CN110459720A - A kind of preparation method of lignin-oxide ceramic coating - Google Patents
A kind of preparation method of lignin-oxide ceramic coating Download PDFInfo
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- CN110459720A CN110459720A CN201910603052.0A CN201910603052A CN110459720A CN 110459720 A CN110459720 A CN 110459720A CN 201910603052 A CN201910603052 A CN 201910603052A CN 110459720 A CN110459720 A CN 110459720A
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- lignin
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- ceramic coating
- colloidal sol
- oxide ceramic
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
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- 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
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- Electrochemistry (AREA)
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- Manufacturing & Machinery (AREA)
- Cell Separators (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of preparation methods of lignin-oxide ceramic coating, belong to lithium ion battery preparation technical field, weigh 8-10g aluminium isopropoxide and are dissolved in 140-160mL deionized water；Solution ph is adjusted to using dust technology to obtain stable transparent colloidal sol at 4,70-90 DEG C after magnetic agitation；By colloidal sol as in 80-100 DEG C of vacuum save 11-13h after be used for impreg carbon powder；Sonic oscillation 0.5-1.5h first, is subsequently placed in 23-25h in vacuum when dipping；Extra colloidal sol is removed using device is filtered, the rape straw charcoal after dipping is 1-2 days dry at 100 DEG C, 2-4h is sintered at 100 DEG C -600 DEG C；By preparation-obtained lignin three-dimensional micropore composite ceramic material with prepare obtained PE diaphragm through wet processing and carry out compound, ceramic coating is prepared.The present invention can effectively improve the security performance and high rate performance of lithium-ion-power cell.
Description
Technical field
The invention belongs to lithium ion battery preparation technical fields, are related to a kind of preparation of lignin-oxide ceramic coating
Method.
Background technique
Lithium ion battery during the preparation process, needs to synthesize template.Timber is both with complex shape natural with form
Composite material, while being the organic combination from micro-scale (cell) to macro-scale (skeleton) again.From the point of view of chemically forming,
Timber is mainly made of cellulose, hemicellulose, lignin and a small amount of inorganic constituents.Lignin is that three kinds of benzene oxide units pass through
The boiomacromolecule with tridimensional network that ehter bond and carbon-carbon bond are interconnected to form, is present in lignum, mainly
Effect is by forming intertexture net come sclereid wall, is secondary wall main component.Lignin be predominantly located at cellulose fibre it
Between, play resistance to compression.In xylophyta, lignin accounts for 25%, is that (cellulose is the most abundant organic matter of second in the world
First).
In currently available technology, there are no a kind of preparation methods of lignin-oxide ceramic coating.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of lignin-oxide ceramic coating, this method uses gas
Atmosphere sintering process prepares multi-stage porous rape straw base cellulose template material, explores point in different sintering process lower die plate material apertures
Cloth optimizes sintering process；The type and quantity for studying rape straw sill quality surface functional group under different sintering conditions, by excellent
Change sintering process, realizes the regulation to functional group；It remains with and is conducive to improve the functional group in conjunction with basement membrane.It will be preparation-obtained
Lignin three-dimensional micropore composite ceramic material with prepare obtained PE diaphragm through wet processing and carry out compound, ceramics are prepared
Coating.
Itself the specific technical proposal is:
A kind of preparation method of lignin-oxide ceramic coating, comprising the following steps:
Step 1 weighs 8-10g aluminium isopropoxide and is dissolved in 140-160mL deionized water；Solution ph is adjusted to 4 using dust technology,
Stable transparent colloidal sol is obtained at 70-90 DEG C after magnetic agitation；
Step 2, by colloidal sol as in 80-100 DEG C of vacuum save 11-13h after be used for impreg carbon powder；
Sonic oscillation 0.5-1.5h first when step 3, dipping, is subsequently placed in 23-25h in vacuum；
Step 4 removes extra colloidal sol using filtering device, and the rape straw charcoal after dipping is 1-2 days dry at 100 DEG C, 100
2-4h is sintered at DEG C -600 DEG C, heating rate is 5 DEG C/min；By preparation-obtained lignin three-dimensional micropore composite ceramic material
It carries out compound with obtained PE diaphragm is prepared through wet processing, ceramic coating is prepared.
Further, step 1 specifically: weigh 9g aluminium isopropoxide and be dissolved in 150mL deionized water；Using dust technology by solution
PH value is adjusted to obtain stable transparent colloidal sol at 4,80 DEG C after magnetic agitation
Further, step 2 specifically: by colloidal sol as in 90 DEG C of vacuum save 12h after be used for impreg carbon powder.
Further, step 3 specifically: sonic oscillation 1h first when dipping is subsequently placed in vacuum for 24 hours.
Further, in step 4,1 day drying time.
Further, in step 4,3h is sintered at 350 DEG C.
Compared with prior art, the invention has the benefit that
The present invention will be closed using the rape straw base biomaterial of three-D pore structure as templated synthesis lignin-oxide ceramic coating
At with hierarchical porous structure and lignin-oxide ceramic coating containing a large amount of functional groups is as lithium-ion power battery dissepiment
The modified coating of material；Electrolysis is improved to increase the specific surface area of diaphragm material by the structure for controlling three-dimensional netted porous grade
The affinity of liquid diaphragm material effectively solves commercial polyolefin class diaphragm or normal to improve diaphragm to the compatibility of electrolyte
Advise ceramic-coated separator performance deficiency, resistance to high current charge-discharge, reduce electrode in terms of improvement lithium from
The chemical property of sub- power battery, to improve the security performance and high rate performance of lithium-ion-power cell.
Detailed description of the invention
Fig. 1 conventional polyolefin diaphragm electromicroscopic photograph；
Fig. 2 composite coating diaphragm electromicroscopic photograph；
The comparison of Fig. 3 difference diaphragm cell cycle life；
The comparison of the high voltage withstanding performance of Fig. 4 difference diaphragm.
Specific embodiment
Technical solution of the present invention is described in more detail combined with specific embodiments below.
Embodiment 1
A kind of preparation method of lignin-oxide ceramic coating, comprising the following steps:
Step 1 weighs 8g aluminium isopropoxide and is dissolved in 140mL deionized water；Solution ph is adjusted at 4,70 DEG C using dust technology
Stable transparent colloidal sol is obtained after magnetic agitation；
Step 2, by colloidal sol as in 80 DEG C of vacuum save 13h after be used for impreg carbon powder；
Sonic oscillation 0.5h first when step 3, dipping, is subsequently placed in 25h in vacuum；
Step 4 removes extra colloidal sol using filtering device, and the rape straw charcoal after dipping is 1 day dry at 100 DEG C, at 100 DEG C
4h is sintered at DEG C, heating rate is 5 DEG C/min；By preparation-obtained lignin three-dimensional micropore composite ceramic material and through wet process
Technique prepares obtained PE diaphragm and carries out compound, and ceramic coating is prepared.
Embodiment 2
It weighs 9g aluminium isopropoxide to be dissolved in 150mL deionized water, solution ph is adjusted to magnetic force at 4,80 DEG C using dust technology and is stirred
Stable transparent colloidal sol is obtained after mixing.By colloidal sol as in 90 DEG C of vacuum save 12h after be used for impreg carbon powder.When dipping first
Sonic oscillation 1h is subsequently placed in vacuum for 24 hours.Extra colloidal sol is removed using device is filtered, by the rape straw charcoal after dipping in 100
It is 1 day dry at DEG C, 3h is sintered at 100 DEG C -600 DEG C, heating rate is 5 DEG C/min；Preparation-obtained lignin is three-dimensional
Micropore composite ceramic material with prepare obtained PE diaphragm through wet processing and carry out compound, ceramic coating is prepared.
Embodiment 3
Step 1 weighs 10g aluminium isopropoxide and is dissolved in 160mL deionized water；Solution ph is adjusted to 4,90 DEG C using dust technology
Stable transparent colloidal sol is obtained after lower magnetic agitation；
Step 2, by colloidal sol as in 100 DEG C of vacuum save 11h after be used for impreg carbon powder；
Sonic oscillation 1.5h first when step 3, dipping, is subsequently placed in 2h in vacuum；
Step 4 removes extra colloidal sol using filtering device, and the rape straw charcoal after dipping is 2 days dry at 100 DEG C, at 600 DEG C
Lower sintering 2h, heating rate are 5 DEG C/min；By preparation-obtained lignin three-dimensional micropore composite ceramic material and through wet process work
Skill prepares obtained PE diaphragm and carries out compound, and ceramic coating is prepared.
Embodiment 4
By preparation-obtained lignin three-dimensional micropore composite ceramic material with through wet processing prepare obtained PE diaphragm into
Row is compound, and ceramic coating is prepared.Prepared sample is analyzed using electron microscope.Fig. 1 is current wet processing preparation
Conventional polyolefin diaphragm electromicroscopic photograph, Fig. 2 is the present invention using new material prescription, the compound painting of new technology preparation
Layer diaphragm electromicroscopic photograph, it can be seen that lithium ion battery wet process diaphragm has the uniform micro point of consistency in electromicroscopic photograph
The microstructure of cloth, lithium ion battery separator shows grid configuration.
It is quite uniform from the micropore distribution that can be seen that wet process diaphragm Electronic Speculum profile in Fig. 2 in microcosmic electron microscope, and have
Certain regularity, the details profile of micropore is more clear as it can be seen that the netted connection in electron microscopic picture is more regular, and layer
It is secondary high-visible, no blind hole, no agglomerate.
5 composite ceramics diaphragm electrochemical performance characterization of embodiment
The lignin three-dimensional micropore structure composite ceramic diaphragm material of preparation and routine PE diaphragm material are pressed into same process respectively
Be assembled into 18650 size battery of battery, and carry out electrochemistry cycle performance test, test condition be in 1.0C, 1.1C, 1.3C,
It discharges under the conditions of 1.5C, 2.0C.Fig. 3 is the cycle-index of this material and common PE under different discharge-rates.From figure
As can be seen that composite ceramics diaphragm and routine PE are at 1000 times under the different condition of the big multiplying power of 2.0C and 1.3C and small multiplying power
After circulation, the gap of battery capacity conservation rate is larger, and the battery capacity of routine PE diaphragm is average in battery appearance after cycling
Conservation rate is measured 90% or so, and the capacitance conservation rate of routine PE diaphragm material is 80% or so, while its rate of decay is far high
In the battery that composite ceramics diaphragm material is assembled.
The 6 high voltage withstanding performance characterization of composite ceramics diaphragm of embodiment
The lignin three-dimensional micropore composite ceramics diaphragm material of preparation and routine PE diaphragm material are pressed into same process assembling respectively
At 18650 size battery of battery, and carry out electrochemistry cycle performance test, test condition be in 4.5V and 4.3V voltage platform,
It discharges under the conditions of 2.0C, detects the rate of decay and capacity retention ratio of battery, test data is as shown in Figure 4.It can from Fig. 4
To find out, using the battery of lignin three-dimensional micropore composite ceramics diaphragm preparation under the conditions of high-voltage state, big multiplying power discharging
Capacity retention ratio it is relatively stable, 1000 times circulation after, capacity retention ratio reaches 92% or so, and routine PE diaphragm material exists
Under the conditions of high voltage high-multiplying power discharge, capacity attenuation is rapid, and after 600 circulations, capacity retention ratio has been lower than 50%, is passing through
After 1000 circulations, battery reaches failure state.
The foregoing is only a preferred embodiment of the present invention, the scope of protection of the present invention is not limited to this, it is any ripe
Know those skilled in the art within the technical scope of the present disclosure, the letter for the technical solution that can be become apparent to
Altered or equivalence replacement are fallen within the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of lignin-oxide ceramic coating, which comprises the following steps:
Step 1 weighs 8-10g aluminium isopropoxide and is dissolved in 140-160mL deionized water；Solution ph is adjusted to 4 using dust technology,
Stable transparent colloidal sol is obtained at 70-90 DEG C after magnetic agitation；
Step 2, by colloidal sol as in 80-100 DEG C of vacuum save 11-13h after be used for impreg carbon powder；
Sonic oscillation 0.5-1.5h first when step 3, dipping, is subsequently placed in 23-25h in vacuum；
Step 4 removes extra colloidal sol using filtering device, and the rape straw charcoal after dipping is 1-2 days dry at 100 DEG C, 100
2-4h is sintered at DEG C -600 DEG C, heating rate is 5 DEG C/min；By preparation-obtained lignin three-dimensional micropore composite ceramic material
It carries out compound with obtained PE diaphragm is prepared through wet processing, ceramic coating is prepared.
2. the preparation method of lignin-oxide ceramic coating according to claim 1, which is characterized in that step 1 is specific
Are as follows: it weighs 9g aluminium isopropoxide and is dissolved in 150mL deionized water；Solution ph is adjusted to magnetic agitation at 4,80 DEG C using dust technology
After obtain stable transparent colloidal sol.
3. the preparation method of lignin-oxide ceramic coating according to claim 1, which is characterized in that step 2 is specific
Are as follows: by colloidal sol as in 90 DEG C of vacuum save 12h after be used for impreg carbon powder.
4. the preparation method of lignin-oxide ceramic coating according to claim 1, which is characterized in that step 3 is specific
Are as follows: sonic oscillation 1h first when dipping is subsequently placed in vacuum for 24 hours.
5. the preparation method of lignin-oxide ceramic coating according to claim 1, which is characterized in that in step 4,
1 day drying time.
6. the preparation method of lignin-oxide ceramic coating according to claim 1, which is characterized in that in step 4,
3h is sintered at 350 DEG C.
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| CN201910603052.0A CN110459720A (en) | 2019-07-05 | 2019-07-05 | A kind of preparation method of lignin-oxide ceramic coating |
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| CN201910603052.0A CN110459720A (en) | 2019-07-05 | 2019-07-05 | A kind of preparation method of lignin-oxide ceramic coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592379A (en) * | 2020-06-15 | 2020-08-28 | 深圳市万泽中南研究院有限公司 | Preparation method of ceramic core coating based on dipping freeze drying technology |
| CN111933878A (en) * | 2020-07-06 | 2020-11-13 | 东莞市创明电池技术有限公司 | Lithium ion battery diaphragm and preparation method and application thereof |
-
2019
- 2019-07-05 CN CN201910603052.0A patent/CN110459720A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592379A (en) * | 2020-06-15 | 2020-08-28 | 深圳市万泽中南研究院有限公司 | Preparation method of ceramic core coating based on dipping freeze drying technology |
| CN111933878A (en) * | 2020-07-06 | 2020-11-13 | 东莞市创明电池技术有限公司 | Lithium ion battery diaphragm and preparation method and application thereof |
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