CN106353352A - Detection method for dispersion effect of carbon material in lead-acid storage battery - Google Patents
Detection method for dispersion effect of carbon material in lead-acid storage battery Download PDFInfo
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- CN106353352A CN106353352A CN201610888322.3A CN201610888322A CN106353352A CN 106353352 A CN106353352 A CN 106353352A CN 201610888322 A CN201610888322 A CN 201610888322A CN 106353352 A CN106353352 A CN 106353352A
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- lead
- dispersion effect
- carbon element
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
Abstract
The invention relates to the technical field of detection for the distribution condition of additives in solid matters. According to a detection method for a dispersion effect of a carbon material in a lead-acid storage battery, the dispersion effect of the carbon material in lead plaster is observed in the manner of combining an electron microscope energy spectrum element image before polar plate treatment with an electron microscope image of the polar plate after treatment, and the size and distribution uniformity of active matter grains after being treated are the factors influencing the dispersion effect of the carbon material. The invention provides a test method for quickly, efficiently and accurately making people directly feel and observe the dispersion effect of the carbon material in the lead plaster. The technical problems of the prior art that the time for detecting the dispersion effect of the carbon material is long, the detection accuracy is low and the dispersion effect cannot be directly observed and judged are solved.
Description
Technical field
The present invention relates to a kind of additive in solid matter distribution situation detection technique field and in particular to a kind of carbon materials
The detection method of material dispersion effect in lead-acid accumulator.
Background technology
Lead-acid battery has had the history of 130 years, has dependable performance, mature production technology, compared with Ni-MH battery and lithium electricity
Pond low cost and other advantages.The current electric bicycle overwhelming majority is using sealing-type lead-acid battery.Sealing-type lead-acid battery is
Positive and negative pole plate interfolded is arranged in battery case, is isolated with insulating barrier between positive and negative pole plate, when electrolyte fills
Enter in battery case, electrolyte carries out chemical reaction with the lead on positive and negative pole plate.When battery charges, become the positive and negative of lead sulfate
Lead on two-plate is discharged into the sulfuric acid components being fixed therein in electrolyte, respectively becomes lead and lead oxide, makes electrolyte
In sulfuric acid concentration be continuously increased, voltage rise, put aside energy；The lead on lead oxide and negative plate during electric discharge, in positive plate
React with the sulphuric acid in electrolyte and become lead sulfate, so that the sulfuric acid concentration in electrolyte is constantly reduced, voltage decline so that
Energy reduces, and battery externally exports energy, therefore the cycle charge-discharge of battery is the process that electric energy and chemical energy are constantly changed,
Finally realize storage and the release of energy.
Valve-regulated lead-acid battery so that it is cheap, safely, be not required to the features such as mend electrolyte, electric vehicle is widely applied.
Battery generally requires series connection and uses in groups, and the overall performance of accumulator battery depends on the worst section of performance in whole group battery, such as
The performance of a whole set of accumulator battery of fruit has big difference, and causes the discreteness of this accumulator battery, thus result in accumulator battery losing too early
Effect, short life, therefore need battery with two side terminals is lifted, to ensure performance and the life-span of whole accumulator battery.In battery
The deployment conditions of internal additives directly influence the overall performance of battery.As Chinese patent: " a kind of acid accumulator negative pole lead adds
Plus agent and preparation method thereof (cn104022287a) ", described additive is stratiform carbon/oxidation lead composite material, layered
The number of plies of carbon is 1-50 layer, and particles of lead oxide is uniformly adhered on stratiform carbon, and the size of described particles of lead oxide is 5-
The mass ratio of 200nm, layered carbon and lead oxide is 1: 1-200.
With the development of research and development science and technology, product quality requires also more and more stricter.To raising inside battery additive
Dispersion situation also serves as a kind of important approach improving battery performance.The dispersion situation of additive is better, the property of lead battery
Can be more stable, this to inside battery material with carbon element dispersibility investigate and dispersibility detection accuracy, convenience, efficiency propose more
High requirement.
At present dispersion effect detection in lead-acid accumulator for the material with carbon element mainly adopts metallography microscope sem observation or thick
The data that rugosity tester the is measured method such as display indirectly, and existed using the dispersion effect that such method detects material with carbon element
Check-Out Time is long, and accuracy in detection is low and can not intuitively go to embody the aspects such as dispersion effect in lead plaster for the material with carbon element
Problem.
Content of the invention
The invention provides one kind can effectively, quick, accurately and people's direct feel can be allowed to observe material with carbon element in lead plaster point
The method of testing of scattered effect；Solve present in prior art detect material with carbon element the dispersion effect time long, detection accurate
Degree the is it is impossible to directly observe the technical problem of judgement.
The above-mentioned technical problem of the present invention is solved by following technical proposals: a kind of material with carbon element is in lead-acid accumulator
The detection method of dispersion effect it is characterised in that: comprise the following steps:
The first step: material with carbon element is added in Hydrocerussitum (Ceruse) as cathode additive agent, mixs homogeneously with Hydrocerussitum (Ceruse) and obtain mixing lead plaster；
Second step: the ripe pole plate scribbling mixing lead plaster is assembled into battery, is then discharged, after electric discharge completely, ripe pole plate is dried
Dry be prepared into measuring samples, measuring samples are put into scanning electron microscope sample room and are observed, scanning shoot sample drawing, open
Kinetic Energy Spectrum tester carries out elementary analysiss to test sample, draws carbon distribution spectrogram；
3rd step: carry out processing lead sulfate therein using chemical reagent by preserving complete sample after testing electronic microscope
Grain, is observed after undissolved sample active dried again under a scanning electron microscope, adjusts scanning electron
Microscopical sweep parameter, shoots sample pictures；
4th step: the mode that after sample active being scanned with power spectrum distribution diagram of element and processing, scanning electron microscope (SEM) photograph combines is carried out
Analysis material with carbon element distribution situation.
Pole plate electron microscope picture after ultramicroscope power spectrum elemental map to pole plate before processing and process combines
Mode observing dispersion effect in lead plaster for the material with carbon element, find impact material with carbon element dispersion effect the form of expression be process after
Active substance particle size and distributing homogeneity, when active material particle apparent size is larger and skewness, show here
In the range of material with carbon element distribution less and disperse uneven；When active material particle apparent size is less and scope in be evenly distributed, table
It is bright that material with carbon element distribution is more sufficient in the range of this and is uniformly dispersed.
Preferably, in the described first step, addition in Hydrocerussitum (Ceruse) for the material with carbon element is the 0.1 ~ 2% of Hydrocerussitum (Ceruse) weight.
Preferably, in the described first step, material with carbon element is passed through concussion alr mode mixing homogeneously with Hydrocerussitum (Ceruse), concussion is stirred
Mixing speed is 120 ~ 240r/min, mixing time 10-20 minute.
Preferably, scanning adopts high power camera lens, accelerating potential during electron microscope scanning in described second step
It is worth for 10kv ~ 30kv, working focal distance is 12 ~ 25mm.
Preferably, when again electron microscope scanning being carried out to undissolved active substance in the 3rd described step, sweeping
Retouch and adopt low power lens, accelerating potential value is 3kv ~ 10kv, working focal distance is 5 ~ 15mm.Chemical reagent in the 3rd described step
For sodium acetate solution or nitric acid and hydrogen peroxide agent.Adopt Surface scan in sample after chemical reagent process for the 3rd step
Mode gather Elemental redistribution.
Preferably, material with carbon element in the described first step be activated carbon, in acetylene black, Graphene, CNT, white carbon black
One or more.
Therefore, a kind of material with carbon element of present invention detection method of dispersion effect in lead-acid accumulator possesses following advantages:
1st, the present invention adopt scanning electron microscope Spectrum acquisition element gather distribution situation in pole plate for the carbon, simultaneously with
The mode that in pole plate after process, lead sulfate particle size and distributing homogeneity combine is judging material with carbon element in lead plaster
Dispersion effect, can quick, intuitive and accurate the dispersibility of material with carbon element be characterized.Using Spectrum acquisition Elemental redistribution and
The judgement detection mode that the electric discharge pole plate lead sulfate particle size of post processing and distributing homogeneity combine is simple to operate, clap
It is clear to take the photograph, and electron microscope and power spectrum Elemental redistribution can intuitively observe the phenotypic forms of material with carbon element dispersion effect, thus drawing accurately
Judgement.
2nd, the present invention can quickly and intuitively judge the overall dispersibility of material with carbon element, will prepare under different technology conditions
Sample carry out parallel control, search out the reason lead to poor dispersion, such that it is able to Instructing manufacture, be easy to targetedly
Carry out production technology improvement.
Brief description
Fig. 1 is untreated pole plate sample carbon distributed effect energy spectrum diagram in embodiment 1.
Fig. 2 is Fig. 1 untreated pole plate sample Electron microscope scanning figure.
Fig. 3 be in Fig. 1 through chemical reagent process after pole plate sample Electron microscope scanning figure.
Fig. 4 is untreated pole plate sample carbon distributed effect energy spectrum diagram in embodiment 2.
Fig. 5 is Fig. 2 untreated pole plate sample Electron microscope scanning figure.
Fig. 6 be in Fig. 2 through chemical reagent process after pole plate sample Electron microscope scanning figure.
Specific embodiment
Below by embodiment, and combine accompanying drawing, the technical scheme of invention is described in further detail.
Embodiment 1:
A kind of detection method of material with carbon element dispersion effect in lead-acid accumulator, the method has a following operating procedure:
The first step, takes 10 grams of carbon blacks to be added in 10 kilograms of Hydrocerussitum (Ceruse), is at the uniform velocity stirred 15 minutes, stirring by the way of concussion stirring
Speed is 180r/min, obtains mixing lead plaster after mix homogeneously；
Second step, is discharged to cell voltage after the battery connection line that the ripe pole plate scribbling above-mentioned mixing lead plaster is assembled completely
1.8v/ single lattice, takes out the sample active being prepared into 2*2*0.5cm after its ripe pole plate rinses drying.By sample active
Put into the sample room of scanning electron microscope together with microscope slide, adjust scanning electron microscope parameter: using high power camera lens, acceleration
Voltage is 20kv, and working focal distance is 20mm, the parameter setting of amplification × 1000, energy-spectrum scanning parameter and electron scanning parameter
It is consistent, pattern is Surface scan, scanning frame number is 64 frames.Draw its carbon distribution energy spectrum diagram (as shown in Figure 1) and electronics
Microscope scanning figure (as shown in Figure 2)；
3rd step, carries out processing the sulphuric acid that sample contains above by having tested power spectrum and having preserved complete sample and receive solution using acetic acid
Lead bulky grain, is observed after undissolved sample active dried, adjustment is swept again under a scanning electron microscope
Retouch the sweep parameter of ultramicroscope: it is 5kv using low power lens, accelerating potential, working focal distance is 5mm, amplification ×
1000 parameter setting, shoots the electron microscope scanning figure (as shown in Figure 3) of sample；
4th step, the mode that after sample active being scanned with power spectrum distribution diagram of element and processing, scanning electron microscope (SEM) photograph combines is carried out
Analysis material with carbon element distribution situation, observes dispersion effect and the relevant surfaces characteristic of material with carbon element, draws accurate material with carbon element dispersibility
Data.
Embodiment 2:
A kind of detection method of material with carbon element dispersion effect in lead-acid accumulator, the method has a following operating procedure:
The first step, takes 70 grams of activated carbons and the mixture of 30 grams of acetylene blacks to be added in 10 kilograms of Hydrocerussitum (Ceruse), using concussion stirring
Mode at the uniform velocity stirs 18 minutes, and stir speed (S.S.) is 220r/min, obtains mixing lead plaster after mix homogeneously；
Second step, is discharged to cell voltage after the battery connection line that the ripe pole plate scribbling above-mentioned mixing lead plaster is assembled completely
1.8v/ single lattice, takes out the sample active being prepared into 1.5*1.5*0.8cm after its ripe pole plate rinses drying.By active substance
Sample puts into the sample room of scanning electron microscope together with microscope slide, adjusts scanning electron microscope parameter: using high power camera lens,
Accelerating potential is 25kv, and working focal distance is 25mm, the parameter setting of amplification × 1000, energy-spectrum scanning parameter and electron scanning
Parameter is consistent, and pattern is Surface scan, and scanning frame number is 64 frames.Draw its carbon distribution energy spectrum diagram (as shown in Figure 4) and
Electron microscope scanning figure (as shown in Figure 5)；
3rd step, carries out processing the sulphuric acid that sample contains above by having tested power spectrum and having preserved complete sample and receive solution using acetic acid
Lead bulky grain, is observed after undissolved sample active dried, adjustment is swept again under a scanning electron microscope
Retouch the sweep parameter of ultramicroscope: it is 8kv using low power lens, accelerating potential, working focal distance is 10mm, amplification ×
1000 parameter setting, shoots the electron microscope scanning figure (as shown in Figure 6) of sample；
4th step, the mode that after sample active being scanned with power spectrum distribution diagram of element and processing, scanning electron microscope (SEM) photograph combines is carried out
Analysis material with carbon element distribution situation, observes dispersion effect and the relevant surfaces characteristic of material with carbon element, draws accurate material with carbon element dispersibility
Data.
Embodiment described above is a kind of preferred version of the present invention, and not the present invention is done with any pro forma limit
System, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (8)
1. a kind of material with carbon element dispersion effect in lead-acid accumulator detection method it is characterised in that: comprise the following steps:
The first step: material with carbon element is added in Hydrocerussitum (Ceruse) as cathode additive agent, mixs homogeneously with Hydrocerussitum (Ceruse) and obtain mixing lead plaster；
Second step: the ripe pole plate scribbling mixing lead plaster is assembled into battery, is then discharged, after electric discharge completely, ripe pole plate is dried
Dry be prepared into measuring samples, measuring samples are put into scanning electron microscope sample room and are observed, scanning shoot sample drawing, open
Kinetic Energy Spectrum tester carries out elementary analysiss to test sample, draws carbon distribution spectrogram；
3rd step: carry out processing lead sulfate therein using chemical reagent by preserving complete sample after testing electronic microscope
Grain, is observed after undissolved sample active dried again under a scanning electron microscope, adjusts scanning electron
Microscopical sweep parameter, shoots sample pictures；
4th step: the mode that after sample active being scanned with power spectrum distribution diagram of element and processing, scanning electron microscope (SEM) photograph combines is carried out
Analysis material with carbon element distribution situation.
2. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1, its feature exists
In: in the described first step, addition in Hydrocerussitum (Ceruse) for the material with carbon element is the 0.1 ~ 2% of Hydrocerussitum (Ceruse) weight.
3. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1 and 2, its feature
Be: in the described first step, material with carbon element is passed through to shake alr mode and mixs homogeneously with Hydrocerussitum (Ceruse), concussion stir speed (S.S.) for 120 ~
240r/min, mixing time 10-20 minute.
4. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1 and 2, its feature
Be: during electron microscope scanning in described second step scanning adopt high power camera lens, accelerating potential value be 10kv ~
30kv, working focal distance is 12 ~ 25mm.
5. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1 and 2, its feature
It is: when carrying out electron microscope scanning again to undissolved active substance in the 3rd described step, scanning adopts low power lens
Head, accelerating potential value is 3kv ~ 10kv, and working focal distance is 5 ~ 15mm.
6. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1 and 2, its feature
It is: the chemical reagent in the 3rd described step is sodium acetate solution or nitric acid and hydrogen peroxide agent.
7. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1 and 2, its feature
It is: the material with carbon element in the described first step is one of activated carbon, acetylene black, Graphene, CNT, white carbon black or many
Kind.
8. the detection method of a kind of material with carbon element dispersion effect in lead-acid accumulator according to claim 1 and 2, its feature
It is: gather Elemental redistribution by the way of Surface scan in sample after chemical reagent process for the 3rd step.
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| CN201610888322.3A CN106353352B (en) | 2016-10-11 | 2016-10-11 | Method for detecting dispersion effect of carbon material in lead-acid storage battery |
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Cited By (4)
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| CN107290292A (en) * | 2017-05-26 | 2017-10-24 | 超威电源有限公司 | The detection method of additive dispersion effect in lead plaster in a kind of lead-acid accumulator |
| CN107611446A (en) * | 2017-09-20 | 2018-01-19 | 厦门稀土材料研究所 | A kind of liberation of hydrogen inhibitor, preparation method and applications |
| CN109916941A (en) * | 2019-03-25 | 2019-06-21 | 苏州大学 | A kind of premixing powder 3D printing method for separating and detecting |
| CN111323417A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Rapid detection method and rapid determination method for storage stability of graphene material dispersion liquid |
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| CN105161770A (en) * | 2015-08-18 | 2015-12-16 | 超威电源有限公司 | Lead plaster additive for lead-acid storage battery, and preparation method and application therefor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107290292A (en) * | 2017-05-26 | 2017-10-24 | 超威电源有限公司 | The detection method of additive dispersion effect in lead plaster in a kind of lead-acid accumulator |
| CN107290292B (en) * | 2017-05-26 | 2020-02-14 | 超威电源集团有限公司 | Method for detecting dispersion effect of additive in lead-acid storage battery in lead plaster |
| CN107611446A (en) * | 2017-09-20 | 2018-01-19 | 厦门稀土材料研究所 | A kind of liberation of hydrogen inhibitor, preparation method and applications |
| CN111323417A (en) * | 2018-12-13 | 2020-06-23 | 山东欧铂新材料有限公司 | Rapid detection method and rapid determination method for storage stability of graphene material dispersion liquid |
| CN109916941A (en) * | 2019-03-25 | 2019-06-21 | 苏州大学 | A kind of premixing powder 3D printing method for separating and detecting |
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| CN106353352B (en) | 2019-12-06 |
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