CN103149249A - Method for quickly detecting graphene in solution - Google Patents
Method for quickly detecting graphene in solution Download PDFInfo
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- CN103149249A CN103149249A CN2013100664099A CN201310066409A CN103149249A CN 103149249 A CN103149249 A CN 103149249A CN 2013100664099 A CN2013100664099 A CN 2013100664099A CN 201310066409 A CN201310066409 A CN 201310066409A CN 103149249 A CN103149249 A CN 103149249A
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Abstract
The invention discloses a method for quickly detecting graphene in a solution. The method comprises the following steps of: adding a pair of metal electrodes or graphite electrodes in the graphene-containing solution, externally connecting a desk-type multimeter with a standard interface, an LCR (Inductance, Capacitance, Resistance) meter or an impedance analyzer with the electrodes, and associating the external device with a microcomputer by programming; and regularly reading data, such as conductance/resistance, admittance/impedance, of the solution, storing the data in the form of a data file, and drawing a graph indicating variation of the conductance/resistance and the admittance/impedance with time so as to track the change of concentration of the graphene in the solution and further realize the aim of rapid detection on the graphene. The graphene solution with the known concentration is detected to obtain a standard work curve, and then the content of the graphene in an unknown solution can be detected according to the standard work curve. The graphene solution detection method provided by the invention is simple and convenient to use, can quickly perform on-line monitoring or off-line detection, and can be used for controlling a graphene production and preparation process, detecting graphene content, researching the characteristics of graphene in solutions, and so on.
Description
Technical field
The invention belongs to the Fast Detection Technique of Graphene content in solution, relate to a kind of Fast Detection Technique of organic or inorganic solution of graphene-containing.
Background technology
Graphene is a kind of emerging two-dimensional nano material, has high mechanical strength and electric conductivity.Adopt the method directly peel off graphite can make to get the Graphene that defective is few, performance is good, as with graphite direct ultrasonic peeling off in 1-METHYLPYRROLIDONE.But in preparation process and the preparation complete after, all need Graphene is detected.
Existing Graphene detection method is to adopt the instruments such as scanning electron microscope, Raman spectrum, X-ray diffraction, uv-vis spectra to detect.These method complicated operations are wasted time and energy, and cost is high, and can't the forming process of on-line monitoring Graphene in solution.Given this, be necessary to develop a kind of method that can the fast detecting Graphene.
Summary of the invention
The object of the invention is to provide a kind of method that can on-line monitoring Graphene generative process, and the content of Graphene in can fast detecting solution.
To achieve these goals, the present invention adopts following technical scheme:
Graphene detection method in a kind of solution, this detection method use pair of metal electrodes or graphite electrode to insert in solution, and external employing has the desk-top multimeter of standard interface, by programming, itself and microcomputer are linked; The electricity that regularly reads solution leads/resistance data and be saved as data file, draw electricity to lead/resistance is to the variation figure along with the time, thereby the concentration change of following the tracks of Graphene in solution reaches the purpose of fast monitored.
Further, for the higher solution of resistance, can adopt the method for measurement AC admittance/impedance to detect.External instrument can be electric impedance analyzer or LCR Meter.
Further, quantitative test Graphene content, the electricity that can at first test different temperatures, different solvents, variable concentrations graphene solution is led, the admittance typical curve, then according to measured data, checks the content that typical curve can obtain Graphene in solution.
Further, described electrode is metal electrode or graphite electrode.
Further, described solution system comprises organic solvent and the mixed organic solvents systems thereof such as organic solvent Graphene system such as dimethyl formamide, dimethyl acetamide, 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), Ergol, inorganic solvent Graphene system such as water and acid, alkali, salt solusion system.
Further, for electric conductivity solution system preferably, can adopt methods such as measuring direct current resistance, electric current, electricity are led, I-V characteristic, AC impedance, admittance to carry out the monitoring of Graphene content.
Further, for the relatively poor solution system of electric conductivity, can adopt the methods such as measurement AC admittance/impedance to carry out the monitoring of Graphene content, comprise admittance, impedance operator under different frequency and bias voltage.
Good effect of the present invention:
1) method is easy.
2) but fast detecting.
3) with low cost.
The present invention is used for the on-line monitoring of direct stripping method Graphene production run, can be used for the fast characterizing of graphene solution concentration.
Description of drawings
Fig. 1 is that in graphite provided by the invention/ultrasonic stripping process of 1-METHYLPYRROLIDONE system, DC conductance is with the variation of ultrasonic time.
Fig. 2 is that in graphite provided by the invention/ultrasonic stripping process of 1-METHYLPYRROLIDONE system, admittance is with the variation of ultrasonic time and frequency.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Detection method provided by the invention uses pair of metal electrodes or graphite electrode to insert in solution, electrode is received on the have standard interface testing apparatus of (gpib interface or RS232 serial ports etc.), as desk-top multimeter Keithley2000, LCR table or electric impedance analyzer Agilent4192A and intelligent temperature controller etc., by programming (as VEE, Labview etc.), itself and microcomputer are linked; Program timing circulation reads the electricity of solution system and leads/data such as resistance data, admittance/impedance, temperature and be saved as data file, draw electricity to lead/resistance, admittance/impedance is to the variation figure along with time, temperature, thereby the concentration change of Graphene in tracking solution reaches the purpose of monitoring.
Embodiment 1: in the 250ml there-necked flask, inserting a pair of area is 1cm
2Copper electrode, insert a P t100 thermal resistance, add 100ml 1-METHYLPYRROLIDONE solvent, add 0.1g graphite, be placed in ultrasonic cleaning machine.Electrode is connected to Keithley2000Multimeter, the PT100 thermal resistance is connected to the XMTG-908 intelligent temperature controller.Microcomputer is connected the employing gpib interface with Keithley2000Multimeter, be connected with intelligent temperature controller to adopt the RS232 interface.The online testing software that has the functions such as timing sampling, drawing, data deposit with the VEE exploitation on microcomputer regularly reads the resistance data (can be converted into electricity leads) of solution under constant temperature 50 degree and ultrasonic state, thus the concentration change of Graphene in reaction solution.
Should be understood that; for those of ordinary skills; can be improved according to the above description or conversion, more particularly be the measurement of the physical quantity of reciprocal relation, and all these improve and conversion all should belong to the protection domain of claims of the present invention.
Claims (7)
1. Graphene detection method in a solution, is characterized in that, this detection method uses pair of metal electrodes or graphite electrode to insert in solution, and external employing has the desk-top multimeter of standard interface, by programming, itself and microcomputer is linked; The electricity that regularly reads solution leads/resistance data and be saved as data file, draw electricity to lead/resistance is to the variation figure along with the time, thereby the concentration change of following the tracks of Graphene in solution reaches the purpose of fast monitored.
2. detection method according to claim 1, is characterized in that, for the higher solution of resistance, adopts the method for measuring AC admittance/impedance to detect; External instrument is electric impedance analyzer or LCR Meter.
3. detection method according to claim 1, it is characterized in that, want quantitative test Graphene content, the typical curves such as the electricity of at first testing different temperatures, different solvents, variable concentrations graphene solution is led, admittance, according to unknown concentration solution measured data, check the content that typical curve can obtain Graphene in solution again.
4. detection method according to claim 1, is characterized in that, described electrode is metal electrode or graphite electrode.
5. detection method according to claim 1, is characterized in that, described solution system comprises organic solvent Graphene system, inorganic solvent Graphene system.
6. detection method according to claim 1, is characterized in that, for electric conductivity solution system preferably, adopts methods such as measuring direct current resistance, electric current, electricity are led, I-V characteristic, AC impedance, admittance to carry out the monitoring of Graphene content.
7. detection method according to claim 1, is characterized in that, for the relatively poor solution system of electric conductivity, can adopt measurement AC admittance/impedance to carry out the monitoring of Graphene content, comprises admittance, impedance operator under different frequency and bias voltage.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100664099A CN103149249A (en) | 2013-03-01 | 2013-03-01 | Method for quickly detecting graphene in solution |
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| CN2013100664099A CN103149249A (en) | 2013-03-01 | 2013-03-01 | Method for quickly detecting graphene in solution |
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| CN103149249A true CN103149249A (en) | 2013-06-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982596A (en) * | 2018-09-26 | 2018-12-11 | 新疆烯金石墨烯科技有限公司 | A kind of measuring method and device of graphene oxide solution concentration |
| CN109974775A (en) * | 2019-01-14 | 2019-07-05 | 天元羲王控股有限公司 | Detection device and its method on the transfer matic of graphene production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2932383Y (en) * | 2006-05-29 | 2007-08-08 | 长春工业大学 | Detector of ion content in solutions |
| CN101776630A (en) * | 2010-03-12 | 2010-07-14 | 清华大学 | Concentration measuring method and device of lithium bromide water solution |
| CN102169102A (en) * | 2011-01-13 | 2011-08-31 | 福州大学 | Method for monitoring and analyzing concentration of nano-carbon material electrophoretic deposition liquid |
| CN202330341U (en) * | 2011-11-24 | 2012-07-11 | 东莞市常晋凹版模具有限公司 | Detector for online detection of sulfuric acid content in acid copper-plating solution by conductivity method |
-
2013
- 2013-03-01 CN CN2013100664099A patent/CN103149249A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2932383Y (en) * | 2006-05-29 | 2007-08-08 | 长春工业大学 | Detector of ion content in solutions |
| CN101776630A (en) * | 2010-03-12 | 2010-07-14 | 清华大学 | Concentration measuring method and device of lithium bromide water solution |
| CN102169102A (en) * | 2011-01-13 | 2011-08-31 | 福州大学 | Method for monitoring and analyzing concentration of nano-carbon material electrophoretic deposition liquid |
| CN202330341U (en) * | 2011-11-24 | 2012-07-11 | 东莞市常晋凹版模具有限公司 | Detector for online detection of sulfuric acid content in acid copper-plating solution by conductivity method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982596A (en) * | 2018-09-26 | 2018-12-11 | 新疆烯金石墨烯科技有限公司 | A kind of measuring method and device of graphene oxide solution concentration |
| CN109974775A (en) * | 2019-01-14 | 2019-07-05 | 天元羲王控股有限公司 | Detection device and its method on the transfer matic of graphene production |
| CN109974775B (en) * | 2019-01-14 | 2022-04-19 | 天元羲王控股有限公司 | Automatic on-line detection equipment and method for graphene production |
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Application publication date: 20130612 |