CN107271386A - A kind of method for setting up graphene Stability of Slurry characterization model - Google Patents
A kind of method for setting up graphene Stability of Slurry characterization model Download PDFInfo
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- CN107271386A CN107271386A CN201710439466.5A CN201710439466A CN107271386A CN 107271386 A CN107271386 A CN 107271386A CN 201710439466 A CN201710439466 A CN 201710439466A CN 107271386 A CN107271386 A CN 107271386A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3185—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry typically monochromatic or band-limited
- G01N2021/3188—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry typically monochromatic or band-limited band-limited
Abstract
The invention discloses a kind of method for setting up graphene Stability of Slurry characterization model, including：S1:Slurry sample is placed in cylindrical container, and divides the sample line of upper, middle and lower three to the sample in cylinder；S2:Respectively from the sample line position sample of upper, middle and lower three, and it is diluted to identical multiple；Test the absorbance of slurry after dilution, loading absorbance is designated as A1, middle sample absorbance and is designated as A2, lower sample absorbance being designated as A3；S3：Above-mentioned slurry was deposited after certain time, the absorbance of upper, middle and lower sampling is carried out according to S2 method；Over time elongated, can repeatedly test the absorbance of storage slurry upper, middle and lower sampling；S4：Take ratio A3/A1, A2/A1 or A3/A2 as settlement parameter, obtain the relation curve of settlement parameter A3/A1, A2/A1 time corresponding with A3/A2, be graphene Stability of Slurry characterization model of the present invention.
Description
Technical field
The present invention relates to a kind of characterizing method of graphene Stability of Slurry, belong to detection method field.
Background technology
Graphene slurry is the liquid composite material using graphene as principle active component, and the application day of graphene slurry is new
The moon is different, for example, be applied to energy field as conductive additive, is applied to the fields such as electronic device as function ink, is used as work(
Energy reinforcing agent is applied to paint field etc..Wherein, the bin stability of graphene slurry is an important index.With dissolving
State is different, and two phase separations that there is solid-liquid between graphene and solvent enable graphene sheet layer stable dispersion in a liquid, still
With the extension or the change of storage requirement of period of storage, the stability that this solid-liquid in graphene slurry is acted on is gradually
Reduction, causes graphene in slurry to occur sedimentation and reunite, this causes the function of slurry to have a greatly reduced quality.Therefore, starched in graphene
The many aspects such as the formula research and development of material, process exploitation, the manufacturing, storage transport, to the bin stability of graphene slurry this
One property is all particularly paid close attention to.
However, graphene slurry is as a kind of brand-new material, lack in existing method of testing and standard to its stability
The decision method of quantization.Such as GB/T 6753.3-1986《Coating storage stability test method》In define and try out in liquid
The method of testing of the bin stability of paint and varnish, uses for reference this method, can use observation skinning, check stale flavor, agitation
Substantially judge the sedimentation degree of slurry etc. the method for non-quantized, and using the difference of viscosity after initial viscosity and storage.But it is preceding
Person is not a kind of method of quantization, and the method for the latter can not monitor the process of sedimentation in real time.Furthermore, graphene slurry generally has
Appearance of black, therefore GB/T 33327-2016 can not be used for reference《The evaluation of ultraviolet-curing paint bin stability》It is mentioned
Observation spheroid movement judge gel method.At present in current standard and Patents, lack and graphene slurry is store
The method of testing of stability is deposited, therefore it is an extremely urgent work to develop a kind of quantization, sustainable monitoring process method
Make.
The content of the invention
It is an object of the invention to set up graphene Stability of Slurry characterization model there is provided one kind for above technological deficiency
Method, this method can essence solution grasp graphene stability；
It is yet another object of the invention to provide the graphene Stability of Slurry characterization model obtained according to the above method judgement
The method of graphene Stability of Slurry.
The purpose of the present invention is implemented by the following technical programs：
A kind of method for setting up graphene Stability of Slurry characterization model, including：
S1:Slurry sample is placed in cylindrical container, and divides the sample line of upper, middle and lower three to the sample in cylinder；
S2:The absorbance test of original state slurry
Respectively from the sample line position sample of upper, middle and lower three, and it is diluted to identical multiple；Test slurry after dilution
Absorbance, loading absorbance is designated as A1, middle sample absorbance and is designated as A2, lower sample absorbance being designated as A3；
S3：The absorbance test of slurry is stored with the time
Above-mentioned slurry was deposited after certain time, the absorbance of upper, middle and lower sampling is carried out according to S2 method；With
Time it is elongated, can repeatedly test the absorbance of storage slurry upper, middle and lower sampling；
S4：Sedimentation and stability analysis
Take ratio A3/A1, A2/A1 or A3/A2 as settlement parameter, obtain settlement parameter A3/A1, A2/A1 and A3/A2 couple
Relation curve between seasonable, is graphene Stability of Slurry characterization model of the present invention.
Preferably, the method for the absorbance of test slurry after dilution is：
First absorption light of the upper, middle and lower sample in 400-1000nm wave-length coverages is tested with UV-vis absorption spectrum instrument
Spectrum, calculates the average value of the scope internal absorbance, A1, A2, A3 is calculated as respectively.
According to an aspect of the present invention, in the S2, the solvent that dilution is used and the graphene slurry to be surveyed
Solvent it is identical, sampling dilution multiple should meet the optimal test scope of uv-visible absorption spectra.
Preferably, in the S2, sampling dilutes 100 times.
According to an aspect of the present invention, in the S2, sampled with long needle tubing, the preferred 2mm of needle tubing diameter.
According to an aspect of the present invention, in the S1, the cylindrical container uses measuring cylinder with cover, and graduated cylinder value footpath is preferably
5-15cm；The height of slurry in a reservoir is 10-20cm.
According to an aspect of the present invention, in the S1, upper, middle and lower three sample lines according to slurry in a reservoir
Highly divide, it is preferable that reach the standard grade and take the position of the upper surface of slurry close in container, slurry height half in center line extracting container
Position, the offline position taken close to container bottom.
According to an aspect of the present invention, in the S3, ratio A3/A1 is taken as settlement parameter.
The graphene Stability of Slurry characterization model obtained according to the above method judges the method for graphene Stability of Slurry,
Including,
Judgement of the settlement parameter to stability in model：
A3/A1 represents the overall sedimentation of slurry, and lower floor is deposited to by upper strata, and when A3/A1 is more than 1, explanation has occurred and that
Sedimentation, A3/A1 is bigger, shows that sedimentation is more notable；
A2/A1 represents the sedimentation on slurry upper strata, and middle level is deposited to by upper strata, and when A2/A1 is more than 1, explanation has occurred and that
Sedimentation, A2/A1 is bigger, shows that sedimentation is more notable；
A3/A2 represents the sedimentation of slurry lower floor, and lower floor is deposited to by middle level, and when A3/A2 is more than 1, explanation has occurred and that
Sedimentation, A3/A2 is bigger, shows that sedimentation is more notable.
Preferably, with A3/A1<1.5 standards good as Stability of Slurry is judged.
Further, the capture of slurry stationary phase：
In model, the relation curve of settlement parameter A3/A1, A2/A1 time corresponding with A3/A2 are subsidence curve, slurry
The corresponding time interval of initial gentle section, represents slurry stationary phase；Preferably, the initial gentle section and A3/A1 in model are in 1-
1.5 scopes, show that Stability of Slurry is good；The corresponding time interval that is changed significantly is the amphibolia of the slurry；It is deposited to and reaches
The gentle section produced after saturation, represents the sedimentation period of saturation of slurry.
Beneficial effect of the present invention：
Present invention firstly provides graphene slurry infall process is quantified using absorption spectrometry, so as to judge its stability
Method.This method can quantify, continuously monitor the infall process of graphene slurry, so that its stability and stationary phase are judged,
The stability of the grasp graphene slurry of comprehensive precise quantification.Its principle is occurred slowly based on graphene slurry in storage process
, there is graphene content in the phenomenon that graphene is sunk to the bottom, the slurry in correspondence original slurry material upper, middle and lower layer region and changes in sedimentation,
As shown in Figure 1.In order to detect the difference of wherein graphene content, the present invention proposes the method using test absorption spectrum, i.e.,
Using graphene can the characteristic with narrow, full spectral absorption, it is preferable that have to Visible-to-Near InfaRed area (600-1000nm) and inhale
Receive, so that the dispersion liquid of debita spissitudo shows corresponding absorption curve on the spectrogram of near infrared region；If in dispersion liquid
The concentration of graphene is bigger, and its corresponding absorption value is also bigger；It is on the contrary then smaller.This method can by monitoring on slurry, in,
Lower floor corresponding Visible-to-Near InfaRed area absorption spectrum quantifies the change procedure of slurry, so as to judge the stability of slurry, change
Interval and terminal.Method proposed by the present invention, can match the variation monitoring of slurry under various storage requirements and environment, meet slurry
Multiple demands such as research and development, product evaluation, storage requirement screening.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, the reality with the present invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is storage of samples and sampling schematic diagram；
Fig. 2 be upper (1w-T) after slurry 1# is stored one week, in (1w-M), under (1w-B) slurry after 100 times of dilution
Absorption spectrum；
Fig. 3 be upper (1w-T) after slurry 1# is stored one week, in (1w-M), under (1w-B) slurry after 100 times of dilution
Absorption spectrum；
Fig. 4 be upper (4w-T) after slurry 1# storage four weekss, in (4w-M), under (4w-B) slurry after 100 times of dilution
Absorption spectrum；
Fig. 5 is the relation curve of slurry 1# ratios A3/A1, A2/A1 and A3/A2 respectively with period of storage, i.e. slurry 1# is steady
Qualitative characterization's model；
Fig. 6 is the abosrption spectrogram of graphene slurry 2# upper stratas sampling；
Fig. 7 is the abosrption spectrogram of graphene slurry 2# middle levels sampling；
Fig. 8 is the abosrption spectrogram of graphene slurry 2# lower floors (right figure) sampling；
Fig. 9 is slurry 2# ratios A3/A1 and the relation curve of period of storage, i.e. slurry 2# stability characterization model；
Figure 10 is the abosrption spectrogram of graphene slurry 3# upper stratas sampling；
Figure 11 is the abosrption spectrogram of graphene slurry 3# middle levels sampling；
Figure 12 is the abosrption spectrogram of graphene slurry 3# lower floors sampling.
Embodiment
In order to further illustrate the essence of the present invention, the technology of the present invention route is deployed respectively to illustrate.
The present invention sets up the technology path of the method for graphene Stability of Slurry characterization model, including following method.
1. preparation of samples
Slurry to be measured is taken, is usually the slurry just prepared.Slurry is placed in container, it is preferable that container is band cover glass
Graduated cylinder, a diameter of 5-15cm.Slurry is poured into graduated cylinder, it is preferable that the height of slurry in a reservoir is 10-20cm.According to sample
Height, by slurry be set to (T), in (M), under (B) three parts, as schematically shown in Figure 1, fix the height of three parts.It is complete
Into line.
2. sample test
The test of 2.1 initial samples
The sample just stored is initial sample, in the fixed position (at dotted line as shown in Figure 1) in upper, middle and lower three, is used
Long needle tubing (preferably, diameter 2mm) draws the graphene slurry of the position of upper, middle and lower three from top to bottom respectively, and sampling regards sample
Depending on product total amount and absorption spectrum sample tankage.Note：Because needle tubing diameter is small, sampling is few, so it is starched overall graphene
The disturbance of material can be ignored.
Taken upper, middle and lower-ranking graphene slurry is transferred in volumetric flask respectively, correspondence adds appropriate solvent by sample
Product are diluted, and are well mixed.Preferably, dilution solvent is consistent with the solvent in slurry.The multiple of dilution should meet it is ultraviolet-
The optimal test scope of visible absorption spectra；The graphene slurry for taking above-mentioned upper, middle and lower sample to be diluted to certain multiple disperses
Liquid, the absorption spectrum of its 400-1000nm wave-length coverage is tested with ultraviolet-visual spectrometer, it is preferable that wave-length coverage is 600-
1000nm。
Slurry 1# stability is for example investigated, slurry is placed in after container and is sampled, as shown in Fig. 2 when being initial state
Upper (0w-T), in (0w-M), under (0w-B) absorption spectrum of the slurry after 100 times of dilution.
Slurry 1# stability is for example investigated, slurry is placed in after container and is sampled, as shown in Fig. 2 when being initial state
Upper (0w-T), in (0w-M), under (0w-B) absorption spectrum of the slurry after 100 times of dilution.
2.2 tests stored with the time
The slurry sample is stored under specified conditions, environment, the condition depending on test purpose, for example room temperature storage,
Exposure storage, high temperature storage etc..
Deposit after certain time, the sampling of upper, middle and lower part and the test of absorption spectrum are carried out according to 2.1 method.Its
In preferably, be diluted according to the equal dilution ratio in 2.1, if the concentration is unsatisfactory for spectrum test scope, can also make phase
It should adjust, but the dilution ratio of upper, middle and lower sample should be consistent.
Period of storage is chosen according to slurry settling character, is tracked with period of storage, the upper, middle and lower layer sample of slurry
Absorption spectrum and corresponding A1, A2 and A3 value.
For example, slurry 1# by one week store, be sampled after storage, as shown in figure 3, be upper (1w-T), in (1w-
M the slurry of (1w-B) is diluting the absorption spectrum after 100 times under),.Slurry 1# is stored by surrounding, is sampled after storage,
As shown in figure 4, for upper (4w-T), in (4w-M), under (4w-B) slurry dilution 100 times after absorption spectrum.
In spectrum, 900-950nm wave-length coverages are chosen, the average value of the scope internal absorbance, record storage one is calculated
A1, A2, A3 of sample after Zhou Hou, storage four weeks.
As shown in Table 3, 4, it is after slurry 1# is stored one week, stores A1, A2, A3 value after four weeks, the ratio between each value
Value.As can be seen that obvious sedimentation, the settlement parameter A3/A1 by upper strata to lower floor occur after storing one week for slurry 1#
For 1.10, i.e. the difference of levels slurry is smaller.After slurry storage four weeks, it is by the settlement parameter A3/A1 on upper strata to lower floor
2.87, the i.e. significant difference of levels slurry, wherein being 2.28 by the settlement parameter A2/A1 on upper strata to middle level, by middle level under
The settlement parameter A3/A2 of layer is 1.26, i.e. sedimentation occurs mainly in upper strata to the interval in middle level.
3. sedimentation and stability analysis
3.1 slurries are with the change of period of storage, and the slurry of upper, middle and lower layer is because of the change of sedimentation generation content, so as to lead
Cause the change of dilution spectrum.Ratio relation between A1, A2 and A3, can reflect the intensity of variation of upper, middle and lower layer, take ratio
A3/A1, A2/A1 and A3/A2 are used as settlement parameter, it is preferable that be used as main settlement parameter using A3/A1.
The meaning of settlement parameter and the judgement to stability：
A3/A1 represents the overall sedimentation of slurry, and lower floor is deposited to by upper strata, and when A3/A1 is more than 1, explanation has occurred and that
Sedimentation, A3/A1 is bigger, shows that sedimentation is more notable.
A2/A1 represents the sedimentation on slurry upper strata, and middle level is deposited to by upper strata, and when A2/A1 is more than 1, explanation has occurred and that
Sedimentation, A2/A1 is bigger, shows that sedimentation is more notable.
A3/A2 represents the sedimentation of slurry lower floor, and lower floor is deposited to by middle level, and when A3/A2 is more than 1, explanation has occurred and that
Sedimentation, A3/A2 is bigger, shows that sedimentation is more notable.
3.2 integrated survey A3/A1, A2/A1 and A3/A2, can help decide the infall process of slurry, analysis slurry sedimentation
In by upper strata to middle level, to the process of lower floor.
The relation curve of settlement parameter A3/A1, A2/A1 time corresponding with A3/A2 of acquisition, represents sedimentation degree, sedimentation ginseng
Number keeps constant corresponding time interval, it is preferable that A3/A1<1.5, represent slurry stationary phase；Be changed significantly corresponding time zone
See the amphibolia for the slurry；Corresponding slurry when settlement parameter tends towards stability.
For example, tracking slurry 1# changes with time, sampled and tested using 2.1 methods describeds, as a result as shown in table 3：
Period of storage is mapped respectively with ratio A3/A1, A2/A1 and A3/A2, as shown in figure 5, the slurry is protected in the last fortnight
It is fixed to keep steady, and then A3/A1 values gradually rise, and at second week to changing obvious between the period 4, that is, occurs significantly sedimentation, then delays
Slow falling drop, sedimentation equilibrium was reached at the 12nd week.Arrive within wherein second week the main (A2/ based on the sedimentation on upper strata to middle level of 4th week
A1 represents that settlement parameter reaches peak value in 4th week), the sedimentation after 4th week occurs mainly in middle level, and to lower floor, (A3/A2 is represented
Settlement parameter slowly raise).
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1：
Certain graphene slurry 2#, wherein graphene content are 2.5%, and solvent is water.Determine the storage under its room temperature condition
Deposit stability.Slurry is placed in glass cylinder with cover (graduated cylinder a diameter of 10cm, height of specimen 10cm).With apart from sample surfaces
At 1cm, 4cm, 8cm be respectively (T), in (M), under (B) three parts).It is sampled using long staight needle head (diameter 2mm).
Respectively to initial state sample, stand 1 day, 2 days, 3 days, 1 week, 2 weeks, 3 weeks, 8 weeks, 10 weeks, 12 weeks samples it is upper,
In, the part of lower floor is sampled.Make to be diluted with water graphene slurry to being well mixed after 100 times, determine its UV absorption light
Compose (spectral region is 400-1000nm).Test result is as shown in Fig. 6,7,8.Based on the absorption spectrum of Fig. 6,7,8,900- is chosen
Absorbance makees average value in 950nm wave-length coverages, respectively obtains A1, A2, A3 value of each period of storage point and corresponding sedimentation
Parameter A3/A1, A2/A1 and A3/A2.As a result it is as shown in table 4.
Based on the absorption spectrum of Fig. 6,7,8, choose absorbance in 900-950nm wave-length coverages and make average value, respectively obtain
A1, A2, A3 value of each period of storage point and corresponding settlement parameter A3/A1, A2/A1 and A3/A2.As a result it is as shown in table 4：
Relation curve is obtained to period of storage mapping with A3/A1, as i.e. slurry 2# stability characterization model.Such as Fig. 9 institutes
Show, it is seen that this graphene slurry changes over time, and stability also changes.Its absorption spectrum curve shows, with quiet
Put time lengthening upper strata and middle layer graphene concentration is gradually reduced, lower layer graphene concentration then shows as first reducing to be increased most afterwards
Constant trend afterwards.A3/A1 value changes are also first to reduce to increase last close to equilibrium valve afterwards, consistent with graphene slurry 2#,
Graphene in this explanation slurry can occur enrichment in standing early stage (in one week) and cause upper strata concentration to be more than bottom concentration first,
And as time of repose continues to increase, graphene can gradually be deposited in bottom, do not occurred close to after an equilibrium valve finally
Change.
Embodiment 2：
Certain graphene slurry 3#, wherein graphene content are 3.5%, and solvent is 1-METHYLPYRROLIDONE.Determine its room
Bin stability under the conditions of temperature.Slurry is placed in glass cylinder with cover (graduated cylinder a diameter of 8cm, height of specimen 20cm).With
At sample surfaces 1cm, 9cm, 17cm be respectively (T), in (M), under (B) three parts).Use long staight needle head (diameter
2mm) it is sampled 0.5g.
Respectively to initial state sample, stand 1 day, 2 days, 3 days, 1 week, 2 weeks, 3 weeks, 7 weeks, 8 weeks, the sample of 9 weeks it is upper,
In, the part of lower floor is sampled.Graphene slurry is diluted to well mixed, measure after 200 times using 1-METHYLPYRROLIDONE
Its ultra-violet absorption spectrum (spectral region is 400-1000nm).Test result is as shown in Figure 10,11,12.Can from Figure 10
Go out, with the change of time of repose, its uv-vis spectra graph discovery changes accordingly, illustrates that this method can distinguish upper strata
The relation that liquid is changed over time.With the extension of time of repose, fluctuating for absorption curve illustrates the upper of graphene concentration
It is lower to float.In the wave-length coverage of near infrared region its absorption spectrum curve gradually move down until change hardly substantially (the 7th week, 8
Curve moves up and down unobvious when week, 9 weeks), illustrate that the concentration of graphene in supernatant liquid gradually subtracts and then progressively reach one
Balance terminal.Figure 11 illustrates the graphene concentration in intermediate layer as respective change also occurs for time of repose change, and it absorbs light
Spectral curve is first moved up and then moved down, and first increases and then decreases trend is presented, the concentration for illustrating the graphene slurry intermediate layer is first to increase
It is gradually reduced after big.As time of repose gradually increases in Figure 12, the absorption spectrum curve of graphene slurry bottom is also sent out therewith
Changing.It can similarly obtain, the concentration of graphene is first to reduce to increase afterwards in the slurry of bottom, while reaching after a balance terminal not
Persistently increase again.
Based on Fig. 6-Fig. 8 absorption spectrum, choose absorbance in 900-950nm wave-length coverages and make average value, respectively obtain
A1, A2, A3 value of each period of storage point and corresponding settlement parameter A3/A1, A2/A1 and A3/A2.As a result it is as shown in table 5：
Period of storage is mapped with A3/A1 and obtains the stability characterization model of relation curve, as graphene slurry 3.With
The extension of time of repose, A3/A1 value changes first reduce to be increased afterwards, finally reach the unconspicuous value of change, this explanation slurry
In graphene cause upper strata concentration more than bottom concentration standing early stage (one week in) enrichment can occur first, and with standing
Time continues to increase, and graphene can be deposited gradually in bottom, is almost no longer changed after depositing to a certain extent.Explanation
Graphene slurry time of repose in certain period of time is longer, and its stability is poorer, reaches and is no longer changed after end point values.
Embodiment 3：
Certain graphene slurry 4#, wherein graphene content are 1.0%, and solvent is ethylene glycol.Determine under its room temperature condition
Bin stability.Slurry is placed in glass cylinder with cover (graduated cylinder a diameter of 8cm, height of specimen 10cm).With apart from sample
At surface 1cm, 4cm, 8cm be respectively (T), in (M), under (B) three parts).Taken using long staight needle head (diameter 2mm)
Sample.
Respectively to initial state sample, stand 1 day, 2 days, 3 days, 1 week, 2 weeks, 3 weeks, the upper, middle and lower layer of 8 weeks samples
Part be sampled.Graphene slurry is diluted using ethylene glycol to be well mixed to after 100 times, determines its ultra-violet absorption spectrum
(spectral region is 400-1000nm).Choose absorbance in 800-900nm wave-length coverages and make average value, respectively obtain each storage
A1, A2, A3 value at time point and corresponding settlement parameter A3/A1, A2/A1 and A3/A2.As a result it is as shown in table 6：
It can be seen that, graphene slurry 4# is more stable, occurs slight sedimentation within 3 days before placement, afterwards in 2 months
Keep stable.
Embodiment 4：
Certain graphene slurry 5#, wherein graphene content are 5.0%, and solvent is NMP.Determine under its 80 DEG C of constant temperatures
Bin stability.Slurry is placed in glass cylinder with cover (graduated cylinder a diameter of 8cm, height of specimen 10cm).With apart from sample
At surface 1cm, 4cm, 8cm be respectively (T), in (M), under (B) three parts).Taken using long staight needle head (diameter 2mm)
Sample.
Sample is placed in the baking oven of 80 DEG C of constant temperature, respectively to initial state sample, stand 0.5 hour, 1 hour, 2 hours, it is 3 small
When, 4 hours, 5 hours, after 6 hours sample upper, middle and lower layer part be sampled.Using NMP dilution graphenes slurry extremely
Be well mixed after 200 times, determine its ultra-violet absorption spectrum (spectral region is 400-1000nm).Choose 800-1000nm wavelength models
Enclose middle absorbance and make average value, respectively obtain each period of storage point A1, A2, A3 value and corresponding settlement parameter A3/A1,
A2/A1 and A3/A2.As a result it is as shown in table 7：
It can be seen that, slurry 5# kept relative stability within 3 hours at high temperature, and significantly sedimentation occurs afterwards.
Embodiment 5：
Certain graphene slurry 5#, wherein graphene content are 5.0%, and solvent is NMP.It is determined in outdoor daylight exposure
Under the conditions of bin stability.Slurry is placed in glass cylinder with cover (graduated cylinder a diameter of 8cm, height of specimen 10cm).With away from
From at sample surfaces 1cm, 4cm, 8cm be respectively (T), in (M), under (B) three parts).Entered using long staight needle head (diameter 2mm)
Row sampling.
Sample is placed under outdoor daylight, respectively to initial state sample, exposure 0.5 hour, 1 hour, 2 hours, 3 hours, it is 4 small
When, 5 hours, 6 hours, 12 hours, 24 hours (be between wherein 6 hours and 12 hours overnight then be exposed to the sun again 6 hours), it is right respectively
The part of the upper, middle and lower layer of sample is sampled.Graphene slurry is diluted using NMP to be well mixed to after 200 times, determines it
Ultra-violet absorption spectrum (spectral region is 400-1000nm).Choose absorbance in 800-1000nm wave-length coverages and make average value, point
A1, A2, A3 value and corresponding settlement parameter A3/A1, A2/A1 and A3/A2 of each period of storage point are not obtained.As a result such as table 8
It is shown：
It can be seen that, slurry 5# by keeing relative stability during sunlight exposure, is being amenable to be exposed to the sun for 4 hours, sudden and violent
Start to settle after shining 6 hours.
Embodiment 6：
Certain graphene slurry 6#, wherein graphene content are 2.0%, and solvent is NMP.It is determined under 5 DEG C of environment
Bin stability.Slurry is placed in closed (beaker a diameter of 10cm, height of specimen 5cm) in beaker.With apart from sample surfaces
At 1cm, 2.5cm, 4cm be respectively (T), in (M), under (B) three parts).It is sampled using long staight needle head (diameter 2mm).
Sample is placed in 5 DEG C of cold storage refrigerators, respectively to initial state sample, refrigeration 1 week, January, 2 months, March, June sample
Upper, middle and lower layer part be sampled.Graphene slurry is diluted using NMP to be well mixed to after 200 times, determines its ultraviolet
Absorption spectrum (spectral region is 400-1000nm).Choose absorbance in 600-1000nm wave-length coverages and make average value, respectively
To A1, A2, A3 value and corresponding settlement parameter A3/A1, A2/A1 and A3/A2 of each period of storage point.As a result it is as shown in table 9：
It can be seen that, slurry 6# under cryogenic, can preferably keep stability, up to not showing in the time of 6 months
Write sedimentation.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality
Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (10)
1. a kind of method for setting up graphene Stability of Slurry characterization model, it is characterised in that：Including：
S1:Slurry sample is placed in cylindrical container, and divides the sample line of upper, middle and lower three to the sample in cylinder；
S2:The absorbance test of original state slurry
Respectively from the sample line position sample of upper, middle and lower three, and it is diluted to identical multiple；Test the extinction of slurry after dilution
Angle value, loading absorbance is designated as A1, middle sample absorbance and is designated as A2, lower sample absorbance being designated as A3；
S3：The absorbance test of slurry is stored with the time
Above-mentioned slurry was deposited after certain time, the absorbance of upper, middle and lower sampling is carried out according to S2 method；Over time
It is elongated, can repeatedly test the absorbance of storage slurry upper, middle and lower sampling；
S4：Sedimentation and stability analysis
Ratio A3/A1, A2/A1 or A3/A2 are taken as settlement parameter, when obtaining settlement parameter A3/A1, A2/A1 and A3/A2 to correspondence
Between relation curve, be graphene Stability of Slurry characterization model of the present invention.
2. the method according to claim 1 for setting up graphene Stability of Slurry characterization model, it is characterised in that：The S2
In, the absorbance is the absorbance of specific wavelength in the range of 400-1000nm.
3. the method according to claim 2 for setting up graphene Stability of Slurry characterization model, it is characterised in that：Test is dilute
The method for releasing the absorbance of disposed slurry is：
First with UV-vis absorption spectrum instrument test upper, middle and lower sample in the absorption spectrum of 400-1000nm wave-length coverages, meter
The average value of the scope internal absorbance is calculated, A1, A2, A3 are calculated as respectively.
4. the method according to claim 1 for setting up graphene Stability of Slurry characterization model, it is characterised in that：The S2
In, dilution use solvent it is identical with the solvent of the graphene slurry to be surveyed, sample dilute multiple should meet it is ultraviolet-
The optimal test scope of visible absorption spectra；Preferably, in the S2, sampling dilutes 100 times.
5. the method according to claim 1 for setting up graphene Stability of Slurry characterization model, it is characterised in that：The S2
In, sampled with long needle tubing, the preferred 2mm of needle tubing diameter.
6. the method according to claim 1 for setting up graphene Stability of Slurry characterization model, it is characterised in that：The S1
In, the cylindrical container uses measuring cylinder with cover, and graduated cylinder value footpath is preferably 5-15cm；The height of slurry in a reservoir is 10-20cm.
7. the method according to claim 1 for setting up graphene Stability of Slurry characterization model, it is characterised in that：The S1
In, the height division according to slurry in a reservoir of the sample line of upper, middle and lower three, it is preferable that reach the standard grade and take the slurry close in container
Upper surface position, the position of slurry height half, the offline position taken close to container bottom in center line extracting container.
8. the method according to claim 1 for setting up graphene Stability of Slurry characterization model, it is characterised in that：The S3
In, ratio A3/A1 is taken as settlement parameter.
9. the graphene Stability of Slurry characterization model obtained according to any one of claim 1-8 methods described judges that graphene is starched
Expect the method for stability, including,
Judgement of the settlement parameter to stability in model：
A3/A1 represents the overall sedimentation of slurry, and lower floor is deposited to by upper strata, when A3/A1 is more than 1, illustrates to have occurred and that sedimentation,
A3/A1 is bigger, shows that sedimentation is more notable；
A2/A1 represents the sedimentation on slurry upper strata, and middle level is deposited to by upper strata, when A2/A1 is more than 1, illustrates to have occurred and that sedimentation,
A2/A1 is bigger, shows that sedimentation is more notable；
A3/A2 represents the sedimentation of slurry lower floor, and lower floor is deposited to by middle level, when A3/A2 is more than 1, illustrates to have occurred and that sedimentation,
A3/A2 is bigger, shows that sedimentation is more notable；
Preferably, with A3/A1<1.5 standards good as Stability of Slurry is judged.
10. the graphene Stability of Slurry characterization model that method is obtained according to claim 9 judges that graphene slurry is stable
The method of property, it is characterised in that：
The capture of slurry stationary phase：
In model, the relation curve of settlement parameter A3/A1, A2/A1 time corresponding with A3/A2 is subsidence curve, slurry it is initial
The corresponding time interval of gentle section, represents slurry stationary phase；Preferably, the initial gentle section and A3/A1 in model are in 1-1.5 models
Enclose, show that Stability of Slurry is good；The corresponding time interval that is changed significantly is the amphibolia of the slurry；It is deposited to up to after saturation
The gentle section produced, represents the sedimentation period of saturation of slurry.
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| CN117092069A (en) * | 2023-10-20 | 2023-11-21 | 瑞浦兰钧能源股份有限公司 | Method for detecting floating of binder in lithium ion battery slurry |
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