CN110261278A - A method of measurement grapheme material powder specific-surface area detection - Google Patents
A method of measurement grapheme material powder specific-surface area detection Download PDFInfo
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Abstract
This application involves grapheme material fields, in particular to a kind of method for measuring grapheme material powder specific-surface area detection.It include: the quality detected using BET specific surface area detection method to grapheme material in test sample；The specific surface area of grapheme material is calculated according to the quality of grapheme material and the first adsorbance.Supporter can support grapheme material, and grapheme material is largely avoided in detection process and disperses, glue the occurrence of wall.The adsorbance of supporter is smaller, much smaller than the adsorbance of graphene.The adsorbance of the value of first adsorbance relatively graphene can draft the adsorbance that the first adsorbance is equal to graphene, the specific surface area of grapheme material can be calculated according to the quality of black alkene material and the first adsorbance.
Description
Technical field
This application involves grapheme material fields, in particular to a kind of measurement grapheme material powder specific-surface area detection
Method.
Background technique
It is conventional at present that more accurately the method for test specific surface area is mainly absorption method.Nitrogen adsorption BET technology is to be used for
The common method of powder body material specific surface area is measured, this test method is the method and mesh of international standard test specific surface area
Preceding test nano material and the maximally efficient test method of porous material, however the grapheme material powder of thin layer is tied by its two dimension
Structure influences, and large specific surface area, apparent density is low, and the adsorbance susceptible of nitrogen in test process eventually leads to surveyed ratio
Surface area is far smaller than true specific surface area value.
Summary of the invention
The embodiment of the present application is designed to provide a kind of method for measuring grapheme material powder specific-surface area detection, is intended to
A kind of method for proposing new measurement grapheme material specific surface area.
The application first aspect provides a kind of method for measuring grapheme material specific surface area, mainly comprises the steps that
Detecting to the adsorbance of test sample is the first adsorbance；It include supporter and the graphene for being carried on supporter to test sample
Material；
Quality to grapheme material in test sample is detected using BET specific surface area detection method；According to the matter of grapheme material
Amount and the first adsorbance calculate the specific surface area of grapheme material.
By graphene-supported (or absorption) on supporter as the adsorbance to test sample detection to test sample；Support physical efficiency
Grapheme material is enough supported, grapheme material is largely avoided in detection process and disperses, glue the occurrence of wall.Due to stone
Black alkene reference area is much larger than the specific surface area of supporter；Therefore the ratio of the first adsorbance is accounted for the adsorbance of supporter in test sample
The difference very little of the adsorbance of value very little, the first adsorbance and graphene can assert that the first adsorbance is the adsorbance of graphene；
Quality to grapheme material in test sample more can be measured accurately；According to the quality and the first adsorbance of black alkene material
Calculate the specific surface area of grapheme material.
In some embodiments of the application first aspect, the adsorbate of above-mentioned BET specific surface area detection method is nitrogen.
In some embodiments of the application first aspect, the method for said determination grapheme material specific surface area is also wrapped
It includes:
The adsorbance for obtaining supporter is the second adsorbance；
According to the difference of the first adsorbance and the second adsorbance, the specific surface of the Mass Calculation grapheme material of grapheme material
Product.
The second adsorbance is obtained, it being capable of the further accurately absorption of black alkene material by the first adsorbance and the first adsorbance
Amount according to the quality of black alkene material and makes the adsorbance of the accurate black alkene material of a step；Keep measurement result more acurrate.
Further, in some embodiments of the application first aspect, the adsorbance of above-mentioned acquisition supporter is second
The step of adsorbance includes:
The second adsorbance is calculated by the quality of supporter and the specific surface area of supporter.
In some embodiments of the application first aspect, supporter is made of the material with gap or supporter
It is made of thin-film material；
Optionally, supporter is made of porous materials；
Optionally, supporter is made of the metal material with gap；
Optionally, the material of supporter includes nickel foam, foam copper, foamed aluminium, foamed iron, foam iron-nickel alloy or bubble
One of foam pltine is a variety of；
Optionally, the material of supporter includes the polymer with hole configurations；
Optionally, the material of supporter includes one of copper foil, aluminium foil or goldleaf or a variety of.
The supporter being made of porous materials as much as possible can adsorb grapheme material more, reduce error, increase final
As a result accuracy.Grapheme material can also be made in thin-film material, avoid the splashing of grapheme material powder.
It is above-mentioned to be made to test sample by following steps in some embodiments of the application first aspect:
By grapheme material solution loadings in supporter, the grapheme material of non-supported body absorption is removed after dry；
Optionally, the supporter by grapheme material solution loadings after cleaning.
In some embodiments of the application first aspect, above-mentioned grapheme material solution is made by following steps:
Admixed graphite alkene material powder and ethanol water are centrifugally separating to obtain grapheme material solution after ultrasonic disperse,
The concentration of grapheme material is 20~30mg/ml in grapheme material solution.
Graphene is well-dispersed in ethanol water, centrifuge separation grapheme material into grapheme material solution
Concentration is 20~30mg/ml；Certain mobility is made it have, is carried on supporter convenient for grapheme material.
In some embodiments of the application first aspect, it is above-mentioned by grapheme material solution loadings in the supporter the step of
Before, further includes: cutting out matrix is the matched size of testing tube with BET specific surface area detection method.
It cuts out as the matched size of testing tube, is conducive to test specimens and is successfully placed in tube bottom, avoid the viscous of graphene powder
Wall.
In some embodiments of the application first aspect, it is above-mentioned by grapheme material solution loadings in the supporter the step of
Before, further includes:
Supporter is impregnated using organic solvent, supporter is placed in water ultrasonic cleaning after ultrasonic cleaning, is then dried.
It is cleaned by ultrasonic supporter, so that it is adsorbed graphene as much as possible, the value of supporter adsorbance can also be made more quasi-
Really.
In some embodiments of the application first aspect, it is above-mentioned by grapheme material solution loadings in the supporter the step of
Include:
Supporter after cleaning is soaked in grapheme material solution, is then freeze-dried.
Detailed description of the invention
Technical solution in ord to more clearly illustrate embodiments of the present application, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only some embodiments of the application, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 shows a kind of embodiment party of the method for measurement grapheme material specific surface area provided by the embodiments of the present application
Formula；
Fig. 2 shows another embodiment party of the method for measurement grapheme material specific surface area provided by the embodiments of the present application
Formula；
Fig. 3 show the embodiment of the present application 1 preparation to test sample scanning electron microscope (SEM) photograph；
Fig. 4 shows the scanning electron microscope (SEM) photograph to test sample of the preparation of the embodiment of the present application 4；
Fig. 5 shows the scanning electron microscope (SEM) photograph of graphene after the drying of 2 directly freezed of comparative example.
Specific embodiment
It, below will be in the embodiment of the present application to keep the purposes, technical schemes and advantages of the embodiment of the present application clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
A kind of method of measurement grapheme material specific surface area of the embodiment of the present application is specifically described below.
It should be noted that grapheme material shall be understood in a broad sense in embodiments herein, including but not limited to stone
Black alkene, graphene oxide, sulfonated graphene etc. be modified after grapheme material or the graphene that is not modified.
Grapheme material powder is influenced vulnerable to its two-dimensional structure, large specific surface area, and apparent density is low.Its adsorbance is detected again
During: when being added in the thin mouth container of specific surface area test, it is easy to happen and disperses, glues the case where wall；With external force by its
When being pushed into test bottle bottom, grapheme material is very easy under external force between layers since interlayer lacks functional group
Stacking occurs to eventually lead to surveyed specific surface area to seriously affect adsorbance and be far smaller than true specific surface area value.
A method of measurement grapheme material specific surface area mainly comprises the steps that
Use BET specific surface area detection method detection detection to the adsorbance of test sample for the first adsorbance；It include branch to test sample
Support body and the grapheme material for being carried on supporter.
Obtain the quality to grapheme material in test sample；Graphite is calculated according to the quality of grapheme material and the first adsorbance
The specific surface area of alkene material.
By graphene-supported (or absorption) on supporter as the adsorbance to test sample detection to test sample；Support physical efficiency
Grapheme material is enough supported, grapheme material is largely avoided in detection process and disperses, glue the occurrence of wall, makes to test
Process is easier.
Graphene reference area may be far longer than the specific surface area of supporter；Therefore the adsorbance to supporter in test sample
Account for the ratio very little of the first adsorbance, the difference of the adsorbance of the first adsorbance and graphene is smaller, can assert the first adsorbance
For the adsorbance of graphene；Quality to grapheme material in test sample more can be measured accurately；According to the matter of black alkene material
Amount and the first adsorbance can calculate the specific surface area of grapheme material.
Further, this method can relatively rapid know the specific surface area of grapheme material.For example, the suction of supporter
Attached amount can be less than the 70% of graphene adsorbance.
Further, in some embodiments of the present application, the adsorbance for further including acquisition supporter is the second adsorbance.
According to the difference of the first adsorbance and the second adsorbance, the specific surface of the Mass Calculation grapheme material of grapheme material
Product.
From the above, after the adsorbance for obtaining supporter, subtracting the second adsorbance by the first adsorbance just can be accurate
Ground obtains the adsorbance of grapheme material, is further accurately obtained the specific surface area of grapheme material.
In the present embodiment, since the adsorbance of grapheme material is the value that the first adsorbance subtracts the second adsorbance, because
This, does not limit the adsorbance of supporter in the present embodiment.
In to test sample, the main function of supporter is, supports or load graphene, avoids the splashing of graphene.
The material of supporter is unrestricted.Further, it can extend into BET testing tube to test sample, supporter has and testing tube
The size matched；It can be by way of cutting, naturally it is also possible to the supporter of smaller size is obtained by modes such as purchases.
It should be noted that the size of supporter can be close with the internal diameter of testing tube, it is enable to wait for that test sample protrudes into just
Testing tube.Certainly, the size of supporter can also be much smaller than the internal diameter of testing tube.
Further, in some embodiments of the present application, supporter is made of the material with gap or supporter
It is made of thin-film material.
Material with gap refers to that from microstructure, inside has the material in perforation or closed gap.Further
Ground, supporter are made of porous materials；Porous material is a kind of by being mutually communicated or closed hole constitutes the material of network structure
Material, the boundary or surface of hole are made of pillar or plate；It can be the two-dimentional holes, or three-dimensional apertures.Material with gap
Supporter made of material or porous material as much as possible can adsorb grapheme material more, increase the graphite for being carried on supporter
The quality of alkene, further decreases error, increases the accuracy of final result.
Thin-film material refers to membrane material of the thickness less than 10 μm, and inside can not have gap.
As illustratively, in some embodiments of the present application, supporter is made of the metal material with gap.Example
Such as, the material of supporter includes in nickel foam, foam copper, foamed aluminium, foamed iron, foam iron-nickel alloy or foam pltine
It is one or more；Or aluminium flake with hole, iron plate, lithium piece etc..
As illustratively, in some embodiments of the present application, the material of supporter includes having gathering for hole configurations
Close object；Such as artificial sponge, polyurethane foam plastics, paper etc..
As illustratively, in some embodiments of the present application, the material of supporter includes copper foil, aluminium foil, in goldleaf
It is one or more.Or the material of supporter includes aluminium foil, alloy material etc..
As illustratively, the embodiment of the present application describes two kinds in numerous embodiments.In following two kinds of embodiments
In, the material of graphene powder is graphene, it is to be understood that in the other embodiments of the application, graphene powder
Material may be graphene after graphene oxide, sulfonated graphene etc. are modified.
Referring to Fig. 1, Fig. 1 shows a kind of embodiment of the embodiment of the present application.
In some embodiments of the present application, the method for measuring graphene powder specific surface area is mainly comprised the steps that
The preparation of supporter: prepare to test the matched supporter of pipe size with BET, further, the size of supporter can
To test pipe size much smaller than BET, avoids supporter from having when protruding into BET testing tube with tube wall and contact too much.
S1: cleaning supporter simultaneously obtains its quality；For example, organic solvent impregnates supporter then ultrasound, then displacement is arrived
Ultrasonic cleaning is impregnated in water；Then by supporter, it is placed in vacuum drying oven, and 80-100 DEG C thoroughly dry, super with hundred a ten thousandths
Precision balance weighs quality, and quality is accurate to 0.1mg.It is understood that can also be adopted in the other embodiments of the application
Supporter is cleaned with other cleaning ways.Organic solvent can be methanol, ethyl alcohol, acetone etc..
S2: grapheme material solution is prepared；Admixed graphite alkene material powder and ethanol water, centrifugation point after ultrasonic disperse
From grapheme material solution is obtained, the concentration of grapheme material is 20~30mg/ml in grapheme material solution.
It should be noted that the solvent of grapheme material solution can use the ethanol water of arbitrary proportion；Such as 10-
The ethanol water of 90vol%, the ethanol water of 20-80vol%, the ethanol water of 25-75vol%, 40-55vol%
Ethanol water, 50% ethanol water etc..Ethanol water can not also be used, ethyl alcohol, water, methanol can be used
Deng other solvents.
Graphene is well-dispersed in ethanol water, centrifuge separation grapheme material into grapheme material solution
Concentration is 20~30mg/ml；Certain mobility is made it have, is carried on supporter convenient for grapheme material.
In detail, in embodiments herein, sufficiently ultrasound is added in the solution of ethanol water in grapheme material powder,
After the solid dry powder not floated to liquid surface, is continuing ultrasound 30 minutes, then the low-speed centrifugal regular hour, outwelling
Clear liquid adds water to continue ultrasound and is centrifuged again, and 3-5 times repeatedly, the simple ethyl alcohol removed in solution is finally centrifuged to graphene in water
Concentration is 20-30mg/ml, until having certain mobility.
S3: making to test sample, by supporter of the grapheme material solution loadings after cleaning, removes after dry and is not supported
The grapheme material of body absorption.
In embodiments herein, can using deposition absorption graphene method by grapheme material solution loadings in
Supporter after cleaning.Such as: supporter is sufficiently infiltrated into graphene slurry, ultrasound 30 minutes, it is ensured that graphene and branch
Support the abundant combination of object；
Graphene slurry containing supporter is quickly immersed in the ultra low temperatures environment such as liquid nitrogen, realizes the solution of graphene
Rapid curing；
It is freeze-dried the graphene containing supporter；
The supporter in dried graphene is taken out, at this moment graphene has been had been filled in supporter inner wall hole, has gone
Except unadsorbed graphene.By the supporter drying containing graphene.
Or using Electro Sorb method by supporter of the grapheme material solution loadings after cleaning for example: take 1ml ammonium hydroxide to add
Enter into 30ml graphene aqueous solution, ultrasonic disperse is sufficiently stirred, makes graphene aqueous solution with electrolyte；
It takes supporter (nickel foam or foam copper) to be respectively turned on the positive and negative anodes of power supply, immerses in graphene aqueous solution, voltage
It is set as 3-5V, DC power supply is powered 10 minutes or so, removes；
Then it places it in the ultra-low temperature surroundings such as liquid nitrogen, after quick solidification, freeze-drying；After having dried, surface is removed
The graphene of absorption loosely.
In the present embodiment, the supporter after cleaning is soaked in grapheme material solution, is then freeze-dried, such as
- 30 DEG C~-60 DEG C are refrigerated to be dried.Further, by grapheme material solution repeatedly drop coating on backing material, or will
Supporter is immersed in grapheme material solution, and low temperature quickly cooling makes the fast quickly cooling of water to -30 DEG C or less (such as -30 DEG C~-60 DEG C)
It is frozen into ice cube state, graphene and supporter are freeze-dried together, until the anhydrous isloation state in surface.
Will it is dry after graphene and supporter mixture take out, the graphene powder that removal supporting body surface is easily fallen obtain to
Test sample.
It should be noted that in the other embodiments of the application, including supporter and the graphene for being carried on supporter
Can being prepared by the above method to test sample for material, can also be prepared by other means, such as pass through purchase etc..It obtains
It takes the quality to test sample: going out the quality of graphene and supporter with hundred a ten thousandth balance accurate weighings.
S4: the quality to grapheme material in test sample is obtained；The quality that quality to test sample subtracts supporter obtains graphite
The quality of alkene material.
S5: the adsorbance to test sample, i.e. the first adsorbance are obtained；In the present embodiment, the first adsorbance is nitrogen adsorption
Amount, in some other embodiments of the application, adsorbate can not also be nitrogen, such as can be argon gas, Krypton etc..Into one
Step ground, in the present embodiment, nitrogen adsorption capacity is obtained using nitrogen adsorption methods.
It should be noted that the absorption to test sample can be obtained using other methods in the other embodiments of the application
Amount, is not limited only to nitrogen adsorption methods.
According to the operating process of nitrogen adsorption BET, testing to the adsorbance of test sample is the first adsorbance.
S6: the specific surface area of grapheme material is calculated:
Specific surface area S are as follows: S=VmNAσ/22400W
In formula: NAFor avogadros constant；σ is the section (nm of each adsorption molecule2)；W is adsorbent mass (g)；
22400 be the volume (mL) of 1mol gas under standard state.VmRequired gas when covering monomolecular gases for adsorbent surface
Volume (mL) measurement, can be calculated by pressure change.
Wherein the sectional area σ of adsorption molecule can be found out by a variety of methods, be calculated using following formula:
σ=1.09 (M/NAd)2/3
In formula: M is the molecular weight of adsorbate (such as nitrogen)；D is the close of the adsorbate (such as nitrogen) under adsorption temp
Degree.For nitrogen, the value that σ often takes in 78K is 0.162nm2。
Fig. 2 shows the another embodiments of the embodiment of the present application.Please refer to Fig. 1 and Fig. 2.
In the present embodiment, step S1-S5 is identical as embodiment shown in Fig. 1, is no longer repeated herein.?
In present embodiment, further includes:
S7: obtaining to the adsorbance of supporter in test sample is the second adsorbance:
In the present embodiment, the adsorbance of supporter can pass through the quality of supporter and the specific surface area meter of supporter
It calculates, measurement can also be passed through.For example, by the specific surface area for detecting identical material support, to calculate to be supported in test sample
The adsorbance of body.
Calculate the specific surface area of grapheme material:
Calculate adsorbance=first the-the second adsorbance of adsorbance of grapheme material；
The specific surface area of grapheme material is calculated using the calculation formula in above embodiment again.
It should be noted that in some embodiments of the present application, not to the method for measurement grapheme material specific surface area
Step is successively limited.
Such as: it is calculated to the quality of grapheme material in test sample, obtains the adsorbance to test sample, obtain supporter
Adsorbance and etc. do not have sequencing.
The feature of the application and performance are described in further detail with reference to embodiments.
Embodiment 1- embodiment 6, comparative example 1- comparative example 3 measure its specific surface area to same a collection of graphene.
Embodiment 1
The present embodiment provides a kind of measuring methods of graphene specific surface area, mainly comprise the steps that
Sufficiently ultrasound is added in 50vol% ethanol water in graphene powder, supernatant is outwelled, water is added to continue ultrasound again
Centrifugation, 3 times repeatedly, concentration is 20mg/ml in water for centrifugation to graphene.
EtOH Sonicate cleans nickel foam, then is cleaned by ultrasonic nickel foam using deionized water, then dries.
The supporter (nickel foam) for weighing 30mg, is cut into small pieces with scissors.
By graphene-supported in supporter: using the repeated multiple times absorption graphene aqueous solution of suction pipe, drop coating is in foam nickel surface
With inside, nickel foam is made to adsorb graphene to greatest extent, then the nickel foam for having adsorbed graphene is freeze-dried, has been lyophilized
Cheng Hou, in placing it in vacuum drying oven, 80 DEG C vacuumize and continue dry 3 hours, it is ensured that the hydrone of graphene surface absorption
Thoroughly gasification；Obtained after the completion of dry to test sample.
Weighing to test sample quality is the second mass；Second mass subtracts support weight (30mg) and obtains third quality.
Use BET method test to the adsorbance of test sample for the first adsorbance.
Pass through the first adsorbance and third Mass Calculation graphene specific surface area；Duplicate measurements 3 times.
Embodiment 1 is prepared as shown in Figure 3 to test sample scanning electron microscope (SEM) photograph.
Embodiment 2
The present embodiment the difference from embodiment 1 is that, in the present embodiment the material of supporter be foam copper.
Embodiment 3
The present embodiment the difference from embodiment 1 is that, in the present embodiment the material of supporter be sponge.
Embodiment 4
The present embodiment the difference from embodiment 1 is that, the graphene-supported process in supporter is different, in the present embodiment
In, the graphene-supported method in supporter are as follows: graphene is diluted to 2mg/ml, the ammonium hydroxide dilution of ph=1 is then added
Nickel foam is connect positive pole by 1ml, and voltage controls within 5V, and energization 10-30 minutes or so, graphene can be adsorbed onto foam
Nickel surface and inner wall, drying is obtained to test sample after being drawn off.
The step of remaining step is provided with embodiment 1 is identical.Scanning electron microscope (SEM) photograph to test sample such as Fig. 4 prepared by embodiment 4
It is shown.
Embodiment 5
The present embodiment provides a kind of measuring methods of graphene specific surface area, mainly comprise the steps that
Sufficiently ultrasound is added in 40vol% ethanol water in graphene powder, supernatant is outwelled, water is added to continue ultrasound again
Centrifugation, 3 times repeatedly, concentration is 20mg/ml in water for centrifugation to graphene.
EtOH Sonicate cleans nickel foam, then is cleaned by ultrasonic copper foil using deionized water, then dries.
The supporter (copper foil) for weighing 30mg is cut into and the matched fritter of testing tube size with scissors.
By graphene-supported in supporter: using the repeated multiple times absorption graphene aqueous solution of suction pipe, drop coating is in foam nickel surface
With inside, nickel foam is made to adsorb graphene to greatest extent, then the nickel foam for having adsorbed graphene is freeze-dried, has been lyophilized
Cheng Hou, in placing it in vacuum drying oven, 80 DEG C vacuumize and continue dry 3 hours, it is ensured that the hydrone of graphene surface absorption
Thoroughly gasification；Obtained after the completion of dry to test sample.
Weighing to test sample quality is the second mass；Second mass subtracts support weight (30mg) and obtains third quality.
Use BET method test to the adsorbance of test sample for the first adsorbance, adsorbate is argon gas.Duplicate measurements 3 times.
Pass through the first adsorbance and third Mass Calculation graphene specific surface area.
Embodiment 6
The present embodiment provides a kind of measuring methods of graphene specific surface area, mainly comprise the steps that
The clean scraps of paper are taken, the size of the scraps of paper is matched with testing tube size.BET method is used to survey the adsorbance of the scraps of paper as second
Adsorbance, adsorbate are argon gas.It is averaged for duplicate measurements 3 times
By graphene-supported in clean supporter (paper), the size of supporter is matched with testing tube size.
With the repeated multiple times absorption graphene aqueous solution of suction pipe, drop coating makes nickel foam maximum limit in foam nickel surface and inside
Then the nickel foam for having adsorbed graphene is freeze-dried by the absorption graphene of degree, after the completion of freeze-drying, dry placing it in vacuum
In case, 80 DEG C vacuumize and continue dry 3 hours, it is ensured that the hydrone of graphene surface absorption thoroughly gasifies；After the completion of dry
Arrive to test sample.
Weighing to test sample quality is the second mass；Second mass subtracts support weight (30mg) and obtains third quality.
Use BET method test to the adsorbance of test sample for the first adsorbance, adsorbate is argon gas.Duplicate measurements 3 times.
Pass through the difference of the first adsorbance and the second adsorbance, third Mass Calculation graphene specific surface area.
Comparative example 1
Graphene directly freezed is dry, using the specific surface area of BET method test graphene.Graphite after directly freezed is dry
The scanning electron microscope (SEM) photograph of alkene is as shown in Figure 5.
Comparative example 2
Graphene atomization drying, using the specific surface area of BET method test graphene.
Comparative example 3
Graphene specific surface area is tested using the method for methylene blue adsorption number.
Embodiment 1- embodiment 4, the test result of comparative example 1- comparative example 3 are as shown in table 1.
Parameter in 1 embodiment of table and comparative example to test sample
2 embodiment of table and go out adsorbance in comparative example according to test result calculations
3 embodiment of table is with the adsorbance and specific surface area of, comparative example
It can be seen that embodiment 1 and embodiment 4 by graphene-supported in supporter from Fig. 3-Fig. 5.From table 1- table 3
It can be seen that the adsorbance of supporter, much smaller than the adsorbance to test sample, correspondingly, the adsorbance of supporter is much smaller than graphene
Adsorbance；Illustrate that the adsorbance using the adsorbance to test sample as graphene, error are smaller.Each to the survey three times of test sample
The measured value of amount very close to；Illustrate that the repetitive rate of method provided by the embodiments of the present application is good, reproducibility is good.
The supporter of embodiment 1- embodiment 3 is not identical, and finally obtained result differs very little, illustrates the material of supporter
Very little is influenced on final result.
Embodiment 1- embodiment 4, comparative example 1- comparative example 3 are detected with a collection of grapheme material, embodiment 1- embodiment 4
As a result very close, in error range, but comparative example 1- comparative example 3 and the result of embodiment fall far short；Illustrate the application
The method that embodiment provides is more accurate.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. a kind of method for measuring grapheme material powder specific-surface area detection, which is characterized in that mainly comprise the steps that
Use the detection of BET specific surface area detection method to the adsorbance of test sample for the first adsorbance；Described to test sample includes supporter
With the grapheme material for being carried on the supporter；
Obtain the quality to grapheme material in test sample；According to the quality of the grapheme material and first adsorbance
Calculate the specific surface area of grapheme material.
2. the method for measurement grapheme material powder specific-surface area detection according to claim 1, which is characterized in that the BET
The adsorbate of specific surface area detection method is nitrogen.
3. the method for measurement grapheme material powder specific-surface area detection according to claim 1, which is characterized in that the measurement
The method of grapheme material specific surface area further include:
The adsorbance for obtaining the supporter is the second adsorbance；
According to graphene described in the difference of first adsorbance and second adsorbance, the Mass Calculation of the grapheme material
The specific surface area of material.
4. the method for measurement grapheme material powder specific-surface area detection according to claim 3, which is characterized in that the acquisition
The adsorbance of the supporter be the second adsorbance the step of include:
Second adsorbance is calculated by the quality of supporter and the specific surface area of supporter.
5. the method for measurement grapheme material powder specific-surface area detection according to claim 1, which is characterized in that the support
Body is made of the material with gap or the supporter is made of thin-film material；
Optionally, the supporter is made of porous materials；
Optionally, the supporter is made of the metal material with gap；
Optionally, the material of the supporter includes nickel foam, foam copper, foamed aluminium, foamed iron, foam iron-nickel alloy or bubble
One of foam pltine is a variety of；
Optionally, the material of the supporter includes the polymer with hole configurations；
Optionally, the material of the supporter includes one of copper foil, aluminium foil or goldleaf or a variety of.
6. the method for measurement grapheme material powder specific-surface area detection according to claim 1-5, which is characterized in that
It is described to be made to test sample by following steps:
By grapheme material solution loadings in the supporter, the graphene material not adsorbed by the supporter is removed after dry
Material；
Optionally, the supporter by the grapheme material solution loadings after cleaning.
7. the method for measurement grapheme material powder specific-surface area detection according to claim 6, which is characterized in that the graphite
Alkene material solution is made by following steps:
Admixed graphite alkene material powder and ethanol water are centrifugally separating to obtain the grapheme material solution after ultrasonic disperse,
The concentration of grapheme material is 20~30mg/ml in the grapheme material solution.
8. the method for measurement grapheme material powder specific-surface area detection according to claim 6, which is characterized in that described by stone
Before the step of black alkene material solution is carried on the supporter, further includes:
Cutting out matrix is the matched size of testing tube with the BET specific surface area detection method.
9. the method for measurement grapheme material powder specific-surface area detection according to claim 6, which is characterized in that described by stone
Before the step of black alkene material solution is carried on the supporter, further includes:
The supporter is impregnated using organic solvent, the supporter is placed in water ultrasonic cleaning after ultrasonic cleaning, is then done
It is dry.
10. the method for measurement grapheme material powder specific-surface area detection according to claim 6, which is characterized in that described to incite somebody to action
Grapheme material solution loadings include: in the step of supporter
The supporter after cleaning is soaked in the grapheme material solution, is then freeze-dried.
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