CN112945997A - Sample preparation method for aqueous graphene slurry before scanning electron microscope - Google Patents
Sample preparation method for aqueous graphene slurry before scanning electron microscope Download PDFInfo
- Publication number
- CN112945997A CN112945997A CN202110136964.9A CN202110136964A CN112945997A CN 112945997 A CN112945997 A CN 112945997A CN 202110136964 A CN202110136964 A CN 202110136964A CN 112945997 A CN112945997 A CN 112945997A
- Authority
- CN
- China
- Prior art keywords
- solution
- graphene slurry
- aqueous graphene
- electron microscope
- scanning electron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 70
- 239000002002 slurry Substances 0.000 title claims abstract description 65
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 33
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 25
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 59
- 238000002604 ultrasonography Methods 0.000 claims description 17
- 238000005119 centrifugation Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 230000032798 delamination Effects 0.000 claims description 3
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- G01N23/2202—Preparing specimens therefor
-
- 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
- G01N23/225—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 using electron or ion
- G01N23/2251—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 using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/102—Different kinds of radiation or particles beta or electrons
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/635—Specific applications or type of materials fluids, granulates
Abstract
The invention discloses a sample preparation method for aqueous graphene slurry before scanning electron microscope treatment, which comprises the following steps: sampling into a centrifugal tube; (II) adding an organic solvent into the centrifugal tube and uniformly mixing to obtain a dispersion solution; thirdly, carrying out ultrasonic treatment on the dispersion solution to obtain an ultrasonic solution; fourthly, centrifuging the ultrasonic solution to obtain a layered solution, removing supernatant, reserving bottom slurry, adding an organic solvent into the bottom slurry, mixing uniformly, centrifuging again, and removing supernatant to reserve bottom slurry; taking the bottom slurry to another centrifugal tube, and adding an organic solvent to mix uniformly to obtain a diluted dispersion solution; carrying out ultrasonic treatment on the diluted dispersion solution to obtain a diluted dispersion ultrasonic treatment solution; and (seventhly), dripping the diluted dispersed ultrasonic treatment solution in the center of the silicon wafer, and performing machine test after vacuum drying or infrared lamp irradiation. The method can be used for more clearly observing the morphology and distribution condition of the graphene sheets in the graphene slurry during testing.
Description
Technical Field
The invention belongs to the technical field of scanning electron microscope testing, and particularly relates to a sample preparation method for aqueous graphene slurry before scanning electron microscope processing.
Background
Graphene is a novel material with super-excellent electrical conductivity and thermal conductivity, and no independent test national standard is made for graphene in the existing national standard, and only terms are described. Generally, before a Scanning Electron Microscope (SEM) test is performed on graphene, graphene and a solvent are stirred and mechanically peeled to prepare a graphene conductive slurry, the graphene conductive slurry is directly dropped on a silicon wafer, and SEM test observation is performed after drying, but the morphology of a graphene sheet in a real state cannot be generally seen through the SEM test of graphene performed by the sample preparation method.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a novel method for preparing a sample by pretreatment of a water-based graphene slurry in a scanning electron microscope, which aims to solve the problems in the background art, and the morphology and the distribution condition of a graphene sheet layer in the graphene slurry can be more clearly observed in the test process through the novel pretreatment sample preparation.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the sample preparation method for the aqueous graphene slurry before scanning electron microscope comprises the following steps:
sampling in the step (I): taking the aqueous graphene slurry into a centrifugal tube;
dispersing in the step (II): adding an organic solvent into the centrifugal tube, and uniformly mixing the organic solvent and the aqueous graphene slurry to obtain a dispersion solution, wherein the volume ratio of the aqueous graphene slurry to the organic solvent is 1: 4;
step (three), ultrasound: carrying out ultrasonic treatment on the dispersion solution to obtain an ultrasonic solution;
step (four) centrifugation: centrifuging the ultrasonic solution to obtain a layered solution, removing supernatant of the layered solution, leaving slurry at the bottom of the layered solution, adding an organic solvent with the volume 2-4 times that of the aqueous graphene slurry, uniformly mixing to obtain a mixed solution, centrifuging to obtain a re-layered solution, removing supernatant of the re-layered solution to obtain slurry at the bottom of the re-layered solution;
step (five), re-dilution and dispersion: adding 1/10 size of the bottom slurry of the delamination solution into another centrifugal tube, adding 2-4 times of the size of the organic solvent into the another centrifugal tube, and uniformly stirring to obtain a diluted dispersion solution;
and (VI) performing ultrasonic treatment: carrying out ultrasonic treatment on the diluted dispersion solution to obtain a diluted dispersion ultrasonic treatment solution;
preparing a sample: dropping the diluted dispersed ultrasonic treatment solution in the center of the silicon wafer, vacuum drying or irradiating by an infrared lamp, and then testing on a machine.
Further, in the step (one) of sampling, the adding amount of the aqueous graphene slurry is 5 ml;
in the dispersion in the step (II), the adding amount of the organic solvent is 20 ml;
in the centrifugation step (IV), the addition amount of the organic solvent is 10-20 ml;
in the step (five), in the re-dilution and dispersion, the adding amount of the organic solvent is 10-20 ml, and the taking amount of the slurry at the bottom of the re-layering solution is 0.5 ml.
Further, the organic solvent is absolute ethyl alcohol or acetone.
In the dispersion in the step (II), the uniform mixing mode is stirring, and the stirring time is 10 s.
Further, in the step (III) of ultrasound, the ultrasound parameters are set to be 150V of power, 25 ℃ of ultrasound temperature and 5min of ultrasound time.
Further, in the centrifugation in the step (IV), the centrifugation rotating speed is 4000 revolutions per minute, and the centrifugation time is 10 minutes.
Further, in the re-ultrasound in the step (six), the ultrasound parameters are set to be 150V in power, 25 ℃ in ultrasound temperature and 2min in ultrasound time.
Further, in the sample preparation in the step (seven), the dropping amount of the diluted and dispersed ultrasonic treatment solution is 15-30 mg.
Further, in the sample preparation in the step (VII), the vacuum drying temperature is 50 ℃ and the time is 5 min.
Further, in the sample preparation in the step (seven), the irradiation time of an infrared lamp is 5 min.
The invention has the beneficial effects that:
1. according to the sample preparation method for the aqueous graphene slurry before the scanning electron microscope, the aqueous adhesive bridge frame is damaged by repeatedly cleaning the aqueous graphene slurry with absolute ethyl alcohol or acetone, so that graphene is completely exposed in a solution, the absolute ethyl alcohol or acetone is volatilized more quickly to accelerate the drying of the graphene, and the secondary agglomeration of the graphene caused by overlong time in the drying process is avoided.
2. According to the sample preparation method for the aqueous graphene slurry before scanning electron microscope, provided by the invention, the agglomerated graphene in the aqueous graphene slurry is dispersed through high-frequency oscillation in ultrasonic treatment, so that the lamellar morphology of the graphene can be observed more clearly.
3. According to the sample preparation method for the aqueous graphene slurry before the scanning electron microscope, solid-liquid separation of the aqueous graphene slurry can be accelerated through a centrifugal machine in centrifugal treatment, compared with a natural sedimentation method, the treatment method is more thorough in solid-liquid separation and faster in sedimentation, not only is the graphene secondary agglomerated caused by overlong time, but also the sample preparation efficiency is high.
Drawings
FIG. 1 is a flowchart of the steps of a sample preparation method according to example 1;
FIG. 2 is an SEM photograph observed in example 1;
fig. 3 is an SEM image observed for the comparative example.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A sample preparation method for aqueous graphene slurry before scanning electron microscope (step flow is shown in figure 1) comprises the following steps:
sampling in the step (I): 5ml of aqueous graphene slurry with the solid content of 1-5% is put into a 25ml centrifugal tube;
dispersing in the step (II): adding 20ml of absolute ethyl alcohol into a centrifugal tube, stirring with the aqueous graphene slurry for 10s, and uniformly obtaining a dispersion solution;
step (three), ultrasound: putting the centrifuge tube filled with the dispersion solution into an ultrasonic cleaning instrument, and carrying out ultrasonic treatment to obtain an ultrasonic solution, wherein ultrasonic parameters are set to be 150V in power, the ultrasonic temperature is 25 ℃, and the ultrasonic time is 5 min;
step (four) centrifugation: placing a centrifugal tube filled with an ultrasonic solution into a centrifugal machine, carrying out centrifugal treatment to obtain a layered solution, removing supernatant of the layered solution, leaving slurry at the bottom of the layered solution, adding 10-20 ml of absolute ethyl alcohol into the slurry, shaking up until no solid-liquid separation phenomenon is seen to obtain a mixed solution, carrying out centrifugal treatment on the mixed solution for 10min to obtain a re-layered solution, removing supernatant of the re-layered solution to obtain slurry at the bottom of the re-layered solution, wherein the centrifugal speed is 4000 revolutions per minute, and the centrifugal time is 10 min;
step (five), re-dilution and dispersion: sucking 0.5ml of slurry at the bottom of the stratified solution by using a disposable dropper, adding the slurry into another centrifugal tube, adding 10-20 ml of absolute ethyl alcohol, and uniformly stirring until no solid-liquid separation phenomenon appears to obtain a diluted dispersion solution;
and (VI) performing ultrasonic treatment: putting the centrifuge tube filled with the diluted dispersion solution into an ultrasonic cleaning instrument, and carrying out ultrasonic treatment again to obtain the diluted dispersion ultrasonic treatment solution, wherein ultrasonic parameters are set to be 150V in power, the ultrasonic temperature is 25 ℃, and the ultrasonic time is 2 min;
preparing a sample: stirring the diluted dispersed ultrasonic treatment solution until no delamination occurs, sucking the solution by a disposable dropper and dripping the solution at the center of a bright surface of a silicon wafer, wherein the dripping amount is 15-30mg, performing vacuum drying at 50 ℃ for 5min or performing on-machine test after irradiating the solution by an infrared lamp for 5min, and the test conditions are that the bombardment voltage is 10.00 +/-1 kV, and the distance from the forefront of an objective lens to a sample plane is 15 +/-1 mm.
Example 2
The sample preparation method for the aqueous graphene slurry before scanning electron microscope is different from that of the example 1 only in that the organic solvent is acetone, and the rest of the settings are the same as those of the example 1.
Comparative example
A sample preparation method for aqueous graphene slurry before scanning electron microscope processing comprises the following steps:
sampling in the step (I): 5ml of aqueous graphene slurry with the solid content of 3.0% is put into a 25ml centrifugal tube;
dispersing in the step (II): adding 20ml of absolute ethyl alcohol into a centrifugal tube, stirring with the aqueous graphene slurry for 10s, and uniformly obtaining a dispersion solution;
step (three), sample preparation: sucking the dispersion solution with disposable dropper, dropping the dispersion solution onto the center of bright surface of silicon wafer at 15-30mg, vacuum drying at 50 deg.C for 5min or irradiating with infrared lamp for 5min, and testing under bombardment voltage of 10.00 + -1 kV and distance from the foremost edge of objective lens to sample plane of 15 + -1 mm.
The SEM image observed by the sample preparation method of example 1 is shown in FIG. 2, and the SEM image observed by the sample preparation method of comparative example is shown in FIG. 3. The sample subjected to the dispersion ultrasonic treatment and the centrifugal treatment by the absolute ethyl alcohol can clearly observe the shape and the distribution condition of graphene sheets under a scanning electron microscope, and the reason is probably because firstly, the aqueous graphene slurry is washed by the absolute ethyl alcohol for many times to destroy an aqueous adhesive bridge frame, so that the graphene is completely exposed in a solution, and the absolute ethyl alcohol can be volatilized more quickly to accelerate the drying of the graphene, so that the secondary agglomeration of the graphene in the drying process is avoided; secondly, dispersing agglomerated graphene in the aqueous graphene slurry through high-frequency oscillation in ultrasonic treatment; and thirdly, solid-liquid separation of the aqueous graphene slurry can be accelerated through centrifugal treatment, the solid-liquid separation is more thorough, the sedimentation is faster, and secondary agglomeration of graphene caused by overlong time is avoided. The samples in the comparative examples are not subjected to ultrasonic treatment, centrifugation and dilution treatment, and graphene is agglomerated together under a scanning electron microscope, so that the morphology and distribution condition of the single sheets are not clear. Therefore, the method can be used for more clearly observing the morphology and distribution condition of the graphene sheets in the graphene slurry during testing.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The sample preparation method for the aqueous graphene slurry before scanning electron microscope is characterized by comprising the following steps:
sampling in the step (I): taking the aqueous graphene slurry into a centrifugal tube;
dispersing in the step (II): adding an organic solvent into the centrifugal tube, and uniformly mixing the organic solvent and the aqueous graphene slurry to obtain a dispersion solution, wherein the volume ratio of the aqueous graphene slurry to the organic solvent is 1: 4;
step (three), ultrasound: carrying out ultrasonic treatment on the dispersion solution to obtain an ultrasonic solution;
step (four) centrifugation: centrifuging the ultrasonic solution to obtain a layered solution, removing supernatant of the layered solution, leaving slurry at the bottom of the layered solution, adding an organic solvent with the volume 2-4 times that of the aqueous graphene slurry, uniformly mixing to obtain a mixed solution, centrifuging to obtain a re-layered solution, removing supernatant of the re-layered solution to obtain slurry at the bottom of the re-layered solution;
step (five), re-dilution and dispersion: adding 1/10 size of the bottom slurry of the delamination solution into another centrifugal tube, adding 2-4 times of the size of the organic solvent of the aqueous graphene slurry, and uniformly mixing to obtain a diluted dispersion solution;
and (VI) performing ultrasonic treatment: carrying out ultrasonic treatment on the diluted dispersion solution to obtain a diluted dispersion ultrasonic treatment solution;
preparing a sample: dropping the diluted dispersed ultrasonic treatment solution in the center of the silicon wafer, vacuum drying or irradiating by an infrared lamp, and then testing on a machine.
2. The scanning electron microscope pretreatment sample preparation method of the aqueous graphene slurry according to claim 1,
in the step (one), in the sampling, the adding amount of the aqueous graphene slurry is 5 ml;
in the dispersion in the step (II), the adding amount of the organic solvent is 20 ml;
in the centrifugation step (IV), the addition amount of the organic solvent is 10-20 ml;
in the step (five), in the re-dilution and dispersion, the adding amount of the organic solvent is 10-20 ml, and the taking amount of the slurry at the bottom of the re-layering solution is 0.5 ml.
3. The scanning electron microscope pretreatment sample preparation method of the aqueous graphene slurry according to claim 1, wherein the organic solvent is absolute ethyl alcohol or acetone.
4. The method for preparing the sample before the scanning electron microscope of the aqueous graphene slurry according to claim 1, wherein in the step (two) of dispersing, the mode of uniform mixing is stirring, and the stirring time is 10 s.
5. The scanning electron microscope pretreatment sample preparation method for the aqueous graphene slurry according to claim 1, wherein in the step (three) of ultrasound, the power is set to 150V, the ultrasound temperature is set to 25 ℃, and the ultrasound time is set to 5 min.
6. The scanning electron microscope pretreatment sample preparation method for the aqueous graphene slurry according to claim 1, wherein in the centrifugation in the step (IV), the centrifugation rotation speed is 4000 rpm, and the centrifugation time is 10 min.
7. The scanning electron microscope pretreatment sample preparation method for the aqueous graphene slurry according to claim 1, wherein in the re-ultrasound in the step (six), the power is set to be 150V, the ultrasound temperature is 25 ℃, and the ultrasound time is 2 min.
8. The method for preparing the sample of the aqueous graphene slurry before scanning electron microscope processing according to claim 1, wherein in the step (seven) of sample preparation, the addition amount of the diluted dispersion ultrasonic treatment solution is 15-30 mg.
9. The method for preparing the sample of the aqueous graphene slurry before scanning electron microscope processing according to claim 1, wherein in the step (seven), the vacuum drying temperature is 50 ℃ and the time is 5 min.
10. The method for preparing the sample before the scanning electron microscope of the aqueous graphene slurry according to claim 1, wherein in the step (seven), the irradiation time of an infrared lamp is 5 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110136964.9A CN112945997A (en) | 2021-02-01 | 2021-02-01 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110136964.9A CN112945997A (en) | 2021-02-01 | 2021-02-01 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112945997A true CN112945997A (en) | 2021-06-11 |
Family
ID=76240796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110136964.9A Pending CN112945997A (en) | 2021-02-01 | 2021-02-01 | Sample preparation method for aqueous graphene slurry before scanning electron microscope |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112945997A (en) |
Citations (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993065A (en) * | 2010-12-17 | 2011-03-30 | 中国科学院上海微***与信息技术研究所 | Method for preparing graphene powder |
| CN102351174A (en) * | 2011-08-23 | 2012-02-15 | 华南理工大学 | Preparation method of dispersible silane functionalized graphene |
| CN102701190A (en) * | 2012-05-31 | 2012-10-03 | 格雷菲尼（北京）科技有限公司 | Process and method for preparing graphene in mixed solution of water and acetone |
| CN103708445A (en) * | 2013-12-25 | 2014-04-09 | 深圳市贝特瑞纳米科技有限公司 | Method for preparing graphene powder material and graphene powder material |
| CN103868768A (en) * | 2014-02-14 | 2014-06-18 | 河南省农业科学院植物保护研究所 | Treatment method of scanning electron microscope samples of insect tentacles and appendages |
| CN103880000A (en) * | 2014-03-07 | 2014-06-25 | 中南大学 | Preparation method of ultralight graphene powder |
| CN104071778A (en) * | 2014-06-20 | 2014-10-01 | 宁波墨西科技有限公司 | Graphene dispersion liquid and method for preparing graphene material power |
| CN104108700A (en) * | 2014-06-20 | 2014-10-22 | 宁波墨西科技有限公司 | Graphene material powder and preparation method |
| CN104777019A (en) * | 2015-03-25 | 2015-07-15 | 富耐克超硬材料股份有限公司 | Preparation method of cubic boron nitride micro-powder scanning electron microscopy sample |
| CN104849127A (en) * | 2015-05-29 | 2015-08-19 | 北京市理化分析测试中心 | Pretreatment method of oil field multi-component oil sludge and application |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| WO2016045035A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Method for preparing graphene |
| CN106025202A (en) * | 2016-05-25 | 2016-10-12 | 福建翔丰华新能源材料有限公司 | Preparation method of silicon-graphene compound conductive paste |
| US20160311688A1 (en) * | 2013-12-31 | 2016-10-27 | Shenzhen Cantonnet Energy Services Co. , Ltd. | A preparation method of graphene and graphene oxide based on mixed acid system |
| US20160347617A1 (en) * | 2013-12-31 | 2016-12-01 | Shenzhen Cantonnet Energy Services Co. , Ltd. | A preparation method of graphene as well as graphene oxide based on anthracite |
| CN106248605A (en) * | 2016-08-05 | 2016-12-21 | 常州第六元素材料科技股份有限公司 | The quantitative detecting method of a kind of graphene oxide degree of oxidation and the building method of standard curve used |
| CN106315566A (en) * | 2016-08-15 | 2017-01-11 | 安徽师范大学 | Preparation method of graphene |
| CN106744841A (en) * | 2016-12-21 | 2017-05-31 | 广东工业大学 | A kind of preparation method of the three-dimensional porous graphene film that single-layer graphene is constructed |
| CN107449649A (en) * | 2017-07-25 | 2017-12-08 | 合肥国轩高科动力能源有限公司 | Pre-treating method during a kind of graphene conductive slurry detection metal element content |
| CN107576624A (en) * | 2017-08-31 | 2018-01-12 | 中国人民解放军第三军医大学 | The detection method of cortisol in a kind of saliva |
| US20180029889A1 (en) * | 2016-06-21 | 2018-02-01 | Shenzhen Cantonnet Energy Services Co. , Ltd. | Preparation method of graphene |
| CN108383111A (en) * | 2018-05-11 | 2018-08-10 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene slurry and preparation method thereof |
| CN108630338A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus for producing graphene conductive slurry in batches and graphene conductive slurry prepared therefrom |
| CN109903931A (en) * | 2019-02-25 | 2019-06-18 | 天津艾克凯胜石墨烯科技有限公司 | A kind of preparation method of high dispersive graphene composite conductive slurry |
| CN110006937A (en) * | 2019-04-02 | 2019-07-12 | 深圳鸿鹏新能源科技有限公司 | Utilize the method for scanning electron microscope test sample under limiting resolution |
| CN111678764A (en) * | 2020-06-17 | 2020-09-18 | 中国科学院地球化学研究所 | Method for preparing sample by pre-treating phosphate oxygen isotope of fresh water sample |
| CN111899985A (en) * | 2020-05-29 | 2020-11-06 | 中山大学 | Preparation method and application of titanium nitride/graphene composite material |
-
2021
- 2021-02-01 CN CN202110136964.9A patent/CN112945997A/en active Pending
Patent Citations (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993065A (en) * | 2010-12-17 | 2011-03-30 | 中国科学院上海微***与信息技术研究所 | Method for preparing graphene powder |
| CN102351174A (en) * | 2011-08-23 | 2012-02-15 | 华南理工大学 | Preparation method of dispersible silane functionalized graphene |
| CN102701190A (en) * | 2012-05-31 | 2012-10-03 | 格雷菲尼（北京）科技有限公司 | Process and method for preparing graphene in mixed solution of water and acetone |
| CN103708445A (en) * | 2013-12-25 | 2014-04-09 | 深圳市贝特瑞纳米科技有限公司 | Method for preparing graphene powder material and graphene powder material |
| US20160347617A1 (en) * | 2013-12-31 | 2016-12-01 | Shenzhen Cantonnet Energy Services Co. , Ltd. | A preparation method of graphene as well as graphene oxide based on anthracite |
| US20160311688A1 (en) * | 2013-12-31 | 2016-10-27 | Shenzhen Cantonnet Energy Services Co. , Ltd. | A preparation method of graphene and graphene oxide based on mixed acid system |
| CN103868768A (en) * | 2014-02-14 | 2014-06-18 | 河南省农业科学院植物保护研究所 | Treatment method of scanning electron microscope samples of insect tentacles and appendages |
| CN103880000A (en) * | 2014-03-07 | 2014-06-25 | 中南大学 | Preparation method of ultralight graphene powder |
| CN104071778A (en) * | 2014-06-20 | 2014-10-01 | 宁波墨西科技有限公司 | Graphene dispersion liquid and method for preparing graphene material power |
| CN104108700A (en) * | 2014-06-20 | 2014-10-22 | 宁波墨西科技有限公司 | Graphene material powder and preparation method |
| WO2016045035A1 (en) * | 2014-09-25 | 2016-03-31 | 深圳粤网节能技术服务有限公司 | Method for preparing graphene |
| CN104777019A (en) * | 2015-03-25 | 2015-07-15 | 富耐克超硬材料股份有限公司 | Preparation method of cubic boron nitride micro-powder scanning electron microscopy sample |
| CN104849127A (en) * | 2015-05-29 | 2015-08-19 | 北京市理化分析测试中心 | Pretreatment method of oil field multi-component oil sludge and application |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| CN106025202A (en) * | 2016-05-25 | 2016-10-12 | 福建翔丰华新能源材料有限公司 | Preparation method of silicon-graphene compound conductive paste |
| US20180029889A1 (en) * | 2016-06-21 | 2018-02-01 | Shenzhen Cantonnet Energy Services Co. , Ltd. | Preparation method of graphene |
| CN106248605A (en) * | 2016-08-05 | 2016-12-21 | 常州第六元素材料科技股份有限公司 | The quantitative detecting method of a kind of graphene oxide degree of oxidation and the building method of standard curve used |
| CN106315566A (en) * | 2016-08-15 | 2017-01-11 | 安徽师范大学 | Preparation method of graphene |
| CN106744841A (en) * | 2016-12-21 | 2017-05-31 | 广东工业大学 | A kind of preparation method of the three-dimensional porous graphene film that single-layer graphene is constructed |
| CN107449649A (en) * | 2017-07-25 | 2017-12-08 | 合肥国轩高科动力能源有限公司 | Pre-treating method during a kind of graphene conductive slurry detection metal element content |
| CN107576624A (en) * | 2017-08-31 | 2018-01-12 | 中国人民解放军第三军医大学 | The detection method of cortisol in a kind of saliva |
| CN108630338A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus for producing graphene conductive slurry in batches and graphene conductive slurry prepared therefrom |
| CN108383111A (en) * | 2018-05-11 | 2018-08-10 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of graphene slurry and preparation method thereof |
| CN109903931A (en) * | 2019-02-25 | 2019-06-18 | 天津艾克凯胜石墨烯科技有限公司 | A kind of preparation method of high dispersive graphene composite conductive slurry |
| CN110006937A (en) * | 2019-04-02 | 2019-07-12 | 深圳鸿鹏新能源科技有限公司 | Utilize the method for scanning electron microscope test sample under limiting resolution |
| CN111899985A (en) * | 2020-05-29 | 2020-11-06 | 中山大学 | Preparation method and application of titanium nitride/graphene composite material |
| CN111678764A (en) * | 2020-06-17 | 2020-09-18 | 中国科学院地球化学研究所 | Method for preparing sample by pre-treating phosphate oxygen isotope of fresh water sample |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111607845B (en) | Tellurium/graphene hybrid fiber with photoelectric effect and preparation method and application thereof | |
| KR101902206B1 (en) | Manufacturing method of silica with improved surface area from biomass | |
| CN112945997A (en) | Sample preparation method for aqueous graphene slurry before scanning electron microscope | |
| CN110364690B (en) | Preparation method of negative electrode material, negative electrode material and lithium battery | |
| JP2006248955A (en) | Method and apparatus for acid treatment | |
| CN110937584B (en) | Boron nitride nanosheet and preparation method thereof | |
| CN112763371A (en) | Method for testing solid content of lithium battery slurry | |
| CN106346019A (en) | Graphene supported micron-gold core-shell structure and preparation method thereof | |
| CN104925786A (en) | Novel method for preparing graphene by utilizing low-boiling-point organic solvent in stripping manner | |
| CN110161066B (en) | Method for extracting inclusions in steel through non-aqueous solution electrolysis | |
| CN114735685A (en) | Preparation method of fluorinated graphene | |
| CN1876288A (en) | Method for preparing high brightness nano-grade aluminum powder using film transition method | |
| CN113754671A (en) | Preparation method of sodium copper chlorophyllin | |
| CN110586930B (en) | Preparation method of nano titanium material for corrosion prevention | |
| CN109052341A (en) | A kind of preparation method of GaSe nano rod | |
| CN115144323B (en) | Method for detecting content of non-metallic inclusions in metal powder for additive manufacturing | |
| CN108783404A (en) | A kind of preparation method of low-temperature instant agar | |
| CN113552152A (en) | Pretreatment method for scanning electron microscope test of aqueous graphene slurry | |
| CN114231930B (en) | Method for preparing ultra-dense hot spot space structure | |
| CN111733481B (en) | Tellurium/graphene hybrid fiber membrane with photoelectric effect and preparation method and application thereof | |
| CN116165232A (en) | Sample preparation method for observing silver halide particles by scanning electron microscope | |
| CN113252413A (en) | Diatom inspection method | |
| CN116067741A (en) | Method for enhancing high-starch-content seed micro CT contrast | |
| CN117777764A (en) | Preparation method of ultra-low cutting point spherical silicon micro powder for HDI | |
| SU1594191A1 (en) | Method of producing nigh-dispersion mica filler |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210611 |