CN102735599B - The method measuring cell structure distribution of pores - Google Patents
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- CN102735599B CN102735599B CN201210207296.5A CN201210207296A CN102735599B CN 102735599 B CN102735599 B CN 102735599B CN 201210207296 A CN201210207296 A CN 201210207296A CN 102735599 B CN102735599 B CN 102735599B
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Abstract
The invention discloses a kind of method measuring cell structure distribution of pores, the steps include: to be filled in cell structure the product that the Organic substance containing characteristic element hydrolyzes in acid/base environment and brittle failure, expose cross section, electron scattering energy disperse spectroscopy is used to gather characteristic element distribution on cross section, utilize computer image analysis and processing method to calculate characteristic element occupied area and the ratio with the gross area thereof, obtain the distribution of specific location pore-size distribution and porosity.The present invention can be widely applied to the sign of cell structure mesopore distribution, the method that the present invention provides can have great importance with characterization processes process and electrochemical process for the impact of loose structure in lithium ion cell electrode sheet for Optimizing Process Parameters and electrochemical process parameter.
Description
Technical field
The present invention relates to the measurement of cell structure distribution of pores, especially one is quick, simply measure lithium-ion electric
The method of the electrode slice mesopore distributed in three dimensions in pond.
Background technology
Lithium ion battery, as the electrochmical power source of a kind of high-energy-density, plays in the fields such as present mobile communication equipment
Irreplaceable effect.Along with the quick growth to lithium ion battery demand of the emerging fields such as electric automobile and energy storage,
The most urgent to the lithium ion battery cathode of high-energy-density and the demand of anode material.Meanwhile, based on existing negative electrode and sun
The design optimization of the electrodes of lithium-ion batteries of pole material becomes the means improving battery energy density the most already, and thick electrode technology is i.e.
For one of them important channel.
Generally, the pole piece of lithium ion battery is constituted main structure body by active substance, conductive agent, dispersant and bonding agent, with
Time in this main structure body, be dispersed with continuous print pore structure, be filled with for electrolyte.Owing to electrolyte is that lithium ion exists
Migrating essential carrier between negative electrode and anode, therefore the pore structure of pole piece has important for the migration of lithium ion
Impact, electrode slice especially high to compacted density, that thickness is big is all the more so.Additionally, lithium ion battery use during, lithium from
The sub embedding at anode strip can cause the expansion of anode, causes its pore structure to change so that the locally electrolysis in hole
Liquid loading is inadequate, causes the phenomenon of cyclic process capacity sharp-decay.Therefore, the pore structure of quantitatively characterizing electrode slice for
In the design of battery pole piece and analysis cyclic process, the change of battery performance, the most significant.
Measuring currently for the hole including the cell structures such as lithium ion cell electrode sheet mainly uses mercury injection method to enter
OK, the method can obtain pore-size distribution and the porosity of cell structure to be measured, but cannot obtain cell structure mesopore
The two dimension of structure or distributed in three dimensions result.Refer to the distinct electrodes of lithium-ion batteries of two shown in Fig. 1 and Fig. 2 kind (figure
In 10,20 be collector, 12,22 is porous membrane, and 14,24 is hole), the knot that its pore structure obtains when measuring by mercury injection method
The most just the same.But, both pore structures but have opposite impacts on for the migration of lithium ion, preferable pore structure
Should be the inverted trapezoidal structure shown in Fig. 1, it be conducive to electrolyte to be substantially filled in hole, it is simple to quickly moving of lithium ion
Move.Visible, mercury injection method cannot meet the hole measurement demand of lithium ion cell electrode sheet, and necessary searching one can be accurate
The method of the internal various location distribution of pores of measuring electrode sheet.
Summary of the invention
It is an object of the invention to: a kind of method measuring cell structure distribution of pores is provided, to realize porous is tied
The convenient, fast measurement of various location distribution of pores in structure body.
In order to realize foregoing invention purpose, the invention provides a kind of method measuring cell structure distribution of pores, its
Comprise the following steps: prepare a kind of flowing material containing characteristic element；Prepared flowing material is filled into be measured many
In the pore structure of pore structure body；Make brittle failure after being soaked in liquid nitrogen by populated cell structure to process, use electronics to dissipate
Penetrate the EDS maps of characteristic element on energy disperse spectroscopy detection loose structure body section；Use computer image analysis method, to being obtained
Characteristic element mapping picture on section do gray processing and process, equidistantly divide along specific direction simultaneously, calculate
Characteristic element area and account for the ratio of the gross area in each equidistant bar-shaped zone, as pore-size distribution and porosity point
Cloth.
Compared with prior art, the present invention can be calculated the aperture of cell structure according to the distribution of characteristic element and divides
Cloth and the Two dimensional Distribution of pore structure, and then the two-dimensional result of the distribution of pores of comprehensive diverse location, calculate and reconstruct porous
The distributed in three dimensions of structure mesopore structure.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, the viscosity of described flowing material is
5～15mPa S.Owing to flowing material has low surface tension, good mobility, porous knot therefore can be easily packed into
In the pore structure of structure, it can be little to tens nanometers, arrive grade greatly with the aperture of filling pore, it is ensured that the essence of distribution of pores
Really measure.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described flowing material can be
It is filled within 10s in the pore structure of cell structure to be measured.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described flowing material is in atmosphere
Can solidify in 1 hour, and after solidification, volume will not shrink and expand.Owing to flowing material does not has during solidification
Having along with the stress produced due to volumetric expansion, will not destroy pore structure to be measured, meanwhile, flowing material is in solidification
During do not occur volume contraction can ensure that filler has accurate replication performance for pore structure, it is ensured that special
Levy element distribution in pore structure and can truly reflect pore structure characteristic and distribution of pores.
A kind of improvement of the method for cell structure distribution of pores, described populated loose structure is measured as the present invention
Body soak time in liquid nitrogen is 5～20 minutes, and brittle failure on the sharp keen edge of a knife after taking out from liquid nitrogen, to obtain surfacing
Fracture be easy to measure.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described characteristic element is can be by
Electron scattering detection of energy spectrometer and be not present in the element in cell structure to be measured.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described flowing material is Organic substance
The hydrolyzate that hydrolysis obtains.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described characteristic element is silicon, institute
Stating flowing material is that siloxanes hydrolyzes the polysiloxane hydrolyzate obtained in an acidic solution.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described cell structure be lithium from
Sub-cathode sheets or anode strip.
Measure a kind of improvement of the method for cell structure distribution of pores as the present invention, described cell structure is for passing through
Lithium-ion cathode sheet after roll-in or chemical conversion or circulation or anode strip.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings and detailed description of the invention, the present invention is measured the method for cell structure distribution of pores and has
Benefit effect is described in detail, wherein:
Fig. 1 and Fig. 2 is the schematic diagram of the pore structure of two kinds of distinct electrodes of lithium-ion batteries.
Fig. 3 is that the anode sheet of lithium ion battery of the embodiment of the present invention 2 fills after polysiloxane hydrolyzate that on cross section the face of silicon
Distribution (a) and scanning electron microscope microstructure (b) of correspondence.
Fig. 4 a is the distribution of the porosity through-thickness that in Fig. 3 a, Si distributed image obtains after treatment, and Fig. 4 b is for using
The porosity that mercury injection method is measured.
Detailed description of the invention
One, the hydrolyzate of siloxanes is prepared: take the clean beaker of a 100ml, a magnetic stick standby.First configure
The dilute nitric acid solution of 1M concentration, pipettes 10～20ml dilute nitric acid solutions in the clean beaker of 100ml with pipet, with accurately control
It is the silicone liquid of 99.9% that the liquid-transfering gun of volume processed adds 10～40 grams of purity in beaker, controls dust technology and siloxanes
Mass ratio be 0.2～2, sealed beaker carries out magnetic agitation at normal temperatures, and speed of agitator is 500～1500rpm.Stir 10 points
Zhong Hou, the solution of original layering becomes clarification, and walls of beaker has obvious fever phenomenon, stops stirring.The test viscosity of hydrolyzed liquid
It is 5～15mPa S.
Two, the hole of filling porous structure: get cell structure thin slice ready, draws with the liquid-transfering gun accurately controlling volume
0.1ml hydrolyzate drops in the middle of thin slice to be measured, hydrolyzate in 10s at the complete drawout of pole piece, penetrate into pole
In sheet.
Three, element silicon distributed image gathers and image analysis processing: soaked in liquid nitrogen 5～20 minutes by above-mentioned thin slice,
Brittle failure on the sharp keen edge of a knife after taking-up.Section, at surface sweeping electricity Microscopic observation, uses electron scattering energy disperse spectroscopy to collect element silicon signal
And draw out the EDS maps of element silicon.The silicon distributed image drawn equidistantly is divided into 5～100 equal portions along thickness direction,
Use computer image analysis, with processing software, the image stick of each equal portions is carried out binary conversion treatment so that on image only
Two kinds of colors of black and white, calculate the area shared by the black region representing silicon content by pixels statistics method and account for total face
Long-pending ratio, obtains pore-size distribution and the porosity distribution of ad-hoc location.The rest may be inferred, obtains the two-dimentional aperture along thickness direction
Distribution and porosity distribution.
More accurately, use said method, the area of element silicon distributed areas can be obtained and account for total image area
The two-dimensional matrix result of ratio, the numerical value that the row and column of matrix comprises is the most, and the Two dimensional Distribution of obtained pore structure is the most smart
Really.
Below with reference to specific embodiment, the present invention is measured the method work of cell structure distribution of pores the most in detail
Description, but embodiments of the invention are not limited to this.
Embodiment 1
Take the clean beaker of a 100ml, a magnetic stick standby.First configure the dilute nitric acid solution of 1M concentration, with shifting
Liquid pipe pipettes 12ml dilute nitric acid solution in the clean beaker of 100ml, adds in beaker with the liquid-transfering gun accurately controlling volume
17 grams of purity are the silicone liquid of 99.9%, and dust technology is 0.7 with the mass values of siloxanes, and sealed beaker enters at normal temperatures
Row magnetic agitation, speed of agitator is 1000rpm.After stirring 5 minutes, obtain the hydrolyzate of clarification.
Cathode plate of lithium ion battery to be measured is dried, draws 0.05ml hydrolysis with the liquid-transfering gun accurately controlling volume and produce
Thing drops in the middle of pole piece to be measured, and hydrolyzate rapidly permeates in pole piece.
Above-mentioned cathode sheets is soaked 10 minutes in liquid nitrogen, brittle failure after taking-up.Electron scattering energy disperse spectroscopy is used to collect section
The EDS maps of upper element silicon, is equidistantly divided into 10 equal portions to the element silicon image collected along thickness direction, uses business
Computer image analysis carries out binary conversion treatment with processing software to the image stick of each equal portions so that only have black and white on image
Two kinds of colors, calculate and represent the area shared by white portion of silicon content and account for the ratio of the gross area, obtain ad-hoc location
Aperture and porosity distribution.The rest may be inferred, obtains the two-dimentional porosity distribution along thickness direction.
Embodiment 2
Take the clean beaker of a 100ml, a magnetic stick standby.First configure the dilute nitric acid solution of 1M concentration, with shifting
Liquid pipe pipettes 12ml dilute nitric acid solution in the clean beaker of 100ml, adds in beaker with the liquid-transfering gun accurately controlling volume
17 grams of purity are the silicone liquid of 99.9%, and sealed beaker carries out magnetic agitation at normal temperatures, and speed of agitator is 1000rpm.
After stirring 5 minutes, obtain the hydrolyzate of clarification.
Anode sheet of lithium ion battery to be measured is dried, draws 0.05ml hydrolysis with the liquid-transfering gun accurately controlling volume and produce
Thing drops in the middle of pole piece to be measured, and hydrolyzate rapidly permeates in pole piece.
Above-mentioned cathode sheets is soaked 5 minutes in liquid nitrogen, brittle failure after taking-up.Electron scattering energy disperse spectroscopy is used to collect on section
The EDS maps of element silicon.The element silicon image collected equidistantly is divided into 20 equal portions along thickness direction, uses business meter
Calculation machine computer assisted image processing software carries out binary conversion treatment to the image stick of each equal portions so that only have black and white two on image
Plant color, calculate and represent the area shared by white portion of silicon content and account for the ratio of the gross area, obtain ad-hoc location
Aperture and porosity distribution.The rest may be inferred, two-dimentional distribution of pores along thickness direction in pole piece after being dried.
Embodiment 3
Prepare the hydrolyzate of siloxanes according to the method in embodiment 1, wherein, dust technology volume is 20ml, and purity is
The siloxanes quality of 99.9% is 10 grams, and dust technology is 2 with the mass ratio of siloxanes, and uses method same as in Example 1
Calculate anode sheet of lithium ion battery after roll-in along the aperture of thickness direction and porosity distribution.
Embodiment 4
Preparing polysiloxane hydrolyzate according to the method in embodiment 1, wherein speed of agitator is 800rpm, and uses with real
Execute the identical method of example 1 to calculate the anode sheet of lithium ion battery after roll-in and divide along aperture and the porosity of thickness direction
Cloth.
Embodiment 5
Prepare polysiloxane hydrolyzate according to the method for embodiment 1, and use method same as in Example 1 to calculate process
Anode sheet of lithium ion battery after roll-in is along the aperture of thickness direction and porosity distribution.
Embodiment 6
Prepare polysiloxane hydrolyzate according to the method for embodiment 1, and use method same as in Example 1 to calculate process
Cathode plate of lithium ion battery after roll-in is along the aperture of thickness direction and porosity distribution.
Embodiment 7
Polysiloxane hydrolyzate is prepared according to the method for embodiment 1；Disassemble the lithium ion battery after chemical conversion, take a piece of anode
Sheet cleans 3 times in dimethyl carbonate solvent, dries after each one minute, uses method same as in Example 1 to calculate and passes through
Pole piece after chemical conversion treatment is along the aperture of thickness direction and porosity distribution.
Embodiment 8
Polysiloxane hydrolyzate is prepared according to the method for embodiment 1；Disassemble the lithium ion battery after chemical conversion, take a piece of negative electrode
Sheet cleans 3 times in dimethyl carbonate solvent, dries after each one minute, uses method same as in Example 1 to calculate and passes through
Pole piece after chemical conversion treatment is along the aperture of thickness direction and porosity distribution.
Embodiment 9
Polysiloxane hydrolyzate is prepared according to the method for embodiment 1；Disassemble the lithium ion battery after 1000 circulations,
Take a piece of anode strip in dimethyl carbonate solvent, to clean 5 times, dry after each one minute, use side same as in Example 1
Method calculates and expands pole piece along the aperture of thickness direction and porosity distribution after circular treatment.
Embodiment 10
Polysiloxane hydrolyzate is prepared according to the method for embodiment 1；Disassemble the lithium ion battery after 1000 circulations,
Take a piece of cathode sheets in dimethyl carbonate solvent, to clean 5 times, dry after each one minute, use side same as in Example 1
Method calculates and expands pole piece along the aperture of thickness direction and porosity distribution after circular treatment.
Referring to Fig. 3, the cross section that it illustrates the anode strip being filled with hydrolyzate in embodiment 2 is surveyed under scanning electron microscope
The result of amount.As shown in Figure 3 a, it can be seen that the distribution situation that the image of characteristic element silicon presents continuously and dispersion combines, due to
In measured anode sheet of lithium ion battery, do not contain element silicon, therefore can be determined that detected element silicon is entirely derived from and fill out
The hydrolyzate of the siloxanes of solidification after filling, and contrast element silicon EDS maps and microstructure schematic diagram (Fig. 3 b) simultaneously gathered
It can be seen that present the place of hole under microstructure, corresponding element silicon distribution is more, therefore can be determined that containing element silicon
Hydrolyzate can be filled in the hole of anode graphite structure.
Fig. 4 a gives the porosity Two dimensional Distribution along thickness direction that calculating is passed through in the cross section in Fig. 3 a, and Fig. 4 b is given
Use the porosity that mercury injection method measurements obtain as a result, it is possible to find out that the method using the present invention to provide can obtain hole and tie
The Two dimensional Distribution of structure, it is possible to association porosity and its particular location in pole piece, contributes to from design of material and technological parameter
Angularly optimize electrode slice pore structure.
In the present invention measures the method for cell structure distribution of pores, can be come by the acid-base value of regulation hydrolytic process
Control the hardening time of hydrolyzate, it would however also be possible to employ containing the Organic substance of further feature element, such as contain titanium, aluminum, magnesium, calcium
Hydrolyze in acid or alkali environment Deng the Organic substance of element and obtain flowing material.
The method that the present invention provides can be widely applied to pore-size distribution and the porosity distribution survey of electrodes of lithium-ion batteries
Amount, is simultaneously suitable for measuring the distributed in three dimensions of electrodes of lithium-ion batteries mesopore under different operation sections, different electrochemical state,
Thus characterization processes process and electrochemical process are for the impact of loose structure in lithium ion cell electrode sheet, for optimizing technique
Parameter and electrochemical process parameter have great importance.But, the present invention is not limited to the hole of electrodes of lithium-ion batteries and surveys
Amount, for knowing those skilled in the art, present disclosure applies equally to other need the aperture to cell structure and
Porosity distribution makees production industry and the research field accurately measured.
The announcement of book and teaching according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula carries out suitable change and amendment.Therefore, the invention is not limited in detailed description of the invention disclosed and described above, to this
Some modifications and changes of invention should also be as falling in the scope of the claims of the present invention.Although additionally, this specification
In employ some specific terms, but these terms are merely for convenience of description, and the present invention does not constitute any restriction.
Claims (9)
1. the method measuring cell structure distribution of pores, it is characterised in that comprise the following steps:
Preparing a kind of flowing material containing characteristic element, described characteristic element is can by electron scattering detection of energy spectrometer and not
It is present in the element in cell structure to be measured；
Prepared flowing material is filled in the pore structure of cell structure to be measured；
Make brittle failure after being soaked in liquid nitrogen by populated cell structure to process, use electron scattering energy disperse spectroscopy detection porous knot
The EDS maps of characteristic element on structure body section；And
Use computer image analysis method, the characteristic element obtained mapping picture on section is done at gray processing
Reason, equidistantly divides along specific direction simultaneously, calculates in each equidistant bar-shaped zone characteristic element area and accounts for total
The ratio of area, as pore-size distribution and the distribution of porosity, obtains the Two dimensional Distribution of pore structure.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that from parallel direction
Diverse location carries out brittle failure process, repeats above-mentioned detection and computational analysis step, obtains the two dimension of a series of pore structure
Distribution, the Two dimensional Distribution result of the distribution of pores of comprehensive diverse location, calculate and reconstruct cell structure mesopore structure
Distributed in three dimensions.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that described flowing material
Viscosity be 5～15mPa S.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that described flowing material
Can be filled within 10s in the pore structure of cell structure to be measured.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that described flowing material
Solidified in 1 hour in atmosphere, and after solidification, volume will not shrink and expand.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that described populated
Cell structure soak time in liquid nitrogen is 5～20 minutes, brittle failure on the sharp keen edge of a knife after taking out from liquid nitrogen.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that described characteristic element
For silicon, described flowing material is that siloxanes hydrolyzes the polysiloxane hydrolyzate obtained in an acidic solution.
The method of measurement cell structure distribution of pores the most according to claim 1, it is characterised in that described loose structure
Body is lithium-ion cathode sheet or anode strip.
The method of measurement cell structure distribution of pores the most according to claim 8, it is characterised in that described loose structure
Body is the lithium-ion cathode sheet after roll-in or chemical conversion or circulation or anode strip.
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| CN103471974B (en) * | 2013-09-05 | 2015-08-12 | 东华大学 | A kind of image method measures the method for fabric theoretic porosity |
| CN106198348B (en) * | 2016-07-13 | 2019-08-16 | 江苏师范大学 | The method for measuring catalyst layer for proton exchange film fuel cell porosity |
| CN109253956B (en) * | 2017-07-13 | 2021-03-12 | 中国石油化工股份有限公司 | Compact core pore connectivity analysis method |
| CN109100279B (en) * | 2018-08-27 | 2021-04-30 | 中国石油天然气股份有限公司 | Rock three-dimensional pore structure determination method for CO2 water-rock reaction |
| CN110423092B (en) * | 2018-11-22 | 2021-06-08 | 中国科学院青海盐湖研究所 | Magnesium oxychloride cement foam concrete air hole structure model manufacturing and characterization method based on magnesium phosphate cement |
| CN110361313B (en) * | 2019-07-11 | 2022-04-05 | 上海应用技术大学 | Electrochemical test method for quantitatively evaluating porosity of phosphating film |
| CN116754211B (en) * | 2023-08-22 | 2023-12-19 | 中国人民解放军火箭军工程大学 | Method and related device for acquiring mechanical property information of solid rocket propeller |
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| US4797906A (en) * | 1987-09-28 | 1989-01-10 | Amoco Corporation | Nondestructive method for analyzing total porosity of thin sections |
| JP4049513B2 (en) * | 2000-05-25 | 2008-02-20 | 独立行政法人科学技術振興機構 | Method for measuring porosity of porous silicon |
| US7609812B2 (en) * | 2002-12-27 | 2009-10-27 | Technos Co., Ltd. | Pore- or particle-size distribution measurement apparatus |
| CN1987419B (en) * | 2006-12-21 | 2010-05-19 | 复旦大学 | Electrochemical method for detecting anodic aluminium oxide formwork effective hole density |
| US8257979B2 (en) * | 2007-11-12 | 2012-09-04 | GM Global Technology Operations LLC | Method for characterizing the porosity in fuel cell electrodes |
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