CN110411901A - The evaluating apparatus of the wetting factor of the evaluation method and measurement electrode of liquid flow cell material of the wetting factor of electrode of liquid flow cell material - Google Patents
The evaluating apparatus of the wetting factor of the evaluation method and measurement electrode of liquid flow cell material of the wetting factor of electrode of liquid flow cell material Download PDFInfo
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Abstract
The present invention relates to flow battery fields, disclose the evaluating apparatus of the evaluation method of the wetting factor of electrode of liquid flow cell material and the wetting factor of measurement electrode of liquid flow cell material, the evaluation method includes: that electrode of liquid flow cell material is fixed below precision mechanics test equipment, and electrode of liquid flow cell material lower part is contacted with liquid phase test agent, liquid level of the electrode of liquid flow cell material perpendicular to liquid phase test agent；It records under different time of contact t, the numerical value for the power F that precision mechanics test equipment measures；The numerical value of the power F is done into figure to the time of contact t and obtains wetability t-F curve；Once linear fitting is carried out to the wetability t-F curve, the once linear function being fitted obtains wetting factor k by the slope of the function.Evaluation method and device provided by the invention have efficient, corrosion-resistant, and accuracy is strong, and stability is high, easy-operating advantage, the final test realized to porous material wetability.
Description
Technical field
The present invention relates to flow battery fields, and in particular to the evaluation method of the wetting factor of electrode of liquid flow cell material and
Measure the evaluating apparatus of the wetting factor of electrode of liquid flow cell material.
Background technique
Flow battery is a kind of electrochemical energy storage technology, generally utilizes activity in anode in charge and discharge process and cathode liquid phase
The storage and release of energy are realized in the variation of substance valence state.What is succeeded in developing at present includes all-vanadium flow battery, siderochrome liquid
The technologies such as galvanic battery and zinc-bromine flow battery.Flow battery is primarily adapted for use in extensive energy storage field, including new-energy grid-connected, electricity
It stands peak regulation, intelligent micro-grid, uninterruptible power supply and independently-powered.Due to the rapid development and energy conservation and environmental protection industry of New Energy Industry
The demand of development, energy storage technology extensive for flow battery etc. is in rapid increase trend.Electrode material is the core of flow battery
Center portion part.Electrode material is generally made of porous carbon material, porous graphite material or carbon graphite fibrous material, liquid electrolytic
Matter is transported to porous electrode inner surface, electrochemical reaction occurs at the interface of electrode material and electrolyte contacts, along with work
The property change of substance valence state and the gain and loss of electronics, to realize the storage and release of electric energy.The wetability of electrode material is directly determined
Determine the size of electrolyte Yu electrode contact interface, to determine the size of cell output current, and then determines battery
Performance and cost.
CN104207320B discloses in a kind of papermaking-method reconstituted tobaccos tobacco chip base to the measurement side of coating fluid absorbability
Method, this method absorb the volume change of liquid by material come judgement material to the wetability of liquid, but in actual mechanical process
Droplet size is difficult to calculate, and especially absorbing remaining droplet size after a certain period of time can not accurately determine.
CN105823706A discloses a kind of gas wetability test method, comprising: hangs rock to be measured in weighing device
Under, and the rock to be measured is immersed in liquid, start simultaneously at timing；According to the first prefixed time interval record absorbent time and
Quality after the rock water suction to be measured；According to after the rock to be measured water suction quality and the absorbent time, described in acquisition
The absorption speed of rock to be measured；After water suction 100% is removed and placed from liquid containing the water saturated rock to be measured in institute
It states on weighing device, starts simultaneously at timing；Volatilization time and the rock volatilization to be measured are recorded according to the second prefixed time interval
Quality afterwards；Quality and the volatilization time after being volatilized according to the rock to be measured obtain the volatilization speed of the rock to be measured
Degree；The gas wetability of the rock to be measured is obtained according to the absorption speed of the rock to be measured and the evaporation rate.Material
The calculating of the rate of liquid aspiration of material has substantial connection with absorption saturation degree of the material to liquid, which can also be from the implementation of this method
Directly find out in example.Calculated rate of liquid aspiration has larger difference when different imbibition saturation degrees, and different materials difficult to realize exist
Identical imbibition saturation degree is kept in test process.If different materials calculate rate of liquid aspiration when imbibition 100% is saturated, this makes
The material for obtaining wetability difference needs the time longer or even cannot achieve.Therefore, this method is not suitable for comparing different materials
Wetability.
CN102890042A discloses a kind of method for measuring the wetability of porous material comprising: by porous material
The sample of material is placed in calorimeter sample cell, contacts the sample with wetting fluid, and test constantly enters the sample
Hot-fluid in pond is filled out according to the result of the heat-flow measurement and in view of the fuel factor of the fluid compression to by the fluid
First wetting contact angle of the hole filled is calculated, at least once by the pressure in the sample cell with the sample from
Initial value starts to increase, and until all holes of the sample are filled by the fluid completely, and test constantly enters the sample
Hot-fluid in product pond, according to the result of the heat-flow measurement and in view of the fuel factor of the fluid compression, to by the fluid
Second wetting contact angle of the hole of filling is calculated, at least once by the pressure in the sample cell with the sample
It is reduced to initial value, and test constantly enters the hot-fluid in the sample cell, according to the result of the heat-flow measurement and considers
The fuel factor of the fluid compression calculates the third wetting contact angle of the hole without the fluid.This method is main
For petroleum and natural gas industry.
Electrode of liquid flow cell material is mostly porous carbon materials, and electrode material surface is coarse so that it is difficult with Conventional contact angle
Tester tests its wetability.In addition, the wetability of electrode of liquid flow cell material primarily directed to variation of valence occurs
Acidic liquid, rather than general aqueous solution, this makes electrode material have bigger difficulty to the wetability test of electrolyte.
It in summary it can be seen, be used to evaluate the wetability of electrode of liquid flow cell material currently without effective method, thus
Quick screening and evaluation difficult to realize to electrode material, it is even more impossible to the electrochemistries to electrode material can be carried out prediction.Therefore,
The method for needing a kind of new measurement and evaluation flow battery porous electrode material wetability.
Summary of the invention
The evaluation that the purpose of the invention is to overcome the problems, such as to be difficult to realize the wetability to electrode of liquid flow cell material,
It provides the evaluation method of the wetting factor of electrode of liquid flow cell material and measures the wetting factor of electrode of liquid flow cell material
Evaluating apparatus.Evaluation method and device provided by the invention have efficient, corrosion-resistant, and accuracy is strong, and stability is high, easy-operating
Advantage, the final test realized to porous material wetability.
To achieve the goals above, first aspect present invention provides a kind of commenting for the wetting factor of electrode of liquid flow cell material
Valence method, the evaluation method include:
Electrode of liquid flow cell material is fixed below precision mechanics test equipments, and electrode of liquid flow cell material lower part with
The contact of liquid phase test agent, liquid level of the electrode of liquid flow cell material perpendicular to liquid phase test agent；
It records under different time of contact t, the numerical value for the power F that precision mechanics test equipment measures；By the numerical value pair of the power F
The time of contact t does figure and obtains wetability t-F curve；
Once linear fitting, the once linear function being fitted, by the function are carried out to the wetability t-F curve
Slope obtains wetting factor k.
Second aspect of the present invention provides a kind of evaluating apparatus of wetting factor for measuring electrode of liquid flow cell material, the device
Include:
Precision mechanics test equipment 1, fixture 2 and liquid storage tank 3；
The fixture 2 is used to for electrode of liquid flow cell material being fixed on 1 lower section of precision mechanics test equipment；
The liquid storage tank 3 is for storing liquid phase test agent；
The placement location of precision mechanics test equipment 1, fixture 2 and liquid storage tank 3 enables electrode of liquid flow cell material lower part
It is enough to be contacted with the liquid phase test agent in liquid storage tank 3；
Precision mechanics test equipment 1 is for measuring under different time of contact t, the stress value F of electrode of liquid flow cell material.
The evaluation method and evaluating apparatus of the wetting factor of electrode of liquid flow cell material provided by the invention have following excellent
Gesture:
(1) evaluation method and device provided by the invention can be used for commonly using electrode of liquid flow cell material, not only quickly, it is quasi-
Really and it is easily operated with realize；
(2) evaluation method and device provided by the invention can be used for electrode of liquid flow cell material to different electrolytes system
Wettability is evaluated, including but not limited to water phase acid metal salting liquid；
(3) the wettability knot of the electrode of liquid flow cell material of the evaluation method and device measurement of attached confession is mentioned using the present invention
Fruit is used to predict the performance of electrode material, and anticipation trend is consistent with battery actual test result.This method can quickly screen liquid
Galvanic battery electrode material simultaneously carries out tentative prediction to its performance.
Detailed description of the invention
Fig. 1 is a kind of evaluation of the wetting factor for determining electrode of liquid flow cell material of specific embodiment provided by the invention
Schematic device；
Fig. 2 is the wetability t-F curve graph that embodiment 1-3 is obtained；
Fig. 3 is the photo of the electrode material surface that optical contact angle tester is shot in comparative example 1 and drop.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
First aspect present invention provides a kind of evaluation method of the wetting factor of electrode of liquid flow cell material, the evaluation method
Include:
Electrode of liquid flow cell material is fixed below precision mechanics test equipments, and electrode of liquid flow cell material lower part with
The contact of liquid phase test agent, liquid level of the electrode of liquid flow cell material perpendicular to liquid phase test agent；
It records under different time of contact t, the numerical value for the power F that precision mechanics test equipment measures；By the numerical value pair of the power F
The time of contact t does figure and obtains wetability t-F curve；
Once linear fitting, the once linear function being fitted, by the function are carried out to the wetability t-F curve
Slope obtains wetting factor k.
Electrode of liquid flow cell material can be cut by a kind of specific embodiment according to the present invention in setup test
Suitable size facilitates fastening to below precision mechanics test equipment.
A kind of specific embodiment according to the present invention, can be arranged on the precision mechanics test equipment can pass through journey
Sequence automatically controls the bracket of adjustable height, can make electrode of liquid flow cell material by the bracket of procedure auto-control adjustable height
Lower part is contacted with liquid phase test agent.
Electrode of liquid flow cell material can be fixed on precision by fixture by a kind of specific embodiment according to the present invention
Below mechanical testing instrument, i.e., one end of fixture is connect with precision mechanics test equipment, the other end and electrode of liquid flow cell material
Connection.
A kind of specific embodiment according to the present invention, this method further include in electrode of liquid flow cell material lower part and liquid phase
Before test agent contact, precision mechanics test equipment and electrode of liquid flow cell material are adjusted to horizontality, and will be smart
Close mechanical testing instrument registration is reset to exclude the influence of electrode of liquid flow cell material gravity.
In the present invention, electrode of liquid flow cell material keeps liquid phase test agent uniform perpendicular to the liquid level of liquid phase test agent
Contact material, and infiltrated along section.
In the present invention, as long as electrode of liquid flow cell material lower part is contacted with liquid phase test agent, it is preferable that described
Vertical range between the bottom surface of electrode of liquid flow cell material and the liquid level of liquid phase test agent is zero." liquid stream electricity of the present invention
Vertical range between the bottom surface of pond electrode material and the liquid level of liquid phase test agent is zero " to refer to electrode of liquid flow cell material
Bottom surface touches the liquid level of liquid phase test agent, but does not arrange liquid phase test agent, it can be understood as the electrode of liquid flow cell
The bottom surface of material is just contacted with the liquid level of liquid phase test agent.Those skilled in the art control according to the actual situation.For example,
When electrode of liquid flow cell material is not contacted with the liquid level of liquid phase test agent, the number for the power F that precision mechanics test equipment measures
Be worth it is constant, and when the bottom surface of electrode of liquid flow cell material is just contacted with the liquid level of liquid phase test agent, then precision mechanics tester
The numerical value for the power F that device measures will appear variation, when the numerical value one for the power F that precision mechanics test equipment measures changes, that is, recognize
Vertical range between the bottom surface of electrode of liquid flow cell material and the liquid level of liquid phase test agent is zero.Those skilled in the art can
To carry out suitable control according to foregoing description.
The present invention is wider to the range of choice of the shape of the electrode of liquid flow cell material, the preferably described electrode of liquid flow cell
Material is regular shape, such as can be at least one of cuboid, triangular prism and cylindrical body.
A preferred embodiment of the invention, the electrode of liquid flow cell material are cuboid, the cuboid
Height be not more than 10cm, it is wide be not more than 5cm, with a thickness of be not more than 0.5cm.Minimum of the present invention to electrode of liquid flow cell material
There is no particular limitation for length and width, thickness, in order to easy to operate, it is further preferred that a height of 1-5cm of the cuboid, width are
1-4cm, with a thickness of 0.01-0.2cm.The present invention most preferably cuboid with a thickness of 0.02-0.08cm, be preferably implemented using this kind
Mode is more advantageous to the accuracy for improving evaluation.
Using the shape of the electrode of liquid flow cell material of the preferred embodiment for the present invention, be more advantageous to liquid phase test agent along
The bottom surface of electrode of liquid flow cell material uniformly extends infiltration upwards, so that evaluation result is more accurate.
A kind of specific embodiment according to the present invention, can be by electrode of liquid flow cell material cutting to be measured at unified big
It is the smallest to control area in cuboid for example, can be the cuboid of high 2cm, width 1cm, thickness 0.02-0.08cm for small shape
Face has just been contacted as bottom surface with the liquid level of liquid phase test agent.
A preferred embodiment of the invention, the porosity of the electrode of liquid flow cell material is 75-96%, excellent
It is selected as 85-90%.
Electrode of liquid flow cell material of the present invention can be various electrode of liquid flow cell materials commonly used in the art,
Preferably, the electrode of liquid flow cell material is at least one of carbon paper, carbon felt, graphite paper and graphite felt.The present invention is implemented
Example part illustrates the evaluation method of the wetting factor of electrode of liquid flow cell material by taking carbon paper and carbon felt as an example.
The rough surface of electrode of liquid flow cell material, so that it is difficult to test its wetability with Conventional contact angle tester,
Using evaluation method provided by the invention, not only precise and high efficiency, and it is easily operated.
In accordance with the present invention it is preferred that the liquid phase test agent be water and/or fluid cell electrolyte, further preferably
Fluid cell electrolyte.The wetability of electrode of liquid flow cell material is directed to the acidic liquid that variation of valence can occur, this makes electricity
The wetability test of pole material on electrolyte has bigger difficulty, so that existing conventional method can not be applicable in.
In accordance with the present invention it is preferred that the fluid cell electrolyte is the acid solution containing metal salt, such as can be
Sulfuric acid solution containing metal salt, the metal salt be selected from mantoquita, molysite, vanadic salts, antimonic salt, bismuth salt, chromic salts, germanium salt, pink salt and
At least one of manganese salt, it is further preferred that the metal salt is selected from least one of vanadic salts, molysite and chromic salts, it is optimal
It is selected as vanadic salts.It such as can be VOSO4、(VO2)2SO4、VSO4And V2(SO4)3At least one of.
There is no particular limitation for concentration of the present invention to the metal salt in the fluid cell electrolyte, those skilled in the art
Member can suitably be selected according to conventional fluid cell electrolyte.For example, the concentration of the metal salt can be 0.5-
1.6mol/L, the concentration of sulfuric acid can be 1.5-2mol/L.
According to the present invention, the precision mechanics test equipment can be commercially available, and precision mechanics test equipment is used for
Test the numerical value of the power F of the electrode of liquid flow cell material under different time of contact t.The precision mechanics test equipment refers to energy
Enough distinguish the mechanical testing instrument of low-force value (mN grades, such as 100mN).
The resolution ratio of a preferred embodiment of the invention, the precision mechanics test equipment is not more than 10mN,
Further preferably it is not more than 1mN.Resolution ratio of the present invention refers to the minimum force value that precision mechanics test equipment can distinguish
Size.
A kind of specific embodiment according to the present invention, the precision mechanics test equipment can be to be commercially available from KRUSS company
The trade mark is the mechanical test instrument of K100, and resolution ratio is 0.3mN.
The present invention is wider to the time of contact t range of choice, and those skilled in the art can carry out according to the actual situation
Appropriate selection, main judgment criteria are in electrode of liquid flow cell material lower part and liquid phase test agent contact process, and precision mechanics are surveyed
When the numerical value for the power F that test instrument measures is substantially unchanged, it can stop.For different electrode of liquid flow cell materials and it is different with
Liquid phase test agent, time of contact t range of choice may be different, if electrode of liquid flow cell material is to the wetability of liquid phase test agent
Particularly poor, even if extending contact time t, the numerical value for the power F that precision mechanics test equipment measures is still substantially unchanged, at this time
It is not necessary to evaluate the wetting factor of the material.
A preferred embodiment of the invention, the maximum value of the time of contact t are 5min, further preferably
2min。
Numerical value of the present invention by the power F does figure to the time of contact t and refers to time of contact t for horizontal seat
Mark, under different time of contact t, the numerical value for the power F that precision mechanics test equipment measures does figure for ordinate and obtains wetability t-F
Curve.
Once linear fitting, the once linear function being fitted, by the function are carried out to the wetability t-F curve
Slope obtains wetting factor k.Wetting factor k shows more greatly the liquid phase test agent to the wettability of the electrode of liquid flow cell material
Good, factor k is smaller shows that the liquid phase test agent is poor to the wettability of the electrode of liquid flow cell material for wetting.
Second aspect of the present invention provides a kind of evaluating apparatus of wetting factor for measuring electrode of liquid flow cell material, such as Fig. 1
Shown, which includes: precision mechanics test equipment 1, fixture 2 and liquid storage tank 3；
The fixture 2 is used to for electrode of liquid flow cell material being fixed on 1 lower section of precision mechanics test equipment；
The liquid storage tank 3 is for storing liquid phase test agent；
The placement location of precision mechanics test equipment 1, fixture 2 and liquid storage tank 3 enables electrode of liquid flow cell material lower part
It is enough to be contacted with the liquid phase test agent in liquid storage tank 3；
Precision mechanics test equipment 1 is for measuring under different time of contact t, the stress value F of electrode of liquid flow cell material.
Electrode of liquid flow cell material can be cut by a kind of specific embodiment according to the present invention in setup test
Then electrode of liquid flow cell material is fixed on 1 lower section of precision mechanics test equipment, the fixture 2 using fixture 2 by suitable size
One end connect with precision mechanics test equipment 1, the other end is connect with electrode of liquid flow cell material.
Shape, size and the type of the electrode of liquid flow cell material as described above, the present invention details are not described herein.Tool
Body, the wide opening less than liquid storage tank 3 of electrode of liquid flow cell material is so that electrode of liquid flow cell material can be surveyed with liquid phase
Reagent contact.
The selection of the precision mechanics test equipment 1 is as described above, details are not described herein.
The evaluating apparatus provided according to the present invention, it is preferable that precision mechanics test equipment 1, fixture 2 and liquid storage tank 3 are put
Seated position makes the vertical range between the liquid level of the liquid phase test agent in the bottom surface and liquid storage tank 3 of electrode of liquid flow cell material to be
Zero.
The evaluating apparatus provided according to the present invention, it is preferable that the precision mechanics test equipment 1, which is provided with, can pass through program
The bracket for automatically controlling adjustable height moves bracket, fixture and electrode of liquid flow cell material jointly by controlling bracket, directly
It is extremely zero by the vertical range between the liquid level of the liquid phase test agent in the bottom surface of electrode of liquid flow cell material and liquid storage tank 3.
A preferred embodiment of the invention, the movement speed of the bracket is 1-10mm/min, further excellent
It is selected as 4-8mm/min.
The evaluating apparatus provided according to the present invention, the selection of the liquid phase test agent is as described above, details are not described herein.
There is no particular limitation for size and shape of the present invention to the liquid storage tank 3, as long as liquid phase test agent can be stored
, such as the liquid storage tank 3 can be cylinder shape groove, it is highly 3-5cm that interior grooves diameter, which is 6-10cm,.
The evaluation method and measurement liquid of the wetting factor of electrode of liquid flow cell material provided by the invention described further below
A kind of specific embodiment of the evaluating apparatus of the wetting factor of galvanic battery electrode material.
It (such as can be high 2cm, width 1cm, thickness by the cuboid that electrode of liquid flow cell material is cut into unified size
0.02cm), electrode of liquid flow cell material horizontal is fixed on by the lower section of precision mechanics test equipment 1 by fixture 2, i.e. fixture 2
One end is connect with precision mechanics test equipment 1, and the other end is connect with electrode of liquid flow cell material top, adjustment precision mechanics test
Instrument 1 is reset to horizontality, and by the registration of precision mechanics test equipment 1 to eliminate the shadow of electrode of liquid flow cell material gravity
It rings.The precision mechanics test equipment 1, which is provided with, to be made by the bracket of procedure auto-control adjustable height by controlling bracket
It obtains bracket, fixture 2 and electrode of liquid flow cell material and moves (support moving speed 1-10mm/min) jointly, until by liquid stream electricity
Pond electrode material lower part can be contacted with the liquid phase test agent in liquid storage tank 3 (preferably the bottom surface of electrode of liquid flow cell material with
Zero) vertical range between the liquid level of liquid phase test agent in liquid storage tank 3 is.Record different time of contact t (time of contact t's
Maximum value is 5min) under, the numerical value for the power F that precision mechanics test equipment measures, using time of contact t as abscissa, with Cont rol Method of Precise Force
Learning the numerical value of power F that test equipment measures is ordinate, does figure and obtains wetability t-F curve, to the wetability t-F curve into
The fitting of row once linear, the once linear function being fitted obtain wetting factor k by the slope of the function.
The present invention will be described in detail by way of examples below.
In following embodiment, precision mechanics test equipment 1 is to be commercially available from the mechanical test that the KRUSS company trade mark is K100
Instrument, resolution ratio 0.3mN.
Embodiment 1
Carbon paper (being commercially available from the product that SGL Group company's trade mark is GDL28AA) is cut into high 2cm, width 1cm, thickness
Then its level is fixed on 1 lower section of precision mechanics test equipment, i.e. one end of fixture 2 by fixture 2 by the cuboid of 0.02cm
It being connect with precision mechanics test equipment 1, the other end is connect with carbon paper top, adjustment precision mechanics test equipment 1 to horizontality,
And the registration of precision mechanics test equipment 1 is reset.
To liquid storage tank 3, (cylinder shape groove, interior grooves diameter are 8cm, are highly electrolysed for 100mL vanadium system is added in 4cm)
Liquid (1mol/L VOSO4+2mol/L H2SO4).As shown in Figure 1, passing through precision mechanics test equipment 1 described in procedure auto-control
Support height so that bracket, fixture 2 and cutting rear carbon paper and moving down (movement speed 6mm/min) jointly until cut rear carbon
Paper just contacts (cutting the vertical range between the bottom surface of rear carbon paper and the liquid level of vanadium system electrolyte is zero), In with vanadium system electrolyte
1min is stopped at this, records the stress condition (registration of precision mechanics test equipment 1) for cutting rear carbon paper in 1min in whole process.
As shown in Fig. 2, the numerical value of the power F measured using precision mechanics test equipment does figure as ordinate using time of contact t as abscissa
Wetability t-F curve is obtained, to wetability t-F curve progress once linear fitting, the once linear function being fitted,
The slope of the function is denoted as wetting factor k, and wetting factor k is -0.582.The wetting factor k that the present embodiment measures is negative value, table
The bright carbon paper is bad to the wellability of vanadium system electrolyte.
Embodiment 2
Carbon paper (being commercially available from the product that SGL Group company's trade mark is GDL38AA) is cut into high 2cm, width 1cm, thickness
Then its level is fixed on 1 lower section of precision mechanics test equipment, i.e. one end of fixture 2 by fixture 2 by the cuboid of 0.04cm
It being connect with precision mechanics test equipment 1, the other end is connect with carbon paper top, adjustment precision mechanics test equipment 1 to horizontality,
And the registration of precision mechanics test equipment 1 is reset.
To liquid storage tank 3, (cylinder shape groove, interior grooves diameter are 8cm, are highly electrolysed for 100mL vanadium system is added in 4cm)
Liquid (same as Example 1).As shown in Figure 1, by the support height of precision mechanics test equipment 1 described in procedure auto-control,
So that bracket, fixture 2 and cut rear carbon paper move down jointly (movement speed 6mm/min) until cut rear carbon paper and vanadium system electrolysis
Liquid just contacts (vertical range cut between the bottom surface of rear carbon paper and the liquid level of vanadium system electrolyte is zero), stops at this
1.5min records the stress condition (registration of precision mechanics test equipment 1) for cutting rear carbon paper in 1.5min in whole process.Such as figure
Shown in 2, using time of contact t as abscissa, the numerical value of the power F measured using precision mechanics test equipment is done figure and obtained as ordinate
Wetability t-F curve carries out once linear fitting, the once linear function being fitted, the letter to the wetability t-F curve
Several slopes is denoted as wetting factor k, and wetting factor k is 0.0441.The wetting factor k that the present embodiment measures is smaller, shows the carbon
Paper is poor to the wellability of vanadium system electrolyte.
Embodiment 3
Carbon felt material (being commercially available from the product that SGL Group company's trade mark is GDL10AA) is cut into high 2cm, width 1cm, thickness
Then its level is fixed on 1 lower section of precision mechanics test equipment, i.e. one end of fixture 2 by fixture 2 by the cuboid of 0.08cm
It is connect with precision mechanics test equipment 1, the other end is connect with carbon felt material top, adjustment precision mechanics test equipment 1 to level
State, and the registration of precision mechanics test equipment 1 is reset.
To liquid storage tank 3, (cylinder shape groove, interior grooves diameter are 8cm, are highly electrolysed for 100mL vanadium system is added in 4cm)
Liquid (same as Example 1).As shown in Figure 1, by the support height of precision mechanics test equipment 1 described in procedure auto-control,
So that bracket, fixture 2 and cut rear carbon felt material move down jointly (movement speed 6mm/min) until cut rear carbon felt material with
Vanadium system electrolyte just contacts (vertical range cut between the bottom surface of rear carbon felt material and the liquid level of vanadium system electrolyte is zero), In
1min is stopped at this, is recorded and is cut the stress condition of rear carbon felt material in 1min in whole process (precision mechanics test equipment 1 shows
Number).As shown in Fig. 2, using time of contact t as abscissa, the numerical value of the power F measured using precision mechanics test equipment as ordinate,
It does figure and obtains wetability t-F curve, once linear fitting, the once linear being fitted are carried out to the wetability t-F curve
Function, the slope of the function are denoted as wetting factor k, and wetting factor k is 4.49.The wetting factor k that the present embodiment measures is larger, table
The bright carbon felt material is preferable to the wellability of vanadium system electrolyte.
Below to the performance test of electrode of liquid flow cell material involved in above-described embodiment 1-3, it is related to flow battery energy
Amount efficiency and flow battery delivery efficiency density.
Test example 1
Using above-mentioned carbon paper described in embodiment 1 as anode and cathode, using perfluorinated sulfonic acid diaphragm as diaphragm, by perfluor
Sulfonic acid diaphragm is placed between anode and cathode, places PTFE stuffing materials in surrounding them, end plate is placed on afflux
On the outside of plate, fastened using bolt by preset hole with upper-part.Assembly is monocell.Anode electrolyte initial concentration is 0.8mol
L-1V(IV)+0.8mol L-1V(IV)+3mol L-1H2SO4, electrolyte liquid concentration is 0.8mol L-1V(II)+0.8mol
L-1V(III)+3mol L-1H2SO4.In room temperature (25 DEG C) condition, under the conditions of electrolyte flow rate is 500mL/min, to the battery into
Row charge-discharge test and polarization curve test.Wherein, flow battery energy efficiency and flow battery output power density are pressed respectively
Following formula is calculated.Test result is listed in table 1.
Flow battery energy efficiency=simple subprogram discharge process output energy/cycle charging process input energy ×
100%.
Flow battery output power density=cell output/electrode projected area × 100%.
Test example 2-3
It is tested according to the method for test example 1, unlike, carbon paper described in embodiment 1 is replaced with into implementation respectively
Carbon paper described in example 2 and carbon felt described in embodiment 3.Test result is listed in table 1.
Table 1
From the results shown in Table 1, the flow battery energy efficiency highest of the carbon felt material of embodiment 3, flow battery
Output power density is maximum, and the carbon paper material of embodiment 2 takes second place, and the flow battery energy efficiency of the carbon paper material of embodiment 1 is most
Low, flow battery power density is minimum.The electrode of liquid flow cell material that the test result and 1-3 of the embodiment of the present invention are measured is to electricity
The result trend of the wellability of solution liquid is identical, and (wellability of carbon felt material on electrolyte described in embodiment 3 is best, embodiment 2
Carbon paper material take second place, the wellability of the carbon paper material on electrolyte of embodiment 1 is worst).Illustrate evaluation side provided by the invention
Method and device can evaluate the wetting property of electrode of liquid flow cell material, and evaluation result is accurate, can be used in predicting
The performance of electrode material, anticipation trend are consistent with battery actual test result.
Comparative example 1
Wetability of the electrode of liquid flow cell material described in embodiment 1 to vanadium system electrolyte is tested, test is specific
Process include: by electrode material to be measured be cut into high 2cm, width 1cm, thickness 0.02cm cuboid and be placed in optical contact angle test
Instrument (being commercially available from KRUSS company, model DSA100) sample stage, dropping liquid needle slowly close to electrode material surface to be measured, work as syringe needle
One drop vanadium system described in embodiment 1 electrolyte of release, makes its freely falling body to electrode material to be measured when close to electrode material to be measured
Surface forms liquid pearl.Photo is shot as shown in figure 3, from figure 3, it can be seen that electrode material surface to be measured has fibrous filament,
Electrode material surface i.e. to be measured is porous non-smooth state, solid-liquid contact point can not be found when measuring by optical method accurately with fixation
Baseline, eventually leads to that measuring result error is larger, is unable to complete quick screening and evaluation to electrode material.
The method that can be seen that prior art offer from comparative example 1 and 1 data of table can not be accurately to flow battery electricity
The wettability of pole material is evaluated and tested.And evaluation method and device provided by the invention are not only quick, accurate and easily operated
With realization；In addition, evaluation method and device provided by the invention can be used for electrode of liquid flow cell material to different electrolytes system
Wettability evaluated, including but not limited to water phase acid metal salting liquid；The evaluation method of attached confession is proposed using the present invention
It is used to predict the performance of electrode material, anticipation trend and electricity with the wettability result of the electrode of liquid flow cell material of device measurement
Pond actual test result is consistent.This method can quickly screen electrode of liquid flow cell material and carry out tentative prediction to its performance.
It is described the prefered embodiments of the present invention in detail above in conjunction with attached drawing, still, the present invention is not limited thereto.At this
, can be with various simple variants of the technical solution of the present invention are made in the range of the technology design of invention, including each technical characteristic
It is combined with any other suitable method, these simple variants and combination equally should be considered as in disclosed in this invention
Hold, all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of evaluation method of the wetting factor of electrode of liquid flow cell material, the evaluation method include:
Electrode of liquid flow cell material is fixed below precision mechanics test equipment, and electrode of liquid flow cell material lower part and liquid phase
Test agent contact, liquid level of the electrode of liquid flow cell material perpendicular to liquid phase test agent；
It records under different time of contact t, the numerical value for the power F that precision mechanics test equipment measures；By the numerical value of the power F to described
Time of contact t does figure and obtains wetability t-F curve；
Once linear fitting, the once linear function being fitted, by the slope of the function are carried out to the wetability t-F curve
Obtain wetting factor k.
2. evaluation method according to claim 1, wherein the bottom surface of the electrode of liquid flow cell material and liquid phase test agent
Liquid level between vertical range be zero；
Preferably, the electrode of liquid flow cell material is cuboid, and the height of the cuboid is not more than 10cm, wide to be not more than 5cm,
With a thickness of no more than 0.5cm.
3. evaluation method according to claim 1, wherein
The porosity of the electrode of liquid flow cell material is 75-96%；
Preferably, the electrode of liquid flow cell material is at least one of carbon paper, carbon felt, graphite paper and graphite felt；
Preferably, the liquid phase test agent is water and/or fluid cell electrolyte, preferably fluid cell electrolyte；
Preferably, the fluid cell electrolyte be the acid solution containing metal salt, the metal salt be selected from mantoquita, molysite,
At least one of vanadic salts, antimonic salt, bismuth salt, chromic salts, germanium salt, pink salt and manganese salt.
4. evaluation method described in any one of -3 according to claim 1, wherein the resolution of the precision mechanics test equipment
Rate is not more than 10mN；
Preferably, the maximum value of the time of contact t is 5min, further preferably 2min.
5. a kind of evaluating apparatus for the wetting factor for measuring electrode of liquid flow cell material, the device include:
Precision mechanics test equipment (1), fixture (2) and liquid storage tank (3)；
The fixture (2) is used to for electrode of liquid flow cell material being fixed below precision mechanics test equipment (1)；
The liquid storage tank (3) is for storing liquid phase test agent；
The placement location of precision mechanics test equipment (1), fixture (2) and liquid storage tank (3) makes electrode of liquid flow cell material lower part
It can be contacted with the liquid phase test agent in liquid storage tank (3)；
Precision mechanics test equipment (1) is for measuring under different time of contact t, the stress value F of electrode of liquid flow cell material.
6. evaluating apparatus according to claim 5, wherein precision mechanics test equipment (1), fixture (2) and liquid storage tank (3)
Placement location make it is vertical between the bottom surface of electrode of liquid flow cell material and the liquid level of the liquid phase test agent in liquid storage tank (3)
Distance is zero.
7. evaluating apparatus according to claim 5 or 6, wherein the resolution ratio of the precision mechanics test equipment (1) is little
In 10mN.
8. the evaluating apparatus according to any one of claim 5-7, wherein the precision mechanics test equipment (1) sets
Bracket, fixture and electrode of liquid flow cell can be made by controlling bracket by the bracket of procedure auto-control adjustable height by being equipped with
Material moves jointly, until between the bottom surface of electrode of liquid flow cell material and the liquid level of the liquid phase test agent in liquid storage tank (3)
Vertical range is zero.
9. the evaluating apparatus according to any one of claim 5-8, wherein the hole of the electrode of liquid flow cell material
Rate is 75-96%；
Preferably, the electrode of liquid flow cell material is at least one of carbon paper, carbon felt, graphite paper and graphite felt.
10. the evaluating apparatus according to any one of claim 5-9, wherein the liquid phase test agent is water and/or liquid
Galvanic battery electrolyte, preferably fluid cell electrolyte；
Preferably, the fluid cell electrolyte be the acid solution containing metal salt, the metal salt be selected from mantoquita, molysite,
At least one of vanadic salts, antimonic salt, bismuth salt, chromic salts, germanium salt, pink salt and manganese salt.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113029809A (en) * | 2021-03-01 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Method and tool for testing hot pressing degree and electrolyte infiltration degree of battery core |
| CN113740195A (en) * | 2021-08-03 | 2021-12-03 | 蜂巢能源科技有限公司 | Powder wettability evaluation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1605852A (en) * | 2004-12-01 | 2005-04-13 | 北京航空航天大学 | Testing method and testing instrument for imbibition characteristic of composite material reinforcement body |
| CN2775645Y (en) * | 2004-12-01 | 2006-04-26 | 北京航空航天大学 | Infiltration property detector |
| CN101153837A (en) * | 2006-09-29 | 2008-04-02 | 廖树帜 | Dynamic testing method and system for wetting property |
| CN106596348A (en) * | 2016-12-23 | 2017-04-26 | 中国海洋石油总公司 | Testing method for rock surface static contact angle and rock surface wettability dynamic change testing method utilizing testing method for rock surface static contact angle |
| CN107576593A (en) * | 2017-08-22 | 2018-01-12 | 巨石集团有限公司 | A kind of glass fibre wellability method of testing |
-
2018
- 2018-04-26 CN CN201810384269.2A patent/CN110411901A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1605852A (en) * | 2004-12-01 | 2005-04-13 | 北京航空航天大学 | Testing method and testing instrument for imbibition characteristic of composite material reinforcement body |
| CN2775645Y (en) * | 2004-12-01 | 2006-04-26 | 北京航空航天大学 | Infiltration property detector |
| CN101153837A (en) * | 2006-09-29 | 2008-04-02 | 廖树帜 | Dynamic testing method and system for wetting property |
| CN106596348A (en) * | 2016-12-23 | 2017-04-26 | 中国海洋石油总公司 | Testing method for rock surface static contact angle and rock surface wettability dynamic change testing method utilizing testing method for rock surface static contact angle |
| CN107576593A (en) * | 2017-08-22 | 2018-01-12 | 巨石集团有限公司 | A kind of glass fibre wellability method of testing |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113029809A (en) * | 2021-03-01 | 2021-06-25 | 昆山宝创新能源科技有限公司 | Method and tool for testing hot pressing degree and electrolyte infiltration degree of battery core |
| CN113740195A (en) * | 2021-08-03 | 2021-12-03 | 蜂巢能源科技有限公司 | Powder wettability evaluation method and application thereof |
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Application publication date: 20191105 |