CN109860499A - Aoxidize the preparation process of sub- silicon and the compound ear pole material of polyimides - Google Patents
Aoxidize the preparation process of sub- silicon and the compound ear pole material of polyimides Download PDFInfo
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Abstract
The present invention provides a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides, is related to technical field of lithium ion.Specifically includes the following steps: preparing cellular porous polyimides；Prepare nano oxidized sub- silicon；The inorganic compound of the porous polyimide, nano oxidized sub- silicon and elemental lithium is subjected to mixing and ball milling and obtains pre-product；The pre-product high-temperature heat treatment obtains composite negative pole material.The present invention prepares integrated ear pole material with polyimides, substitutes copper foil by polyimides, improves copper interface and negative electrode material interface phase tolerance performance；Due to not adding macromolecule alite paste, negative electrode active material is directly contacted with polyimides, effectively increases electron-transport speed and electronic circulation stability.Solving existing tab from the root of material for preparing tab, there are the technical problems of electric conductivity difference.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of sub- silicon of oxidation and the compound tab material of polyimides
The preparation process of material.
Background technique
With the huge advance and fast development of information age, multifunctional portable electronic equipment, electric car, flight
More stringent requirements are proposed to energy storage material for the equipment such as device, artificial power-assisted.Therefore, height ratio capacity, high magnification, high security are researched and developed
Equal novel lithium batteries electrode material is extremely urgent.
Tab is a kind of raw material of lithium ion polymer battery product.Battery divides positive and negative anodes, and tab is exactly from electricity
The metallic conductor for extracting positive and negative anodes in core, the popular ear for saying battery positive and negative polarities are connecing when carrying out charge and discharge
Contact.
During the preparation process, high polymer binder need to be added in negative electrode material to existing tab in conjunction with copper foil, due to bonding
Agent is non-conductive polymer, hinders electronic conduction channel, reduces transmission speed, causes the electric conductivity of tab poor.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of systems for aoxidizing sub- silicon and the compound ear pole material of polyimides
Standby technique, solves the technical problem of existing tab electric conductivity difference.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of preparation process aoxidizing sub- silicon and the compound ear pole material of polyimides, specifically includes the following steps:
Prepare cellular porous polyimides；
Prepare nano oxidized sub- silicon；
The inorganic compound progress mixing and ball milling of the porous polyimide, nano oxidized sub- silicon and elemental lithium is obtained pre-
Product；
The pre-product high-temperature heat treatment obtains composite negative pole material.
Preferably, the specific steps for preparing cellular porous polyimides are as follows:
S1-1: with pyromellitic acid anhydride, 4,4 '-diaminodiphenyl ethers, dimethyl acetamide, -2 pyrrolidines of N- methyl
Ketone, fluorine compounds are that raw material dissolves under nitrogen protection；
S1-2: the solution that the step S1-1 is obtained is added polystyrene, stirs under nitrogen protection and the 2-10h that flows back；
S1-3: the solution after leading to the step S1-2 reflux is prepared into 25~100 μm of film by injection-calendering formation,
It is dry at 40-80 DEG C；
S1-4: carrying out graphitization processing for film of the step S1-3 after dry, and treatment temperature is 2500~3000 DEG C, is protected
Warm 5-10h.
Preferably, which is characterized in that the specific steps for preparing nano oxidized sub- silicon are as follows:
S2-1: HIGH-PURITY SILICON and the sub- silicon mixing and ball milling of oxidation obtain mixing and ball milling powder, the condition of the ball milling are as follows: and ball milling 8~
10h, ball-milling medium are zirconium oxide；
S2-2: for the step S2-1 mixing and ball milling powder under atmosphere protection, 600~1200 DEG C sinter the sub- silicon of oxidation into；
S2-3: the step S2-2 fires to obtain and aoxidizes sub- silicon powder and heat in high temperature furnace, is received by powder by spraying equipment
Integrate as nanometer powder；
Wherein, the warm temperature of the step S2-3 high temperature furnace is 60~400 DEG C, and spraying medium is argon gas.
Preferably, the inorganic compound mixing and ball milling of the porous polyimide, nano oxidized sub- silicon and elemental lithium obtains
The specific steps of pre-product are as follows:
Take the inorganic compound of elemental lithium, carbon source material, absolute alcohol, zirconium oxide balls and nano oxidized sub- silicon, porous
Polyimides mixing and ball milling.
Preferably, the inorganic compound of the elemental lithium is one of lithium metasilicate, lithium carbonate, lithium halide, lithium nitrate
Or it is a variety of.
Preferably, the carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, petroleum, peanut, pitch, graphite, powder
One of cake is a variety of.
Preferably, the mass ratio of each component are as follows: the inorganic compound of elemental lithium is 1~20 part, carbon source material 1~10
Part, nano oxidized sub- silicon: 5~30 parts, 2~20 parts of porous polyimide.
Preferably, the pre-product high-temperature heat treatment specific steps:
It is sintered in the environment of protective gas, under vacuum condition.
Preferably, the protective gas is nitrogen or argon gas, and vacuum degree is 50~1000pa.
(3) beneficial effect
The present invention provides a kind of preparation processes for aoxidizing sub- silicon and the compound ear pole material of polyimides.With prior art phase
Than, have it is following the utility model has the advantages that
The present invention prepares integrated ear pole material with polyimides, substitutes copper foil by polyimides, improves copper interface
With negative electrode material interface phase tolerance performance；Due to not adding macromolecule alite paste, negative electrode active material is directly contacted with polyimides,
Effectively increase electron-transport speed and electronic circulation stability.Solves existing pole from the root of material for preparing tab
There are the technical problems of electric conductivity difference for ear.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is cellular porous polyimides scanning figure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, to the technology in the embodiment of the present invention
Scheme is clearly and completely described, it is clear that and described embodiments are some of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
The embodiment of the present application by providing a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides, due to
It is existing in the preparation process of negative electrode material tab, negative electrode material need to be added high polymer binder in conjunction with copper foil, and binder
For non-conductive polymer, electronic conduction channel is hindered, transmission speed is reduced；Simultaneously because macromolecule adhesive property is with electronics
Transmission and copper interface and negative electrode material interface compatibility difference influence, affect circulating battery stability and capacity.Therefore existing
With the presence of tab electric conductivity difference technical problem.
Technical solution in the embodiment of the present application is to solve the problems, such as above-mentioned crosstalk, and general thought is as follows: sub- using polyamides
Amine substitutes copper foil, improves copper interface and negative electrode material interface phase tolerance performance；Due to not adding macromolecule alite paste, cathode is living
Property object is directly contacted with polyimides, effectively increases electron-transport speed and electronic circulation stability.From the material for preparing tab
Solving existing tab at the root of material, there are the technical problems of electric conductivity difference.
In order to better understand the above technical scheme, in conjunction with appended figures and specific embodiments to upper
Technical solution is stated to be described in detail.
A kind of preparation process aoxidizing sub- silicon and the compound ear pole material of polyimides, specifically includes the following steps:
Prepare cellular porous polyimides；
Prepare nano oxidized sub- silicon；
The inorganic compound progress mixing and ball milling of the porous polyimide, nano oxidized sub- silicon and elemental lithium is obtained pre-
Product；
The pre-product high-temperature heat treatment obtains composite negative pole material.
Integrated tab electrode material is prepared by above-mentioned technique, copper foil is substituted using polyimides, improves copper interface
With negative electrode material interface phase tolerance performance；Due to not adding macromolecule alite paste, negative electrode active material is directly contacted with polyimides,
Effectively increase electron-transport speed and electronic circulation stability.Solves existing pole from the root of material for preparing tab
There are the technical problems of electric conductivity difference for ear.
In specific implementation process, the specific steps for preparing cellular porous polyimides are as follows:
S1-1: with pyromellitic acid anhydride, 4,4 '-diaminodiphenyl ethers, dimethyl acetamide, -2 pyrrolidines of N- methyl
Ketone, fluorine compounds are that raw material dissolves under nitrogen protection；
S1-2: the solution that the step S1-1 is obtained is added polystyrene, stirs under nitrogen protection and the 2-10h that flows back；
The partial size of specific polystyrene is 50-200 nanometers, content 5wt%；
S1-3: the solution after leading to the step S1-2 reflux is prepared into 25~100 μm of film by injection-calendering formation,
It is dry at 40-80 DEG C；
S1-4: carrying out graphitization processing for film of the step S1-3 after dry, and treatment temperature is 2500~3000 DEG C, is protected
Warm 5-10h.
Fig. 1 is cellular porous polyimides scanning figure, it can be seen that porous polyimide, hole is 10-30 μm,
In class honeycomb, connected for three-dimensional network.
Cellular porous polyimides is prepared through the above steps, technical principle is that polystyrene is spherical macromolecule,
Simultaneously because it residual carbon is seldom when sintering at high temperature, leave porous structure after heat treatment volatilization, and PI (polyimides) is remained
Carbon is more, so porosity is higher；PI itself is polymer substance, in heat treatment, due to volatilizing and shrinking etc., in heat
Many Jie's micropores are left after processing.
In specific implementation process, the specific steps for preparing nano oxidized sub- silicon are as follows:
S2-1: HIGH-PURITY SILICON and the sub- silicon mixing and ball milling of oxidation obtain mixing and ball milling powder, the condition of the ball milling are as follows: and ball milling 8~
10h, ball-milling medium are zirconium oxide；Wherein HIGH-PURITY SILICON refers to that silicone content is greater than 99.5%；
S2-2: for the step S2-1 mixing and ball milling powder under atmosphere protection, 600~1200 DEG C sinter the sub- silicon of oxidation into；
S2-3: the step S2-2 fires to obtain and aoxidizes sub- silicon powder and heat in high temperature furnace, is received by powder by spraying equipment
Integrate as nanometer powder；
Wherein, the warm temperature of the step S2-3 high temperature furnace is 60~400 DEG C, and spraying medium is argon gas.
In specific implementation process, the inorganic compound mixing of the porous polyimide, nano oxidized sub- silicon and elemental lithium
Ball milling obtains the specific steps of pre-product are as follows:
Take inorganic compound, carbon source material, absolute alcohol, zirconium oxide balls and the nano oxidized sub- silicon, honeycomb of elemental lithium
Shape porous polyimide mixing and ball milling.
In specific implementation process, the inorganic compound of the elemental lithium is lithium metasilicate, lithium carbonate, lithium halide, lithium nitrate
One of or it is a variety of.Those skilled in the art also can choose other lithium base inorganic compounds.
In specific implementation process, the carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, petroleum, peanut, pitch,
One of graphite, muffin are a variety of.
In specific implementation process, the mass ratio of each component are as follows: the inorganic compound of elemental lithium is 1~20 part, carbon source
1~10 part of substance, nano oxidized sub- silicon: 5~30 parts, 2~20 parts of polyimides.By said ratio, help to expand from silicon
Aspect, it is ensured that the holding of silicon-carbon structure and the guarantee of circulating battery.
In specific implementation process, the pre-product high-temperature heat treatment specific steps:
It is sintered in the environment of protective gas, under vacuum condition.
In specific implementation process, the protective gas is nitrogen or argon gas, and vacuum degree is 50~1000pa.Wherein furnace internal pressure
Power is micro-positive pressure.
Below with reference to specific embodiment, it is described in detail:
Embodiment 1:
A kind of preparation process aoxidizing sub- silicon and the compound ear pole material of polyimides, specifically includes the following steps:
(1) cellular porous polyimides is prepared；
S1-1: with pyromellitic acid anhydride, 4,4 '-diaminodiphenyl ethers, dimethyl acetamide, -2 pyrrolidines of N- methyl
Ketone, fluorine compounds are that raw material dissolves under nitrogen protection；
S1-2: the solution that the step S1-1 is obtained is added polystyrene, stirs under nitrogen protection and the 2h that flows back；Tool
The polystyrene partial size of body is 50 nanometers, content 5wt%；
S1-3: the solution after leading to step S1-2 reflux is prepared into 25 μm of film by injection-calendering formation, at 40 DEG C
It is dry；
S1-4: carrying out graphitization processing for film of the step S1-3 after dry, and treatment temperature is 2500 DEG C, keeps the temperature 5h.
(2) nano oxidized sub- silicon is prepared；
S2-1: HIGH-PURITY SILICON and the sub- silicon mixing and ball milling of oxidation obtain mixing and ball milling powder, the condition of the ball milling are as follows: ball milling 8h,
Ball-milling medium is zirconium oxide；
S2-2: for the step S2-1 mixing and ball milling powder under atmosphere protection, 600 DEG C sinter the sub- silicon of oxidation into；
S2-3: the step S2-2 fires to obtain and aoxidizes sub- silicon powder and heat in high temperature furnace, and warm temperature is 60 DEG C；Pass through
Powder by spraying equipment is collected as nanometer powder, and specific spraying medium is argon gas.
(3) inorganic compound of the porous polyimide, nano oxidized sub- silicon and elemental lithium mixing and ball milling is carried out to obtain
To pre-product；Specific steps are as follows:
Take inorganic compound, carbon source material, absolute alcohol, zirconium oxide balls and the nano oxidized sub- silicon, honeycomb of elemental lithium
Shape porous polyimide mixing and ball milling.
Wherein the inorganic compound of elemental lithium be 1 part, 10 parts of carbon source material, nano oxidized sub- silicon: 5 parts, polyimides 20
Part.
(4) the pre-product high-temperature heat treatment obtains composite negative pole material, specific steps:
It is sintered in the environment of protective gas, under vacuum condition, the protective gas is nitrogen or argon gas, and vacuum degree is
50pa。
Embodiment 2:
A kind of preparation process aoxidizing sub- silicon and the compound ear pole material of polyimides, specifically includes the following steps:
(1) cellular porous polyimides is prepared；
S1-1: with pyromellitic acid anhydride, 4,4 '-diaminodiphenyl ethers, dimethyl acetamide, -2 pyrrolidines of N- methyl
Ketone, fluorine compounds are that raw material dissolves under nitrogen protection；
S1-2: the solution that the step S1-1 is obtained is added polystyrene, stirs under nitrogen protection and the 10h that flows back；Tool
The polystyrene partial size of body is 200 nanometers, content 5wt%；
S1-3: the solution after leading to step S1-2 reflux is prepared into 100 μm of film by injection-calendering formation, and 80 DEG C
Lower drying；
S1-4: carrying out graphitization processing for film of the step S1-3 after dry, and treatment temperature is 3000 DEG C, keeps the temperature 10h.
(2) nano oxidized sub- silicon is prepared；
S2-1: HIGH-PURITY SILICON and the sub- silicon mixing and ball milling of oxidation obtain mixing and ball milling powder, the condition of the ball milling are as follows: ball milling 10h,
Ball-milling medium is zirconium oxide；
S2-2: for the step S2-1 mixing and ball milling powder under atmosphere protection, 1200 DEG C sinter the sub- silicon of oxidation into；
S2-3: the step S2-2 fires to obtain and aoxidizes sub- silicon powder and heat in high temperature furnace, and warm temperature is 400 DEG C；It is logical
It crosses powder by spraying equipment and is collected as nanometer powder, specific spraying medium is argon gas.
(3) inorganic compound of the porous polyimide, nano oxidized sub- silicon and elemental lithium mixing and ball milling is carried out to obtain
To pre-product；Specific steps are as follows:
Take inorganic compound, carbon source material, absolute alcohol, zirconium oxide balls and the nano oxidized sub- silicon, honeycomb of elemental lithium
Shape porous polyimide mixing and ball milling.
Wherein the inorganic compound of elemental lithium be 20 parts, 1 part of carbon source material, nano oxidized sub- silicon: 30 parts, polyimides 2
Part.
(4) the pre-product high-temperature heat treatment obtains composite negative pole material, specific steps:
It is sintered in the environment of protective gas, under vacuum condition, the protective gas is nitrogen or argon gas, and vacuum degree is
1000pa。
Embodiment 3:
A kind of preparation process aoxidizing sub- silicon and the compound ear pole material of polyimides, specifically includes the following steps:
(1) cellular porous polyimides is prepared；
S1-1: with pyromellitic acid anhydride, 4,4 '-diaminodiphenyl ethers, dimethyl acetamide, -2 pyrrolidines of N- methyl
Ketone, fluorine compounds are that raw material dissolves under nitrogen protection；
S1-2: the solution that the step S1-1 is obtained is added polystyrene, stirs under nitrogen protection and the 2-10h that flows back；
Specific polystyrene partial size is 120 nanometers, content 5wt%；
S1-3: the solution after leading to step S1-2 reflux is prepared into 65 μm of film by injection-calendering formation, and 460 DEG C
Lower drying；
S1-4: carrying out graphitization processing for film of the step S1-3 after dry, and treatment temperature is 2800 DEG C, keeps the temperature 8h.
(2) nano oxidized sub- silicon is prepared；
S2-1: HIGH-PURITY SILICON and the sub- silicon mixing and ball milling of oxidation obtain mixing and ball milling powder, the condition of the ball milling are as follows: ball milling 9h,
Ball-milling medium is zirconium oxide；
S2-2: for the step S2-1 mixing and ball milling powder under atmosphere protection, 900 DEG C sinter the sub- silicon of oxidation into；
S2-3: the step S2-2 fires to obtain and aoxidizes sub- silicon powder and heat in high temperature furnace, and warm temperature is 230 DEG C；It is logical
It crosses powder by spraying equipment and is collected as nanometer powder, specific spraying medium is argon gas.
(3) inorganic compound of the porous polyimide, nano oxidized sub- silicon and elemental lithium mixing and ball milling is carried out to obtain
To pre-product；Specific steps are as follows:
Take inorganic compound, carbon source material, absolute alcohol, zirconium oxide balls and the nano oxidized sub- silicon, honeycomb of elemental lithium
Shape porous polyimide mixing and ball milling.
Wherein the inorganic compound of elemental lithium be 10 parts, 6 parts of carbon source material, nano oxidized sub- silicon: 17 parts, polyimides 11
Part.
(4) the pre-product high-temperature heat treatment obtains composite negative pole material, specific steps:
It is sintered in the environment of protective gas, under vacuum condition, the protective gas is nitrogen or argon gas, and vacuum degree is
500pa。
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (9)
1. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides, which is characterized in that specifically include following step
It is rapid:
Prepare cellular porous polyimides；
Prepare nano oxidized sub- silicon；
The inorganic compound of the porous polyimide, nano oxidized sub- silicon and elemental lithium is subjected to mixing and ball milling and obtains pre- production
Object；
The pre-product high-temperature heat treatment obtains composite negative pole material.
2. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides as described in claim 1, which is characterized in that
The specific steps for preparing cellular porous polyimides are as follows:
S1-1: with pyromellitic acid anhydride, 4,4 '-diaminodiphenyl ethers, dimethyl acetamide, -2 pyrrolidones of N- methyl, fluorine
Compound is that raw material dissolves under nitrogen protection；
S1-2: the solution that the step S1-1 is obtained is added polystyrene, stirs under nitrogen protection and the 2-10h that flows back；
S1-3: the solution after leading to the step S1-2 reflux is prepared into 25~100 μm of film, 40-80 by injection-calendering formation
It is dry at DEG C；
S1-4: carrying out graphitization processing for film of the step S1-3 after dry, and treatment temperature is 2500~3000 DEG C, keeps the temperature 5-
10h。
3. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides as described in claim 1, which is characterized in that
The specific steps for preparing nano oxidized sub- silicon are as follows:
S2-1: HIGH-PURITY SILICON and the sub- silicon mixing and ball milling of oxidation obtain mixing and ball milling powder, the condition of the ball milling are as follows: 8~10h of ball milling,
Ball-milling medium is zirconium oxide；
S2-2: for the step S2-1 mixing and ball milling powder under atmosphere protection, 600~1200 DEG C sinter the sub- silicon of oxidation into；
S2-3: the step S2-2 fires to obtain and aoxidizes sub- silicon powder and heat in high temperature furnace, is collected as by powder by spraying equipment
Nanometer powder；
Wherein, the warm temperature of the step S2-3 high temperature furnace is 60~400 DEG C, and spraying medium is argon gas.
4. the preparation process as described in claim 1 for aoxidizing sub- silicon and the compound ear pole material of polyimides, which is characterized in that institute
The inorganic compound mixing and ball milling for stating porous polyimide, nano oxidized sub- silicon and elemental lithium obtains the specific steps of pre-product
Are as follows:
Take inorganic compound, carbon source material, absolute alcohol, zirconium oxide balls and the nano oxidized sub- silicon, porous polyamides of elemental lithium
Imines mixing and ball milling.
5. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides as claimed in claim 4, which is characterized in that
The inorganic compound of the elemental lithium is one of lithium metasilicate, lithium carbonate, lithium halide, lithium nitrate or a variety of.
6. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides as claimed in claim 4, which is characterized in that
The carbon source material are as follows: resin, glucose, carbohydrate, fatty acid, one of petroleum, peanut, pitch, graphite, muffin or more
Kind.
7. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides as claimed in claim 4, which is characterized in that
The mass ratio of each component are as follows: the inorganic compound of elemental lithium is 1~20 part, 1~10 part of carbon source material, nano oxidized Asia
Silicon: 5~30 parts, 2~20 parts of porous polyimide.
8. a kind of preparation process for aoxidizing sub- silicon and the compound ear pole material of polyimides as described in claim 1, which is characterized in that
The pre-product high-temperature heat treatment specific steps:
It is sintered in the environment of protective gas, under vacuum condition.
9. the preparation process as claimed in claim 8 for aoxidizing sub- silicon and polyimides composite negative pole material, which is characterized in that institute
Stating protective gas is nitrogen or argon gas, and vacuum degree is 50~1000pa.
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| CN111792646A (en) * | 2020-07-21 | 2020-10-20 | 苏州华赢新能源材料科技有限公司 | Polyimide modified nano silicon negative electrode material and preparation method and application thereof |
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