KR101790506B1 - Graphene family organic elements analysis method and apparatus using plasma - Google Patents
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Abstract
The present invention relates to a method and apparatus for analyzing an organic element component of a graphene family using plasma.
The present invention relates to: (a) a step of preparing an aqueous graphene solution in which a graphene family is dissolved in water; (b) inducing the water and the water-soluble graphene family into a plasma state to completely dissolve the graphene family; And (c) analyzing the components by sending the organic elements in the plasma to a detector; A method of analyzing a graphene family organic element component comprising the steps of:
Description
The present invention relates to a method and apparatus for analyzing an organic element component of a graphene family using plasma.
Graphite Oxide (GO) has been manufactured and studied in various forms for over 100 years. For example, Hofman and Frenzel (Ber. 53B, 1248 (1930)), Hamdi (Kolloid Beihefte, 54, 554 (1943)), Carbon 42, 292937 (2004), Chem. Mater. 19, 4396 (2007).
Graphite oxides (GO) maintains between 1 and 20 layers of graphite, has many defects and surface reactors, and is very well dispersed in water. These surface reactors can also be various substituents through simple reactions. Include a functional group bonded to this reaction, such as before and after the graphite oxide -OH, -COOH, -CONH 2, -NH 2, -COO-, -SO 3 -, -NR 3+, -CH = O, C-OH, ≫ O, CX and the like, and the combination of the graphite oxide with the functional group also falls within the category of graphite oxide.
These graphite oxides (GO) can be produced in the form of graphene through a chemical reduction method (hydrazine treatment or the like) or a thermal reduction method. At this time, the reduced graphene is called Reduced Graphene Oxide (RGO).
On the other hand, a graphene nanoplate (GNP or carbon nanoplate) having a thickness of 5 to 100 nm which is obtained by physically peeling the graphite or expanding the graphite intercalation compound and peeling the graphite from the solvent or physically peeling the graphite Graphene (GP) having a thickness of 5 to 10 nm or less, CVD-GP (CVD-GP) manufactured using a CVD method, and graphene quantum dot (GP-QD) having a diameter of 30 nm or less.
Hereinafter, GO, RGO, GNP, GP, CVD-GP, and GP-QD will be collectively referred to as graphene families. As described above, the graphene family is classified according to the thickness, the composition, the manufacturing method, and the like, and derivatives, dopants, and surface treatment structures of the graphene family are also included in the category of the graphene family.
The constituent elements of the graphene family include most of carbon elements and elements such as oxygen, sulfur, phosphorus, hydrogen, nitrogen, hydrogen, and boron. Analysis of these elemental components is essential for the determination of graphene purity, doping elements and formulas.
A typical CS or elemental analyzer is inadequate for use in graphene applications where error rates exceed 1% and require precision.
Chemical analysis using X-ray photoelectron spectroscopy (XPS) is an analytical technique with 0.1% equipment error rate. However, even with chemical binding analysis by XPS, trace elements are not detected, and multiple peaks are superimposed on the result of the analysis, so that elaborate chemical bonding information can not be obtained. In addition, it is possible to analyze only the surface components, and there is a problem that analysis is not possible for the inner and lower graphenes of the analyte.
The most accurate analytical method for elemental analysis of PPm and ppb or less is the ICP-AES (inductively-coupled plasma atomic-emission spectrometer) or ICP-MS (ICP mass spectrometer) analysis.
However, these ICP-AES and ICP-MS analyzes are difficult to analyze organic components such as carbon elements for the following two reasons.
(1) Carbon components are oxidized and an exothermic reaction occurs, resulting in an incomplete inductively coupled plasma.
(2) Organics are not well ionized in the plasma, but adhere to equipment nozzles and pollute.
For the above reasons, the use of organic solvents in ICP is prohibited. In addition, we burn all the organic substances in advance, or burn out all of them in boiling strong acid. Therefore, only the remaining inorganic components are analyzed.
It is an object of the present invention to provide a method and apparatus for precisely analyzing organic components of a graphene family.
The present invention relates to: (a) a step of preparing an aqueous graphene solution in which a graphene family is dissolved in water; (b) inducing the water and the water-soluble graphene family into a plasma state to completely dissolve the graphene family; And (c) analyzing the components by sending the organic elements in the plasma to a detector; A method of analyzing a graphene family organic element component comprising the steps of:
Wherein the graphene family is one of GO, RGO, GP, GNP, CVD-GP and GP-QD, and the weight of the graphene family in step (a) is not more than 0.1 wt% . In the step (a), the graphene family having the hydrophilic group introduced therein may be dissolved in water to prepare the graphene aqueous solution.
In the step (b), the graphene aqueous solution may be sprayed onto the inductively coupled plasma or laser to be irradiated to induce a plasma and a water-soluble and graphene family dissolved in water.
The detector may be an Atomic-Emission Spectrometer (AES) or a Mass Spectrometer (MS).
Further, the present invention relates to " an introduction part into which an aqueous graphene solution is injected; A vacuum chamber coupled with the inlet; An aqueous solution supplier providing the aqueous solution of graphene from the inlet to the vacuum chamber; An energy supply for irradiating energy to induce a material in the vacuum chamber into a plasma state; And a detector communicating with the vacuum chamber, wherein the organic element in the plasma of the vacuum chamber is configured to move to the detector.
The aqueous solution supply unit may be configured to inject the graphene aqueous solution toward the vacuum chamber.
Through the above-described present invention, the organic element component of the graphene family can be analyzed with high accuracy.
1 is a schematic diagram of an apparatus for analyzing an organic element component of a graphene family provided by the present invention.
1. Graphene Family Organic Elements Analysis Method
The present invention relates to a process for producing a graphene aqueous solution, comprising the steps of: (a) preparing a graphene aqueous solution having a graphene family content of 0.1 wt% or less (excluding 0 wt%); (b) Spraying a solution of the graphene aqueous solution and water into a plasma state to completely dissolve the graphene family, and (c) analyzing the components of the plasma by sending the organic elements to the detector. A method of analyzing a graphene family organic element component comprising the steps of:
The step (a) is a step of preparing an aqueous solution of graphene in which a graphene family is dissolved in water.
The graphene family is any one of GO, RGO, GP, GNP, CVD-GP, and GP-QD. Derivatives, dopants and surface treatment structures of such graphene families may also be included in the category of graphene families have.
In the step (a), the weight of the graphene family is preferably 0.1 wt% or less (excluding 0 wt%) of the aqueous solution. If the weight of the graphene family exceeds 0.1 wt% of the aqueous solution, there is a risk of natural contamination (if the weight of the graphene family exceeds 0.1 wt% of the aqueous solution, the entire organic material may not be 100% decomposed And the organic matter adheres to the vicinity of the introduction portion of the aqueous solution and the portion of the aqueous solution supply (nozzle), so that it can operate as a permanent contaminant). The optimum concentration of the graphene aqueous solution is 0.1PPb to 100PPm.
In the step (a), a graphene family having a hydrophilic group (typically -OH or -COOH) introduced therein may be dissolved in water to prepare the graphene aqueous solution. The graphene family may be acid-treated to introduce a hydrophilic group into the graphene family, or a hydrophilic group may be introduced by a method of applying strong energy such as ultrasonic waves.
In the step (b), the water and the water-soluble graphene family are introduced into a plasma state to completely dissolve the graphene family. In the step (b), the graphene aqueous solution may be injected into the irradiated inductively coupled plasma or laser to induce the water and the graphene family dissolved in the water to a plasma state. That is, in this step, the graphene aqueous solution is injected into a laser or an inductively coupled plasma having sufficient energy to decompose the injected aqueous solution into elements such as ions. The spraying of the graphene aqueous solution may be performed in a liquid phase, liquid phase microcapsule, aerosol state, or the like.
When the graphene aqueous solution is injected, an optimal plasma induction environment can be created by controlling the injection amount, the amount of the mixed gas, and the like.
Plasma for the complete dissociation of the graphene family must have a higher energy efficiency or energy density than the plasma of conventional ICP equipment with an energy sufficient to break the graphene carbon bond structure and ionize it.
The step (c) is a step of analyzing the components by sending the organic elements in the plasma to a detector. An AES (Atomic-Emission Spectrometer) or MS (Mass Spectrometer) may be used as the detector, and a cation or an anion of organic elements present on the plasma can be detected through the AES or MS.
For example, when the MS device is used in step (c), either an anion mass analysis or a cation mass analysis can be performed.
delete
2. Graphene family organic element composition analyzer
The present invention is characterized by: an introduction portion into which a graphene aqueous solution having a graphene family content of 0.1 wt% or less (excluding 0 wt%) is injected; A vacuum chamber coupled with the inlet; An aqueous solution supplier for spraying the graphene aqueous solution from the inlet portion toward the vacuum chamber; An energy supply for irradiating an inductively coupled plasma or laser to induce a material in the vacuum chamber into a plasma state; And a detector in communication with the vacuum chamber; Wherein water in the aqueous solution of the graphene solution injected into the vacuum chamber and the graphene family dissolved in the water are introduced into a plasma state and the organic element in the plasma generated by the complete dissociation of the graphene family is moved to the detector And a graphene family organic element component analyzer configured to perform the analyzing process.
The lead-in portion is a unit in which the graphene family is injected with an aqueous solution of graphene dissolved in water. The introduction portion may be configured to be accommodated in a state in which the graphene aqueous solution is injected in a predetermined amount, or may be configured to discharge the graphene aqueous solution into the vacuum chamber through the aqueous solution supply portion, which will be described later.
The vacuum chamber is coupled to the inlet. Since the graphene family is dissociated in a plasma state in the vacuum chamber, the vacuum chamber must be resistant to plasma etching.
The aqueous solution provider may be configured to inject the graphene aqueous solution toward the vacuum chamber, the component providing the graphene aqueous solution from the inlet to the vacuum chamber.
The energy providing unit is a component for irradiating energy to induce a substance in the vacuum chamber into a plasma state, and any one of a laser irradiation apparatus or an inductively coupled plasma providing apparatus can be applied. The inductively coupled plasma provided in the inductively coupled plasma providing apparatus must be stable in the reaction of exothermic reaction of organic matter, be capable of cracking the graphene family, and contain high energy capable of ionizing carbon.
The detector may detect an organic element moved in the vacuum chamber. The detector may be an Atomic-Emission Spectrometer (AES) or a Mass Spectrometer (MS), and the organic Cations or anions of the elements can be detected.
The concentration gradient due to the pressure difference occurs at the detector side where the vacuum is maintained, and the ions selected by the pulling force generated by the electrical repulsive force generated by the finally selected anion or cation and the pulling force generated by the electrical attraction collide with the detector .
3. Graphene Family Organic Elements Component Qualitative Analysis Method
(1) preparing the graphene family element component analysis; (2) deriving an elemental component reference of a reference material using the graphene family element analysis apparatus; (3) analyzing an element component of the analyte using the graphene family element analyzer; And (4) qualitatively analyzing an element component of the analyte on the basis of the reference; A method for qualitative analysis of graphene family organic element components "
4. Quantification Analysis example
This analysis example is an analysis of an organic element component according to the present invention on GO-hydrolytically synthesized commercial GP-QD two species (-OH introduced species and -COOH introduced species).
The GO applied to this present example was obtained by using the Modified Hummers method, and the specific method is as follows.
Add 50 g of micro graphite powder and 40 g of NaNO 3 in 200 mL of H 2 SO 4 solution and slowly add 250 g of KMnO 4 over 1 hour while cooling. Then slowly add 5 L of 4-7 % H 2 SO 4 over 1 hour and add H 2 O 2 . After that, the precipitate is washed with 3% H 2 SO 4 -0.5% H 2 O 2 and distilled water to obtain a yellowish brown graphene oxide (GO) water-based slurry.
The weight ratio of the solute in the GO and GP-QD solutes was 0.01 wt% for the GO aqueous solution, 0.1 wt% for the GP-QD with the -OH group, and the GP-QD aqueous solution containing the -COOH group And 0.01 wt%, respectively.
A laser was used to introduce a strong plasma to completely dissociate the graphene family of the aqueous solution. Specifically, the GO aqueous solution dissolved in water and the aqueous solution of the two kinds of GP-QD were injected into a vacuum chamber using a micro-syringe, respectively, and a strong laser beam was applied to the sprayed liquid to make plasma and graphene components contained in water and water.
Next, the organic elements in the plasma are sent to the mass spectrometer by an electric propulsion force for mass analysis.
[Table 1] summarizes the results of the above analysis. The values in the table are the MS intensity values relative to 100 carbon. The MS intensity value is the intensity intensity value according to the detection sensitivity, and the sensitivity is different depending on the element, and accurate quantitative analysis is performed by reference measurement. However, it provides important key information that can be used to estimate relative quantitative differences and approximate quantitative analyzes per sample.
In this analytical example, a laser is used to induce water and graphene components into a plasma state, but complete dissociation of the graphene family can be achieved by irradiating the inductively coupled plasma.
5. Qualitative Analysis Example
(0.1 ppb, 0.1 ppm, 0.1mwt%) of high purity ethanol as a reference material for qualitative analysis, respectively, and then, using the principle of the present invention, a calibration curve for carbon, hydrogen and oxygen Can be obtained. If the concentration is correct, the amount of carbon, hydrogen, and oxygen for the aqueous solution is accurate, and the calibration error can be obtained by measuring three or more different concentrations. By using the obtained calibration curve as a reference, the amount of carbon, oxygen, and hydrogen contained in graphene can be quantified by measuring an aqueous solution of graphene having an unknown concentration.
Since carbon and oxygen can easily flow in from contamination sources, errors of quantitative value can be large. Therefore, when reference is made to ethanol or other organic matter containing carbon isotope 13 or ethanol or organic matter containing oxygen isotope, Can be developed.
10: introduction part 20: vacuum chamber 30: aqueous solution supply
40: Energy supply 50: Detector
Claims (9)
(b) injecting the graphene aqueous solution into an inductively coupled plasma or laser irradiated in a vacuum chamber to induce a plasma state of the graphene family dissolved in water and water of the graphene aqueous solution to completely dissolve the graphene family; And
(c) analyzing the components by sending the organic elements in the plasma to a detector; ≪ / RTI >
Wherein the graphene family is one of GO, RGO, GP, GNP, CVD-GP, and GP-QD.
Wherein the step (a) comprises dissolving the hydrophilic group-introduced graphene family in water.
Wherein the detector is an Atomic-Emission Spectrometer (AES) or a Mass Spectrometer (MS).
A vacuum chamber coupled with the inlet;
An aqueous solution supplier for spraying the graphene aqueous solution from the inlet portion toward the vacuum chamber;
An energy supply for irradiating an inductively coupled plasma or laser to induce a material in the vacuum chamber into a plasma state; And
A detector in communication with said vacuum chamber; , ≪ / RTI >
A graphene family dissolved in water and a water-soluble graphene family injected into the vacuum chamber are introduced into a plasma state, and the organic molecules in the plasma generated by the graphene family are completely dissociated, Element composition analyzer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20190121576A (en) | 2018-04-18 | 2019-10-28 | 한국세라믹기술원 | Analysis method of physical properties of graphene |
| KR20200116747A (en) | 2019-04-02 | 2020-10-13 | 한국세라믹기술원 | Analysis method of physical properties of graphene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014135455A1 (en) * | 2013-03-06 | 2014-09-12 | Directa Plus S.P.A. | Concentrated water dispersion of graphene and method for the preparation thereof |
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| WO2014135455A1 (en) * | 2013-03-06 | 2014-09-12 | Directa Plus S.P.A. | Concentrated water dispersion of graphene and method for the preparation thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190121576A (en) | 2018-04-18 | 2019-10-28 | 한국세라믹기술원 | Analysis method of physical properties of graphene |
| KR20200116747A (en) | 2019-04-02 | 2020-10-13 | 한국세라믹기술원 | Analysis method of physical properties of graphene |
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