preparation method and application of the graphene-based metal oxide of electrochemical stripping | |
| CN106865496A (en) | Nickel cobalt lithium aluminate cathode material of aluminium nanometer doped zinc oxide cladding and preparation method thereof | |
| CN106025228A (en) | Nanocomposite loading carbon-coated SnO2 nano particles on graphene sheets and preparation method of nanocomposite | |
| CN109742378B (en) | CoTe nanowire-graphene composite material and preparation method thereof | |
| CN103887489A (en) | Preparation method of high-specific-capacity graphene coated nickel-cobalt lithium manganate material | |
| CN108832107B (en) | Graphene quantum dot-bio-based activated carbon composite material and preparation method thereof | |
| CN112968173A (en) | Porous carbon-coated sulfur vacancy composite electrode material, preparation method thereof and circular electrode adopting material | |
| Chen et al. | Designing of carbon cloth@ Co-MOF@ SiO2 as superior flexible anode for lithium-ion battery | |
| CN105609746B (en) | A kind of combination electrode of simultaneous electrochemical storage sodium and storage lithium and preparation method thereof | |
| CN103872306A (en) | Preparation method of lithium titanate negative electrode slurry | |
| CN107959017A (en) | A kind of solid carbon ball lithium ion battery negative material of graphene/oxide coated by zinc and preparation method thereof | |
| Zhang et al. | CNTs boosting superior cycling stability of ZnFe2O4/C nanoparticles as high-capacity anode materials of Li-ion batteries | |
| CN108878847A (en) | Lithium sulfur battery anode material and preparation method thereof | |
| CN105633385B (en) | A kind of SnCoS4Composite nanocrystalline-graphene composite material and preparation method thereof | |
| CN104979557A (en) | High-rate lithium iron phosphate positive electrode material and battery electrode sheet | |
| CN107959019A (en) | A kind of preparation of graphene tinbase silicon based cells negative material | |
| CN106784728A (en) | Conduction high polymer cladding sulfur electrode material and its manufacture method of a kind of high-capacity secure | |
| CN111285408A (en) | Method for preparing iron oxide negative electrode material of lithium ion power battery | |
| CN103887477B (en) | A kind of preparation method of the Graphene modified phosphate ferrum lithium anode material of high power capacity | |
| WO2024036906A1 (en) | Lithium-ion battery positive electrode material and preparation method therefor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180424 |
|
| RJ01 | Rejection of invention patent application after publication |