CN109884247A - A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry - Google Patents
A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry Download PDFInfo
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- CN109884247A CN109884247A CN201910093019.8A CN201910093019A CN109884247A CN 109884247 A CN109884247 A CN 109884247A CN 201910093019 A CN201910093019 A CN 201910093019A CN 109884247 A CN109884247 A CN 109884247A
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Abstract
The invention discloses a kind of methods of Fast Evaluation graphene composite conductive Stability of Slurry, comprising the following steps: takes electrocondution slurry to stir evenly, tests solid content, be denoted as W1；It takes the electrocondution slurry stirred evenly to be centrifuged, measures the solid content of upper slurry, be denoted as W2；Coefficient of stabilization S=W2/W1 is calculated, by coefficient of stabilization S come the stability of graphene composite conductive slurry described in Fast Evaluation.The present invention uses ultracentrifugal method, it can accelerate the infall process of slurry, so as to shorten the testing time, achieve the purpose that the stability for quickly determining electrocondution slurry, the present invention can highly precisely evaluate the stability of electrocondution slurry using the ratio of upper slurry solid content before and after high speed centrifugation.
Description
Technical field
The present invention relates to the technical field of evaluation electrocondution slurry stability more particularly to a kind of Fast Evaluation graphene are compound
The method of electrocondution slurry stability.
Background technique
With the exhaustion of traditional energy and becoming increasingly conspicuous for environmental problem, lithium ion battery is as new cleaning fuel
Attention of the developing direction increasingly by national governments and scientist is constantly dedicated to the more practical and efficient lithium of developmental research
Ion battery.The advantages that grapheme material is a kind of novel conductive agent, and conductive energy is excellent, additive amount is few, Ke Yiming
It is aobvious to improve amount of active mass, improve compacted density, play the work for reducing electrode reaction resistance and improving battery energy density
With.
Currently, electrocondution slurry is often the multiple elements design system of grapheme material, carbon nanotube, conductive black etc..Graphite
Two phase separations in alkene material paste between grapheme material, dispersing agent and solvent there are solid-liquid enable graphene sheet layer to stablize point
Dissipate in a liquid, but with the extension of period of storage or the variation of storage requirement, in grapheme material slurry it is this it is solid-
The stability of liquid effect gradually decreases, and causes graphene in slurry that sedimentation occurs and reunites, different material particle is in whole system
In be unevenly distributed, less efficient dispersal, this makes the function of slurry have a greatly reduced quality.Therefore, the storage stability of electrocondution slurry
It is an important index, this is directly related to the using effect of product.
However, graphene composite conductive slurry is as a kind of brand-new material, existing frequently-used is to carry out electrocondution slurry standing
The variation for observing slurry, since electrocondution slurry has certain viscosity, standing process needs long time, generally requires 3-6
A month, the method for rapidly judging to its stability is lacked in existing test method and standard.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of Fast Evaluation graphene composite conductive slurries
The method of stability, the present invention use ultracentrifugal method, can accelerate the infall process of slurry, so as to shorten test
Time achievees the purpose that the stability for quickly determining electrocondution slurry, and the present invention is using upper slurry solid content before and after high speed centrifugation
Ratio can highly precisely evaluate the stability of electrocondution slurry.
A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry proposed by the present invention, comprising the following steps:
S1, it takes electrocondution slurry to stir evenly, tests solid content, be denoted as W1；
S2, it takes the electrocondution slurry stirred evenly to be centrifuged, measures the solid content of upper slurry, be denoted as W2；
S3, coefficient of stabilization S=W2/W1 is calculated, the stabilization of the graphene composite conductive slurry is evaluated by coefficient of stabilization S
Property.
Preferably, in S1, the electrocondution slurry is oleaginous system or water-based system.
Preferably, it is 50-100% that grapheme material, which accounts for the ratio of conductive material, in S1, in the electrocondution slurry, conductive
The solid content of slurry is 3-8%.
Preferably, in S1, S2, the test method of solid content is oven drying method, weighs stock quality to be measured and is calculated as G1, then
It is laid on aluminium foil, is put into 110-130 DEG C of baking oven baking 40-80min to claim its quality to be calculated as G2, G2/ after cooling up to constant weight
The ratio of G1 is solid content.
Preferably, in S1, speed of agitator 800-1200rpm, mixing time 2-4h.
Preferably, in S2, the revolving speed of centrifugation is 500-8000rpm, centrifugation time 5-15min.
Preferably, in S3, the coefficient of stabilization S of calculating and evaluation criterion are compared, to judge the graphene composite conductive
The stability of slurry.
Wherein it is preferred to can be carried out using following but not unique mode during establishing evaluation criterion:
Standing shelf test is carried out to Qingdao Hao Xin New Energy Technology Co., Ltd. HX-G6 type oiliness electrocondution slurry, is tested
The solid content on slurry upper layer after placement 0d, 7d, 15d, 30d, 60d, 90d, defining coefficient of stabilization is different storage number of days and the upper layer 0d
The ratio of slurry solid content, as a result as follows:
| Stand number of days | 0d | 7d | 15d | 30d | 60d | 90d |
| Upper layer solid content | 6.11% | 6.10% | 6.11% | 6.10% | 6.09% | 6.03% |
| Coefficient of stabilization | 100% | 99.84% | 100% | 99.84% | 99.67% | 98.69% |
From test result as can be seen that upper slurry solid content by 6.11% is reduced to 6.03% after slurry storage 90d, surely
Determining rate is 98.69%, and solid content varies less, it is believed that it is stable.
Will after the electrocondution slurry after mixing evenly high speed centrifugation test upper slurry solid content, centrifugation time 10min,
Centrifugal rotational speed is respectively 0rpm, 500rpm, 1000rpm, 2000rpm, 4000rpm, 8000rpm, then calculates solid content and stablizes
Rate, defining coefficient of stabilization is the ratio after different rotating speeds are centrifuged with 0rpm upper slurry solid content, as a result as follows:
| Centrifugal rotational speed | 0rpm | 500rpm | 1000rpm | 2000rpm | 4000rpm | 8000rpm |
| Upper layer solid content | 6.11% | 6.11% | 6.01% | 5.69% | 5.22% | 4.01% |
| Coefficient of stabilization | 100% | 100% | 98.36% | 93.13% | 85.43% | 65.63% |
Likewise, carrying out standing shelf test to Shenzhen alkene power Science and Technology Ltd. XDLI type electrocondution slurry, test is put
The solid content on slurry upper layer after 0d, 7d, 15d, 30d, 60d, 90d is set, defining coefficient of stabilization is different storage number of days and the upper layer 0d slurry
Expect the ratio of solid content, as a result as follows:
| Stand number of days | 0d | 7d | 15d | 30d | 60d | 90d |
| Upper layer solid content | 6.03% | 6.00% | 5.97% | 5.80% | 5.71% | 5.60% |
| Coefficient of stabilization | 100% | 99.50% | 99.01% | 96.19% | 94.69% | 92.87% |
From test result as can be seen that upper slurry solid content by 6.03% is reduced to 5.72% after slurry storage 90d, surely
Determining rate is 92.87%, and solid content variation is relatively large, more than 5%, it is believed that it is not sufficiently stable.
Will after the electrocondution slurry after mixing evenly high speed centrifugation test upper slurry solid content, centrifugation time 10min,
Centrifugal rotational speed is respectively 0rpm, 500rpm, 1000rpm, 2000rpm, 4000rpm, 8000rpm, then calculates solid content and stablizes
Rate, defining coefficient of stabilization is the ratio after different rotating speeds are centrifuged with 0rpm upper slurry solid content, as a result as follows:
| Centrifugal rotational speed | 0rpm | 500rpm | 1000rpm | 2000rpm | 4000rpm | 8000rpm |
| Upper layer solid content | 6.03% | 6.03% | 5.88% | 3.80% | 2.76% | 1.65% |
| Coefficient of stabilization | 100% | 100% | 97.51% | 63.02% | 45.77% | 27.36% |
After standing experiment and centrefuge experiment by above-mentioned two electrocondution slurry, stable slurry and unstable slurry have substantially been obtained
The coefficient of stabilization range of upper slurry solid content widely counts temporarily using it as evaluation criterion in the later period after material different rotating speeds centrifugation
It is accurate according to being continued to optimize after accumulation.
By comparative evaluation's standard, coefficient of stabilization is greater than stability criterion and then thinks slurry within a certain period of time and be stable, surely
Determine rate and then think slurry within a certain period of time less than unstable standard to be unstable.The evaluation criterion of coefficient of stabilization can be continuous
Optimization is accurate, and the more big then Stability of Slurry of coefficient of stabilization is better, and coefficient of stabilization is greater than stability criterion and then thinks slurry within a certain period of time
Be it is stable, coefficient of stabilization is less than unstable standard, and then to think slurry within a certain period of time be unstable.
Compared with prior art, the beneficial effects of the present invention are:
The first, for the present invention by the sedimentation of high speed centrifugation acceleration electrocondution slurry, high speed centrifugation is the high speed by centrifuge
Operating, making centrifugal acceleration is more than hundreds and thousands of times of acceleration of gravity, and increases sinking speed, to accelerate particle in slurry
Precipitating shortens the testing time to reach.
The second, the present invention passes through the ratio for calculating centrifugation front and back electrocondution slurry upper slurry solid content, and and evaluation criterion
Compare, and then judge the stability of slurry, can quantify and extremely accurate evaluate the stability of slurry, and contrast standard can
It is accurate to continue to optimize.
Third, judgment method of the invention are with simple and quick, the testing time is short, test result is accurate, practicability
The advantages that strong.
Detailed description of the invention
Fig. 1 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 1, and compared with reference line.
Fig. 2 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 2, and compared with reference line.
Fig. 3 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 3, and compared with reference line.
Fig. 4 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 4, and compared with reference line.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry, comprising the following steps:
S1,150mL oiliness graphene composite conductive slurry is taken to be placed in the beaker of 250mL, electrocondution slurry solid content is
6%, it is stirred evenly using churned mechanically mode, speed of agitator 1000rpm, mixing time 3h, testing conductive slurry
Solid content is denoted as W1；
S2, the electrocondution slurry stirred evenly in right amount is taken to be placed in the centrifuge tube of 10mL, high speed centrifugation, centrifugation time is
10min, centrifugal rotational speed are respectively 500rpm, 1000rpm, 2000rpm, 4000rpm, 8000rpm, then measure upper slurry
Solid content is denoted as W2；
S3, coefficient of stabilization S=W2/W1 is calculated, and judges the stability of slurry with Comparison of standards, coefficient of stabilization is greater than stability criterion
Then think slurry within a certain period of time and be stable, it is not that coefficient of stabilization, which is less than unstable standard then to think slurry within a certain period of time,
Stable.
Fig. 1 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 1, and compared with reference line, as can be seen from the results,
The coefficient of stabilization of the slurry is greater than the reference line of stable slurry, therefore thinks that the slurry is stable.
Embodiment 2
A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry, comprising the following steps:
S1,150mL oiliness graphene composite conductive slurry is taken to be placed in the beaker of 250mL, electrocondution slurry solid content is about
6%, it is stirred evenly using churned mechanically mode, speed of agitator 1000rpm, mixing time 3h, testing conductive slurry
Solid content is denoted as W1；
S2, the electrocondution slurry stirred evenly in right amount is taken to be placed in the centrifuge tube of 10mL, high speed centrifugation, centrifugation time is
10min, centrifugal rotational speed are respectively 500rpm, 1000rpm, 2000rpm, 4000rpm, 8000rpm, then measure upper slurry
Solid content is denoted as W2；
S3, coefficient of stabilization S=W2/W1 is calculated, and judges the stability of slurry with Comparison of standards, coefficient of stabilization is greater than stability criterion
Then think slurry within a certain period of time and be stable, it is not that coefficient of stabilization, which is less than unstable standard then to think slurry within a certain period of time,
Stable.
Fig. 2 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 2, and compared with reference line, as can be seen from the results,
The coefficient of stabilization of the slurry is less than the reference line of unstable slurry, therefore thinks that the slurry is unstable.
Embodiment 3
A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry, comprising the following steps:
S1,150mL oiliness graphene composite conductive slurry is taken to be placed in the beaker of 250mL, electrocondution slurry solid content is about
6%, it is stirred evenly using churned mechanically mode, speed of agitator 1000rpm, mixing time 3h, testing conductive slurry
Solid content is denoted as W1；
S2, the electrocondution slurry stirred evenly in right amount is taken to be placed in the centrifuge tube of 10mL, high speed centrifugation, centrifugation time is
10min, centrifugal rotational speed are respectively 500rpm, 1000rpm, 2000rpm, 4000rpm, 8000rpm, then measure upper slurry
Solid content is denoted as W2；
S3, coefficient of stabilization S=W2/W1 is calculated, and judges the stability of slurry with Comparison of standards, coefficient of stabilization is greater than stability criterion
Then think slurry within a certain period of time and be stable, it is not that coefficient of stabilization, which is less than unstable standard then to think slurry within a certain period of time,
Stable.
Fig. 3 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 3, and compared with reference line, as can be seen from the results,
The coefficient of stabilization of the slurry can not temporarily determine whether the slurry is stable between stable slurry and unstable slurry reference line.
It is obtained by standing storage experiment, slurry upper layer solid content is 94.15% after storage 90 days, less than 95%, therefore thinks the slurry
Be it is unstable, the subsequent reference line by unstable slurry is changed to the data of the embodiment.
Embodiment 4
A kind of method of Fast Evaluation graphene composite conductive Stability of Slurry, comprising the following steps:
S1,150mL oiliness graphene composite conductive slurry is taken to be placed in the beaker of 250mL, electrocondution slurry solid content is about
6%, it is stirred evenly using churned mechanically mode, speed of agitator 1000rpm, mixing time 3h, testing conductive slurry
Solid content is denoted as W1；
S2, the electrocondution slurry stirred evenly in right amount is taken to be placed in the centrifuge tube of 10mL, high speed centrifugation, centrifugation time is
10min, centrifugal rotational speed are respectively 500rpm, 1000rpm, 2000rpm, 4000rpm, 8000rpm, then measure upper slurry
Solid content is denoted as W2；
S3, coefficient of stabilization S=W2/W1 is calculated, and judges the stability of slurry with Comparison of standards, coefficient of stabilization is greater than stability criterion
Then think slurry within a certain period of time and be stable, it is not that coefficient of stabilization, which is less than unstable standard then to think slurry within a certain period of time,
Stable.
Fig. 4 is the coefficient of stabilization that the slurry under different rotating speeds is calculated in embodiment 4, and compared with reference line, as can be seen from the results,
The coefficient of stabilization of the slurry can not temporarily determine whether the slurry is stable between stable slurry and unstable slurry reference line.
It is obtained by standing storage experiment, slurry upper layer solid content is 96.46% after storage 90 days, is greater than 95%, therefore thinks the slurry
It is stable, the subsequent data that the reference line of stable slurry is changed to the embodiment.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of method of Fast Evaluation graphene composite conductive Stability of Slurry, which comprises the following steps:
S1, it takes electrocondution slurry to stir evenly, tests solid content, be denoted as W1；
S2, it takes the electrocondution slurry stirred evenly to be centrifuged, measures the solid content of upper slurry, be denoted as W2；
S3, coefficient of stabilization S=W2/W1 is calculated, by coefficient of stabilization S come the stabilization of graphene composite conductive slurry described in Fast Evaluation
Property.
2. the method for Fast Evaluation graphene composite conductive Stability of Slurry according to claim 1, which is characterized in that
In S1, the electrocondution slurry is oleaginous system or water-based system.
3. the method for Fast Evaluation graphene composite conductive Stability of Slurry according to claim 1, which is characterized in that
In S1, the mass ratio that grapheme material accounts for conductive material in the electrocondution slurry is 50-100%, and the solid content of electrocondution slurry is
3-8%.
4. the method for Fast Evaluation graphene composite conductive Stability of Slurry according to claim 1, which is characterized in that
In S1, S2, the test method of solid content is oven drying method, weighs stock quality to be measured and is calculated as G1, is then laid on aluminium foil, is put into
110-130 DEG C of baking oven baking 40-80min after cooling to claim its quality to be calculated as G2, the ratio of G2/G1 as contains admittedly up to constant weight
Amount.
5. the method for Fast Evaluation graphene composite conductive Stability of Slurry according to claim 1, which is characterized in that
In S1, speed of agitator 800-1200rpm, mixing time 2-4h.
6. the method for Fast Evaluation graphene composite conductive Stability of Slurry according to claim 1, which is characterized in that
In S2, the revolving speed of centrifugation is 500-8000rpm, centrifugation time 5-15min.
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Cited By (1)
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| CN112161900A (en) * | 2020-09-23 | 2021-01-01 | 东莞瑞泰新材料科技有限公司 | Method for rapidly measuring anti-settling property of graphene slurry |
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Application publication date: 20190614 |