CN102169102B - Method for monitoring and analyzing concentration of nano-carbon material electrophoretic deposition liquid - Google Patents
Method for monitoring and analyzing concentration of nano-carbon material electrophoretic deposition liquid Download PDFInfo
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- CN102169102B CN102169102B CN201110006821.2A CN201110006821A CN102169102B CN 102169102 B CN102169102 B CN 102169102B CN 201110006821 A CN201110006821 A CN 201110006821A CN 102169102 B CN102169102 B CN 102169102B
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Abstract
The invention relates to a method for monitoring and analyzing concentration of nano-carbon material electrophoretic deposition liquid. The method uses the conductivity method and the infrared spectrometry as analysis means, and realizes the real-time monitoring and quantitative analysis of the concentration changes of the ionophore and the nano-carbon material in the nano-carbon material electrophoretic deposition liquid by employing the change law of the conductivity of the nano-carbon material electrophoretic deposition liquid to the concentration of the ionophore and the change law of the absorbance of the nano-carbon material electrophoretic deposition liquid to the concentration of the nano-carbon material. The method for monitoring and analyzing concentration of nano-carbon material electrophoretic deposition liquid has the advantages of easy operation, high reliability, on-line monitoring, low cost and short time operation, and can be used to monitor and analyze the concentrations of the ionophore and the nano-carbon material of the nano-carbon material electrophoretic deposition liquid.
Description
Technical field
The invention belongs to nano-carbon material field, more specifically relate to a kind of nano-carbon material electrophoretic deposition liquid concentration monitor and analytical approach.
Background technology
Nano-carbon material is the class new material just progressively growing up at late 1980s, the beginning of the nineties.After this concept forms, cause common people's close attention, the peculiar property that it has, as unusual mechanics electrical properties, good chemical activity, the high characteristics such as physical strength, makes it at the electronics such as flat-panel monitor, light source, microwave amplifier, millimetric wave device and field of optoelectronic devices, have a wide range of applications.Nano-carbon material, as carbon nano-tube, Graphene, carbon nano-fiber and fullerene, due to its most advanced and sophisticated nano level radius-of-curvature and lower work function, is considered to the ideal material of field emission cold-cathode.At present, the preparation method of nano-carbon material field-transmitting cathode mainly contains direct growth method, silk screen print method and electrophoretic deposition etc.Direct growth method needs higher growth temperature (about 600～1000 ℃), has limited the application of the backing materials such as glass; The nano-carbon material of growing contains the impurity that is difficult for removal simultaneously, affects the field emission performance of nano-carbon material negative electrode.Method for printing screen has been avoided the problem of high growth temperature, but can introduce organic additive, affects to a certain extent the field emission performance of nano-carbon material, needs certain subsequent treatment could improve its field emission performance.Electrophoretic deposition technique is simple, with low cost, manufacturing cycle is short, thickness distribution is even, can realize the large-area even growth of nano-carbon material field-transmitting cathode under cryogenic conditions.
Generally, in the process of electrophoretic deposition nano-carbon material, there is a preferably concentration range in the ionophore in nano-carbon material electrophoretic deposition liquid and nano-carbon material, the ion that ionophore ionizes out in solution is attached on nano-carbon material powder, ion is subject to electric field action nano-carbon material is deposited on to electrode surface, forms one deck nano-carbon material film.But the prolongation along with electrophoresis time, ionophore concentration and the nano-carbon material concentration of nano-carbon material electrophoretic deposition liquid reduce gradually, cause the variation of operating voltage and working current in electrophoretic deposition process, prepared nano-carbon material film quality is declined.Therefore in order to improve the quality of nano-carbon material film prepared by electrophoretic deposition, be necessary to adjust electrophoretic deposition process parameter or change electrophoretic deposition liquid or supplement solute in good time, wherein the adjustment of electrophoretic deposition process parameter is by improving electrophoretic voltage or improving electrophoretic current or increase electrophoresis time and realize.But be that any method of adjustment all can have problems, as improved voltage or electric current or increasing electrophoresis time, can cause that the electrolysis of electrophoretic deposition liquid solvent or burning or prepared nano-carbon material uniformity of film are poor; As supplemented solute or change electrophoretic deposition liquid in good time, need a kind of mechanism that can judge nano-carbon material electrophoretic deposition liquid solute concentration.
On October 29th, 2003, disclosed Chinese invention patent application number was the method for a kind of semiquantitative characterization of carbon nanotube suspension stability of 03116185.5 explanation.This patent was drawn 10 times of upper strata stillness of night dilutions and is measured every 0.5 hour, but just because extension rate is too high, moment changes density between solution carbon nano-tube significantly, cause the acting force between carbon nano-tube in suspending liquid to alter a great deal, therefore to carbon nanotube dispersed in suspending liquid is exerted an influence.And on September 12nd, 2007, disclosed Chinese invention patent application number was 200610056306.6 characteristics that are directly proportional to the concentration of auxiliary salt in solution according to voltage in electrophoresis process or curent change, set up the regression function of electric current and time, prediction and adjustment electrophoretic liquid concentration.But due to its regretional analysis, analytic process is comparatively loaded down with trivial details, needs in addition first to learn the part by weight of carbon nano-tube and magnesium nitrate, therefore fail the concentration of carbon nano-tube and magnesium nitrate to carry out real-time estimate and adjustment.
Summary of the invention
In order to overcome above problem, the invention provides a kind of nano-carbon material electrophoretic deposition liquid concentration monitor and analytical approach.It is analysis means that the method be take electrical conductivity method and infra-red sepectrometry, the conductivity of utilizing nano-carbon material electrophoretic deposition liquid is the Changing Pattern with nano-carbon material concentration with the Changing Pattern of ionophore concentration and the absorbance of nano-carbon material electrophoretic deposition liquid, the concentration change of Real-Time Monitoring and quantitative test nano-carbon material electrophoretic deposition liquid intermediate ion carrier and nano-carbon material.
The present invention implements by following technical solution:
The monitoring of nano-carbon material electrophoretic deposition liquid concentration and an analytical approach, wherein monitor and analyze the concentration of two kinds of components in described electrophoretic deposition liquid, and described method is:
1) ionophore is joined in the solvent that is dissolved with nano-carbon material, measure the conductivity of nano-carbon material electrophoretic deposition liquid, make the typical curve equation of ionophore concentration to conductivity, according to the Conductivity Calculation of typical curve equation and electrophoretic deposition liquid to be measured, treat the ionophore concentration of test sample.
2) ionophore is joined in the solvent that is dissolved with nano-carbon material, adopt the absorbance of infrared spectrometry nano-carbon material electrophoretic deposition liquid, make the typical curve equation of nano-carbon material concentration to absorbance, according to the absorbance of typical curve equation and electrophoretic deposition liquid to be measured, calculate the nano-carbon material concentration for the treatment of test sample.
Described nano-carbon material is One-dimensional nanoreticular carbon materials.
Described nano-carbon material is any one or a few of carbon nano-tube, Graphene, carbon nano-fiber, fullerene, sodium rice porous carbon.
Described step 1) and step 2) in ionophore be any one or a few in magnesium nitrate, aluminium nitrate, indium nitrate, zinc nitrate, silver nitrate, lanthanum nitrate, magnesium chloride, aluminum chloride, inidum chloride.
Described step 1) and step 2) in the solvent that is dissolved with nano-carbon material, solvent is water or organic solvent.
Described organic solvent is any one or a few in ethanol, isopropyl alcohol, ethylene glycol, propyl alcohol, butanols.
The concentration of the typical curve equation intermediate ion carrier of described step 1) is 0～5g/L.
Described step 2) nano-carbon material concentration 0～0.35g/L in typical curve equation.
Described step 2) mid-infrared spectral characteristic absorption wave number is 1605 ~ 1630cm
-1.
The invention has the advantages that: the present invention have advantages of easy and simple to handle, reliability is high, on-line monitoring, cost is low, the time is brief, can Real-Time Monitoring and ionophore concentration and the nano-carbon material concentration of quantitative test nano-carbon material electrophoretic deposition liquid.
Accompanying drawing explanation
Fig. 1 is the test curve of embodiment of the present invention nano-carbon material electrophoretic deposition liquid electrical conductivity method, and wherein horizontal ordinate is ionophore concentration (g/L), and ordinate is conductivity (us/cm).
Fig. 2 is the test curve of embodiment of the present invention nano-carbon material electrophoretic deposition liquid infra-red sepectrometry, and wherein horizontal ordinate is nano-carbon material concentration (g/L), and ordinate is absorbance.
Embodiment
It is analysis means that electrical conductivity method and infra-red sepectrometry are take in the present invention, the conductivity of utilizing nano-carbon material electrophoretic deposition liquid is the Changing Pattern with nano-carbon material concentration with the Changing Pattern of ionophore concentration and the absorbance of nano-carbon material electrophoretic deposition liquid, the concentration change of quantitative test and Real-Time Monitoring nano-carbon material electrophoretic deposition liquid intermediate ion carrier and nano-carbon material, and then according to the concentration of its situation of change survey ionophore processed and nano-carbon material.
Described method is:
1) ionophore is joined in the solvent that is dissolved with nano-carbon material, measure the conductivity of nano-carbon material electrophoretic deposition liquid, make the typical curve equation of ionophore concentration to conductivity, according to the Conductivity Calculation of typical curve equation and electrophoretic deposition liquid to be measured, treat the ionophore concentration of test sample.
2) ionophore is joined in the solvent that is dissolved with nano-carbon material, adopt the absorbance of infrared spectrometry nano-carbon material electrophoretic deposition liquid, make the typical curve equation of nano-carbon material concentration to absorbance, according to the absorbance of typical curve equation and electrophoretic deposition liquid to be measured, calculate the nano-carbon material concentration for the treatment of test sample.
Described nano-carbon material is One-dimensional nanoreticular carbon materials.
Described nano-carbon material is any one or a few of carbon nano-tube, Graphene, carbon nano-fiber, fullerene, sodium rice porous carbon.
Described step 1) and step 2) in ionophore be any one or a few in magnesium nitrate, aluminium nitrate, indium nitrate, zinc nitrate, silver nitrate, lanthanum nitrate, magnesium chloride, aluminum chloride, inidum chloride.
Described step 1) and step 2) in the solvent that is dissolved with nano-carbon material, solvent is water or organic solvent.
Described organic solvent is any one or a few in ethanol, isopropyl alcohol, ethylene glycol, propyl alcohol, butanols.
The concentration of the typical curve equation intermediate ion carrier of described step 1) is 0～5g/L.
Described step 2) nano-carbon material concentration 0～0.35g/L in typical curve equation.
Described step 2) mid-infrared spectral characteristic absorption wave number is 1605 ~ 1630cm
-1.
According to step 1), 2) in the concentration difference of the best electrophoretic deposition liquid intermediate ion carrier that obtains in resulting electrophoretic deposition liquid to be measured and specific operation process and the concentration difference of nano-carbon material, give corresponding magnitude of recruitment or change electrophoretic deposition liquid, the object that realizes monitoring and analyze.
Embodiment 1
The first, described electrical conductivity method is analyzed the relation of its corresponding conductivity of ionophore concentration of nano-carbon material electrophoretic deposition liquid; Ionophore magnesium nitrate concentration range in described electrical conductivity method is 0～5g/L, and preferred, the ionophore magnesium nitrate concentration range in the present embodiment electrical conductivity method is 0.025～2.5g/L.
Refer to Fig. 1, in the present embodiment electrical conductivity method, the carbon nano-tube electrophoretic deposit fluid that quantitative magnesium nitrate is added to certain carbon nano-tube concentration, ultrasonic dispersion, use again the conductivity value of carbon nano-tube electrophoretic deposit fluid under conductivity meter measuring chamber temperature, repeat afterwards above work until the magnesium nitrate concentration of carbon nano-tube electrophoretic deposit fluid is 2.5g/L, wherein carbon nano-tube electrophoretic deposit fluid carbon nano-tube concentration remains unchanged, thereby determines the corresponding conductivity value of carbon nano-tube electrophoretic deposit fluid different ions carrier magnesium nitrate concentration.Its corresponding conductivity value of ionophore magnesium nitrate concentration of carbon nano-tube electrophoretic deposit fluid is carried out to matching.Ask for an interview Fig. 1, the carbon nano-tube electrophoretic deposit fluid of ionophore concentration and the test curve equation of its respective electrical conductance are formula 1:
Wherein
be magnesium nitrate concentration in solution, unit is
;
be electrical conductivity of solution, unit is
,
with
for fitting parameter.
The second, described infra-red sepectrometry is analyzed the relation of its corresponding absorptivity of nano-carbon material concentration of nano-carbon material electrophoretic deposition liquid.Nano-carbon material carbon nano-tube concentration range in described infra-red sepectrometry is 0～0.35 g/L.The mensuration characteristic absorption wave number of described infra-red sepectrometry nano-carbon material carbon nano-tube concentration is 1605 ~ 1630cm
-1, exact value is determined according to instrument situation and nano material kind.Preferentially, the mensuration characteristic absorption wave number of the present embodiment infra-red sepectrometry nano-carbon material carbon nano-tube concentration is 1630cm
-1.
Refer to Fig. 2, the specific implementation process of the present embodiment infra-red sepectrometry is that carbon nano-tube and magnesium nitrate are added in isopropanol solvent, ultrasonic dispersion is prepared into the carbon nano-tube electrophoretic deposit fluid that a series of carbon nano-tube concentration is 0.03～0.35g/L, and wherein electrophoretic deposition liquid magnesium nitrate concentration keeps the same.The present embodiment infra-red sepectrometry be take isopropyl alcohol as reference, and the carbon nano-tube electrophoretic deposit fluid that is 0.03～0.35g/L to carbon nano-tube concentration carries out infrared absorption spectrum analysis.Its corresponding carbon nano-tube concentration of resulting carbon nano-tube electrophoretic deposit fluid absorbance is carried out to matching, thus the calibration curve of the carbon nano-tube electrophoretic deposit fluid absorbance corresponding with it of the carbon nano-tube concentration that settles the standard.The test curve equation of the carbon nano-tube electrophoretic deposit fluid absorbance corresponding with it of carbon nano-tube concentration is formula 2:
Wherein
be carbon nano-tube concentration in solution, unit is
;
solution absorbance,
with
it is fitting parameter.
The 3rd, described electrical conductivity method and infra-red sepectrometry respectively according to the variation relation of its corresponding conductivity of ionophore magnesium nitrate concentration, the variation relation of its corresponding absorbance of nano-carbon material carbon nano-tube concentration is surveyed magnesium nitrate concentration processed, carbon nano-tube concentration in real time.It is all that the carbon nano-tube electrophoretic deposit fluid of definite value is standard electrophoretic deposition liquid that the present embodiment is established magnesium nitrate concentration and carbon nano-tube concentration, and the carbon nano-tube electrophoretic deposit fluid of establishing under this ionophore concentration and carbon nano-tube concentration is the best ionophore concentration of carbon nano-tube film depositing and the carbon nano-tube electrophoretic deposit fluid of carbon nano-tube concentration.According to difference between the magnesium nitrate of the formula 1 of the present embodiment, formula 2 calculating electrophoretic deposition liquids to be measured and standard electrophoretic deposition liquid and carbon nano-tube concentration, supplementary magnesium nitrate and carbon nano-tube or replacing electrophoretic deposition liquid make its electrophoretic deposition liquid solute concentration that is near the mark again and in time, are more conducive to electrophoretic deposition work next time.
Embodiment 2
Described nano-carbon material is carbon nano-fiber.
Described step 1) and step 2) in ionophore be magnesium nitrate and aluminium nitrate.
Described step 1) and step 2) in the solvent that is dissolved with nano-carbon material, solvent is water.
The concentration of the typical curve equation intermediate ion carrier of described step 1) is 0～5g/L.
Described step 2) nano-carbon material concentration 0～0.35g/L in typical curve equation.
Described step 2) mid-infrared spectral characteristic absorption wave number is 1605cm
-1.
Not mentioned part is identical with specific embodiment 1 above.
Embodiment 3
Described nano-carbon material is Graphene and fullerene.
Described step 1) and step 2) in ionophore be aluminum chloride.
Described step 1) and step 2) in the solvent that is dissolved with nano-carbon material, described organic solvent is ethylene glycol and butanols.
The concentration of the typical curve equation intermediate ion carrier of described step 1) is 0～5g/L.
Described step 2) nano-carbon material concentration 0～0.35g/L in typical curve equation.
Described step 2) mid-infrared spectral characteristic absorption wave number is 1620cm
-1.
Not mentioned part is identical with specific embodiment 1 above.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. the monitoring of nano-carbon material electrophoretic deposition liquid concentration and an analytical approach, wherein monitor and analyze the concentration of two kinds of components in described electrophoretic deposition liquid, it is characterized in that: described method is:
1) ionophore is joined in the solvent that is dissolved with nano-carbon material, measure the conductivity of nano-carbon material electrophoretic deposition liquid, make the typical curve equation of ionophore concentration to conductivity, according to the Conductivity Calculation of typical curve equation and electrophoretic deposition liquid to be measured, treat the ionophore concentration of test sample;
2) ionophore is joined in the solvent that is dissolved with nano-carbon material, adopt the absorbance of infrared spectrometry nano-carbon material electrophoretic deposition liquid, make the typical curve equation of nano-carbon material concentration to absorbance, according to the absorbance of typical curve equation and electrophoretic deposition liquid to be measured, calculate the nano-carbon material concentration for the treatment of test sample;
Described nano-carbon material is One-dimensional nanoreticular carbon materials;
Described nano-carbon material is any one or a few of carbon nano-tube, Graphene, carbon nano-fiber, fullerene, nanoporous carbon;
Described step 1) and step 2) in ionophore be any one or a few in magnesium nitrate, aluminium nitrate, indium nitrate, zinc nitrate, silver nitrate, lanthanum nitrate, magnesium chloride, aluminum chloride, inidum chloride;
Described step 1) and step 2) in the solvent that is dissolved with nano-carbon material, solvent is water or organic solvent;
Described organic solvent is any one or a few in ethanol, isopropyl alcohol, ethylene glycol, propyl alcohol, butanols;
The concentration of typical curve equation intermediate ion carrier described step 1) is 0～5g/L;
Described step 2) nano-carbon material concentration 0～0.35g/L in typical curve equation;
Described step 2) mid-infrared spectral characteristic absorption wave number is 1605～1630cm
-1.
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| CN102944528A (en) * | 2012-11-14 | 2013-02-27 | 上海交通大学 | Method for measuring concentration of C60 nanocrystal particles in water medium |
| CN103149249A (en) * | 2013-03-01 | 2013-06-12 | 青岛大学 | Method for quickly detecting graphene in solution |
| CN103434207A (en) * | 2013-08-19 | 2013-12-11 | 南京航空航天大学 | Foam metal-carbon nanotube composite material and preparation method thereof |
| CN104589459B (en) * | 2015-01-05 | 2017-02-01 | 中国东方电气集团有限公司 | Weight control method for electrophoretic deposition ceramic green body |
| DE102015223789A1 (en) * | 2015-10-07 | 2017-04-13 | Sms Group Gmbh | Online analysis by means of near-infrared spectroscopy analysis NIR, in particular for the production of polyaluminum chloride hydroxide |
| CN109265817A (en) * | 2018-07-12 | 2019-01-25 | 凌云工业股份有限公司上海凌云汽车研发分公司 | The preparation method of carbon nanotube enhancing thermoplastic carbon fiber polymer matrix composites |
| 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 |
| US11340205B2 (en) | 2019-01-24 | 2022-05-24 | Hong Kong Applied Science And Technology Research Institute Co., Ltd. | Systems and methods for determining concentrations of materials in solutions |
| CN109923415B (en) * | 2019-01-24 | 2021-06-22 | 香港应用科技研究院有限公司 | System and method for determining concentration of substance in solution |
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| CN1196924C (en) * | 2003-04-04 | 2005-04-13 | 中国科学院上海硅酸盐研究所 | Method for semiquantitative characterization of carbon nanotube suspension stability |
| CN101034079A (en) * | 2006-03-08 | 2007-09-12 | 东元电机股份有限公司 | Judgement and control method for carbon nano-tube electrophoretic liquid concentration |
| CN101567309A (en) * | 2008-04-22 | 2009-10-28 | 株式会社平间理化研究所 | Device for blending etching solution and device for determinating concetration of etching solution |
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| US7252749B2 (en) * | 2001-11-30 | 2007-08-07 | The University Of North Carolina At Chapel Hill | Deposition method for nanostructure materials |
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| CN1196924C (en) * | 2003-04-04 | 2005-04-13 | 中国科学院上海硅酸盐研究所 | Method for semiquantitative characterization of carbon nanotube suspension stability |
| CN101034079A (en) * | 2006-03-08 | 2007-09-12 | 东元电机股份有限公司 | Judgement and control method for carbon nano-tube electrophoretic liquid concentration |
| CN101567309A (en) * | 2008-04-22 | 2009-10-28 | 株式会社平间理化研究所 | Device for blending etching solution and device for determinating concetration of etching solution |
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