CN101324538B - Method for measuring powder body material electric conductivity and electric conductivity measuring apparatus suitable for the method - Google Patents
Method for measuring powder body material electric conductivity and electric conductivity measuring apparatus suitable for the method Download PDFInfo
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- CN101324538B CN101324538B CN 200710075037 CN200710075037A CN101324538B CN 101324538 B CN101324538 B CN 101324538B CN 200710075037 CN200710075037 CN 200710075037 CN 200710075037 A CN200710075037 A CN 200710075037A CN 101324538 B CN101324538 B CN 101324538B
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- 239000000843 powder Substances 0.000 title claims abstract description 112
- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000005259 measurement Methods 0.000 claims description 19
- 239000012254 powdered material Substances 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000004020 conductor Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims 1
- 238000013461 design Methods 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 7
- 238000005457 optimization Methods 0.000 abstract description 4
- 238000009472 formulation Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 30
- 229910002804 graphite Inorganic materials 0.000 description 14
- 239000010439 graphite Substances 0.000 description 14
- 229910052799 carbon Inorganic materials 0.000 description 10
- 230000007246 mechanism Effects 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005056 compaction Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000002931 mesocarbon microbead Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
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Abstract
The invention provides a method for measuring the conductivity of the powder material. The method comprises the following steps: (a) keeping the powder material to be measured in a cylinder shape and applying a certain pressure P to the powder material until the shape of the cylinder powder body can be kept stable; (b) measuring the length L, the cross-sectional area S and the resistance R of thecylinder powder body; and (c) calculating the conductivity of powder material based on the formula that Sigma is equal to L divide (R multiply S). The invention further provides a device for measuring the conductivity, which comprises a powder container, two conductive pistons, a pressure device, and a resistance measuring device. By adopting the method and the device, the conductivity of the powder material to be measured in a pressurized state can be measured, thereby the conductivity of the powder material to be measured in an operating pressure can be quantitatively provided. The relationship of the conductivity of the powder material to be measured varying with the pressure P can be obtained through changing the pressure value of the powder material to be measured and measuring the conductivity thereof. The method facilitates the selection of the electrode material, the optimization of the electrode material formulation and the integrated design of the battery system.
Description
Technical field
The present invention relates to measuring method and the device of conductivity, especially can measure measuring method and the device of the conductivity of powder under pressured state.
Background technology
At present, in production practices, the negative material of lithium ion battery all adopts material with carbon element basically, as electrographite, native graphite, acetylene black, intermediate phase pitch-based carbosphere (MCMB), petroleum coke, carbon fiber, pyrolysis resin carbon etc.Lithium ion battery requires its carbon material used as anode to have good electric conductivity, often judges by the conductivity of measuring the carbon powder material whether the electric conductivity of material with carbon element meets the requirements in manufacture process when selecting material with carbon element.
The common practice of measuring electrical conductivity of powdered material is that pressed by powder is become a chip solid, then adopts this chip solid resistance value of four-terminal method or bridge measurement, obtains its conductivity value in conjunction with area and the THICKNESS CALCULATION of this chip solid.Material with carbon element is in pressured state in battery, said method measures is conductivity after the pressed by powder moulding, material with carbon element material grain is the state after being in forming pressure and cancelling when adopting said method to measure, different from the duty (material with carbon element material grain is in pressured state) in battery, the electric conductivity of material is also different under these two kinds of different conditions, and the conductivity that measures is also different.Therefore said method can not directly react the conductivity under the pressured state of material with carbon element in battery, adopt the conductivity of said method under can not the pressured state of quantitative response material with carbon element in battery, resulting measurement result can only be as the reference that qualitatively judges material electric conductivity.And the powder body material plasticity such as graphite are low, and processability is poor, suppress more difficult in flakes.This also can affect and adopt carrying out smoothly and order of accuarcy of said method measurement.Concerning selection and battery design, how under the surveying work state, the conductivity of powder is the important topic that the scientific research personnel faces.
In addition, the conductivity of negative material is one of the factor that need to consider in battery system when design, and the conductivity of negative material must be considered with combined factors such as the optimal compaction density of battery, pole piece thickness.The battery compacted density is larger, and the conductivity of negative material is larger.But the excessive embedding process of taking off to lithium ion of compacted density has negative effect, to material gram volume performance, discharging efficiency and cycle performance are also disadvantageous first.If can obtain the conductivity of powder body material and the relation of material pressure, will be for battery optimal compaction density determine to provide the gross data support, with the relation of the conductivity of powder body material and material pressure and the performance of material gram volume, the factor such as discharging efficiency, cycle performance combines and considers first, instructs the optimization of electrode material formula and the global design of battery system.
Summary of the invention
A technical matters to be solved by this invention is to provide a kind of measuring method of measuring the conductivity of powder under pressured state.
For solving the problems of the technologies described above, the invention provides a kind of electrical conductivity of powdered material measuring method, comprise the following steps:
A, make tested powder keep column and apply certain pressure P to this column powder, keep dimensionally stable to this column powder;
Length L, the cross-sectional area S of b, measurement this column powder this moment, and the resistance value R of column powder;
C, by following formula:
σ＝L/(R×S)
Calculate the conductivity of this column powder.
Adopt the inventive method can measure the conductivity of powder under pressured state.Pressure P can be determined according to pressure or design pressure that material in battery is subject to.
For the conductivity that obtains powder body material and the relation of material pressure, can change based on the above method pressure P, measure the conductivity of material under different pressures.As the improvement of the inventive method, carry out following steps after step c:
D, change pressure P, repeating step a, b and c under each force value obtain the sprills bulk conductivity value σ corresponding with each pressure P, correspondingly draw the sprills bulk conductivity.Relation with the pressure P variation.
The change of pressure can be determined according to the pressure that material in battery may be subject to.
In the specific implementation form of the inventive method, step a can realize like this: tested powder is placed in straight tube shape cavity, from an end of this straight tube shape cavity or apply certain pressure P from the two ends of this straight tube shape cavity to tested powder simultaneously, keep dimensionally stable to tested powder.
In step a from an end of straight tube shape cavity or realize like this to the process that tested powder applies certain pressure P from the two ends of straight tube shape cavity simultaneously: adopt two pistons from both sides with tested powder shutoff in straight tube shape cavity and make tested powder keep column, one or two in these two pistons applies certain pressure P to tested powder.
Two pistons are resistance value electric conductor as can be known; The process of measuring the resistance value R of column powder in step b realizes like this: adopt resistance apparatus, during measurement two of this resistance apparatus calibrating terminals respectively with two pistons end in contact away from tested powder separately, the resistance that the gained resistance data deducts two pistons namely gets the resistance value R of column powder.The resistance value of two pistons can adopt four-terminal method or bridge measurement to obtain.
As the improvement of the inventive method, in two pistons, at least one is provided with the vent port that straight tube shape cavity is communicated with space outerpace, and the gas when piston applies certain pressure P to tested powder in straight tube shape cavity is discharged from this vent port.The result that records like this will be more true and reliable.The large I in vent port aperture determines according to the particle size range of tested powder, processability etc., and for graphite material, the vent port aperture is chosen as Φ 1-2mm.
Further improve as the inventive method, piston is electric conductor; The material of two pistons adopts copper or gold.Like this, the resistance value of piston itself is very small, can ignore.
Further improve as the inventive method, two pistons end away from tested powder separately is taper.During test, two of resistance apparatus calibrating terminals contact with the taper end points of two pistons respectively, make between the taper end points of the calibrating terminal of resistance apparatus and piston to keep less contact resistance, further guarantee measuring accuracy.
Another technical matters to be solved by this invention is to provide a kind of measurement mechanism of measuring the conductivity of powder under pressured state.
For solving this technical problem, the invention provides a kind of conductivity measuring apparatus of applicable above-mentioned measuring method, comprise with straight tube shape cavity and tested powder can be enclosed in straight tube shape cavity with the powder container of tested powder insulation, two and make tested powder keep column the conduction piston, can be in two pistons, at least one applies pressue device, the resistance apparatus of quantitative pressure.
During work, tested powder is placed in straight tube shape cavity, two pistons are enclosed in tested powder in this straight tube shape cavity from the two ends of straight tube shape cavity, and at least one applies quantitative pressure to pressue device in two pistons, piston is exerted pressure to tested powder, keep dimensionally stable to tested powder.Measure length L, the cross-sectional area S of this column powder this moment, and the resistance value R of described column powder; By following formula:
σ＝L/(R×S)
Calculate the conductivity of this column powder.Pressure P can be determined according to pressure or design pressure that material in battery is subject to.
Can also change pressure P, repeat above-mentioned conductivity measurement process under each force value, obtain the sprills bulk conductivity value σ corresponding with each pressure P, correspondingly draw the relation that sprills bulk conductivity σ changes with pressure P.The change of pressure can be determined according to the pressure that material in battery may be subject to.
As the improvement of measurement mechanism of the present invention, in two pistons, at least one is provided with the vent port that straight tube shape cavity is communicated with space outerpace, and the gas when piston applies certain pressure P to tested powder in straight tube shape cavity is discharged from this vent port.The result that records like this will be more true and reliable.The large I in vent port aperture determines according to the particle size range of tested powder, processability etc., and for graphite material, the vent port aperture is chosen as Φ 1-2mm.
Further improve as measurement mechanism of the present invention, piston is electric conductor; The material of two pistons adopts copper or gold.Like this, the resistance value of piston itself is very small, can ignore.
Further improve as measurement mechanism of the present invention, two pistons end away from tested powder separately is taper.During test, two of resistance apparatus calibrating terminals contact with the taper end points of two pistons respectively, make between the taper end points of the calibrating terminal of resistance apparatus and piston to keep less contact resistance, further guarantee measuring accuracy.
Adopt the electrical conductivity of powdered material measurement mechanism of electrical conductivity of powdered material measuring method of the present invention and applicable the method, can carry out to the tested powder material grain under pressured state conductivity measurement calculates, during measurement, tested powder pressure can be selected according to the pressure state of tested powder when working, thereby the conductivity data of tested powder under the working pressure state can quantitatively be provided; Can also by changing tested powder pressure value, measure the conductivity of tested powder under each force value, obtain the relation that tested powder conductivity changes with pressure P.For battery, adopt measuring method of the present invention and measurement mechanism will help electrode material selection, the optimization of electrode material formula and the global design of battery system.
Description of drawings
Below by embodiment also by reference to the accompanying drawings, the present invention is described in further detail:
Fig. 1 is the cross-sectional schematic of a kind of embodiment of conductivity measuring apparatus of the present invention;
Fig. 2 is the conductivity that adopts the native graphite powder that conductivity measuring apparatus shown in Figure 1 records.Relation curve with pressure P;
Fig. 3 is the cross-sectional schematic of the another kind of embodiment of conductivity measuring apparatus of the present invention.
Embodiment
Embodiment one
Fig. 1 shows a kind of embodiment of conductivity measuring apparatus of the present invention.
As shown in Figure 1, this conductivity measuring apparatus comprise powder container 1, upper piston 2, lower piston 3, sheeter (be the pressue device in technical solution of the present invention, not shown in Fig. 1; The pressurization scope can be selected in 0-10MPa), DC resistance meter (being the resistance apparatus in technical solution of the present invention, not shown in Fig. 1).
Establish straight tube shape cavity in powder container 1, the xsect of this straight tube shape cavity is circular; The xsect of upper piston 2 and lower piston 3 is also circular; In Fig. 1, below this straight tube shape cavity, be provided with stepped hole in powder container 1, radial dimension and this stepped hole of the end that lower piston 3 contacts with tested powder are suitable; The straight tube shape cavity of the radial dimension of the end that upper piston 2 contacts with tested powder and powder container 1 is suitable, upper piston 2 is provided with the vent port 4 that the straight tube shape cavity with powder container 1 is communicated with space outerpace, this conductivity measuring apparatus is used for measuring the conductivity of graphite material, and the aperture of vent port 4 is Φ 1.5mm (can select in the scope of Φ 1-2mm).Powder container 1 adopts the insulation material, and the internal diameter of its straight tube shape cavity is chosen as 10mm to 50mm; The material of upper piston 2 and lower piston 3 is copper.
As shown in Figure 1, during work, lower piston 3 is inserted the stepped hole of powder container 1 lower end, and the lower end of lower piston 3 is placed on sheeter, then the straight tube shape cavity to powder container 1 adds a certain amount of natural spherical powder graphite 5 (D
50Be 21 μ m, carbon content is 99.95%), then fill in upper piston 2 from the upper end of straight tube shape cavity; Sheeter applies certain pressure from the up and down both direction to upper piston 2 and lower piston 3 respectively, and (force value is determined according to pressure or design pressure that natural spherical powder graphite 5 is subject to battery, can select in 0-10MPa) natural spherical powder graphite 5 length to the straight tube shape cavity stable (this moment natural spherical powder graphite 5 keep stable cylindrical shapes), measure the resistance of this moment 3 of upper piston 2 and lower pistons with DC resistance meter, obtain resistance value R.The resistance value of copper upper piston 2 and lower piston 3 itself is very low, can ignore, and resistance value R can see the resistance value of the natural spherical powder graphite 5 in straight tube shape cavity as.Measuring at this moment, upper piston 2 stretches into the interior length of straight tube shape cavity, length in straight tube shape cavity deducts upper piston 2 and stretches into the length L that the interior length of straight tube shape cavity is the column graphite composite powder, the cross-sectional area of the straight tube shape cavity of powder container 1 is S, by following formula:
σ＝L/(R×S)
Calculate the conductivity of graphite composite powder.
Change sheeter and be applied to force value on upper piston 2 and lower piston 3, measure according to the method described above and calculate the conductivity of graphite composite powder under the different pressures value, the relation that the conductivityσ of tested native graphite powder changes with pressure P is as shown in Fig. 2 and table one.
The conductivity of the tested native graphite powder of table one.Relation with pressure P
| Pressure (KPa) | 3.981 | 5.349 | 6.074 | 6.482 | 7.867 |
| Conductivity of graphite (S/m) | 14.82 | 21.97 | 44.92 | 52.99 | 79.96 |
Adopt conductivity measuring apparatus and the measuring method of the present embodiment, powder body material low to plasticity such as graphite, that processability is poor, compressing tablet is difficult carries out conductivity measurement smoothly, but and the conductivity under the pressured state of the tested powder of quantitative measurement in battery, for the judgement of the powder electric conductivities such as graphite provides immediate data.
By changing tested powder pressure value, measure the conductivity of tested powder under each force value, obtain the pressure-dependent relation of tested powder conductivity, help electrode material selection, the optimization of electrode material formula and the global design of battery system.
The conductivity measuring apparatus of the present embodiment and measuring method also are applicable to other powder outside graphite.
Embodiment two
Fig. 3 shows the another kind of embodiment of conductivity measuring apparatus of the present invention.
Comparison diagram 1 and Fig. 3, the difference of this conductivity measuring apparatus and embodiment one is: on upper piston 2 and lower piston 3 separately away from the taper that is shaped as of an end of tested powder.
During test, two of DC resistance meter calibrating terminals contact with lower piston 3 taper end points separately with upper piston 2 respectively, make between the taper end points of the calibrating terminal of DC resistance meter and upper piston 2 and lower piston 3 to keep less contact resistance, further guarantee measuring accuracy.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (7)
1. electrical conductivity of powdered material measuring method is characterized in that: comprise the following steps:
A, make tested powder keep column and apply certain pressure P by pressing machine to this column powder, keep dimensionally stable to this column powder; Step a realizes like this: tested powder is placed in straight tube shape cavity, from an end of this straight tube shape cavity or apply certain pressure P from the two ends of this straight tube shape cavity to tested powder simultaneously, concrete adopt two pistons from both sides with tested powder shutoff in described straight tube shape cavity and make tested powder keep column, one or two in these two pistons applies certain pressure P to tested powder, to tested powder maintenance dimensionally stable, two described pistons are resistance value electric conductor as can be known, and two described pistons end away from tested powder separately is taper;
Length L, the cross-sectional area S of b, measurement this column powder this moment, and the resistance value R of described column powder;
C, by following formula:
σ＝L/(R×S)
Calculate the conductivity of this column powder.
D, change pressure P, repeating step a, b and c under each force value obtain the sprills bulk conductivity value σ corresponding with each pressure P, correspondingly draw the relation that sprills bulk conductivity σ changes with pressure P.
2. electrical conductivity of powdered material measuring method according to claim 1, it is characterized in that: the process of measuring the resistance value R of described column powder in step b realizes like this: adopt resistance apparatus, during measurement two of this resistance apparatus calibrating terminals respectively with two described pistons end in contact away from tested powder separately, the resistance that the gained resistance data deducts two described pistons namely gets the resistance value R of described column powder.
3. electrical conductivity of powdered material measuring method according to claim 2, it is characterized in that: in described two pistons, at least one is provided with the vent port that described straight tube shape cavity is communicated with space outerpace, and the gas when described piston applies certain pressure P to tested powder in described straight tube shape cavity is discharged from this vent port.
4. electrical conductivity of powdered material measuring method according to claim 3, is characterized in that: material employing copper or the gold of two described pistons.
5. be suitable for the conductivity measuring apparatus of the described measuring method of claim 1, it is characterized in that: comprise with straight tube shape cavity and tested powder can be enclosed in described straight tube shape cavity with the powder container of tested powder insulation, two and make tested powder keep column the conduction piston, can be in two described pistons, at least one applies pressue device, the resistance apparatus of quantitative pressure, two described pistons end away from tested powder separately is taper.
6. conductivity measuring apparatus according to claim 5, it is characterized in that: in described two pistons, at least one is provided with the vent port that described straight tube shape cavity is communicated with space outerpace, and the gas when described piston applies certain pressure P to tested powder in described straight tube shape cavity is discharged from this vent port.
7. conductivity measuring apparatus according to claim 6, it is characterized in that: described piston is electric conductor; The material of two described pistons adopts copper or gold.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710075037 CN101324538B (en) | 2007-06-14 | 2007-06-14 | Method for measuring powder body material electric conductivity and electric conductivity measuring apparatus suitable for the method |
| HK09104487.3A HK1125696A1 (en) | 2007-06-14 | 2009-05-18 | Conductivity measuring method for powder material and conductivity measuring device thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200710075037 CN101324538B (en) | 2007-06-14 | 2007-06-14 | Method for measuring powder body material electric conductivity and electric conductivity measuring apparatus suitable for the method |
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| CN101324538A CN101324538A (en) | 2008-12-17 |
| CN101324538B true CN101324538B (en) | 2013-06-12 |
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| HK (1) | HK1125696A1 (en) |
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| RU2722574C1 (en) * | 2019-09-24 | 2020-06-01 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" (Госкорпорация "Росатом") | Contact device for determination of electrophysical parameters of powder material during its compression |
| RU207289U1 (en) * | 2021-06-04 | 2021-10-21 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Новосибирский Государственный Технический Университет" | CONDUCTIVITY MEASURING CELL COMPACTED MATERIALS |
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| CN101706529A (en) * | 2009-10-09 | 2010-05-12 | 上海微纳科技有限公司 | Device and method for testing conductivity of solid powder material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2722574C1 (en) * | 2019-09-24 | 2020-06-01 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" (Госкорпорация "Росатом") | Contact device for determination of electrophysical parameters of powder material during its compression |
| RU207289U1 (en) * | 2021-06-04 | 2021-10-21 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Новосибирский Государственный Технический Университет" | CONDUCTIVITY MEASURING CELL COMPACTED MATERIALS |
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| Publication number | Publication date |
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| HK1125696A1 (en) | 2009-08-14 |
| CN101324538A (en) | 2008-12-17 |
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