CN102169102A - 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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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 the 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 a class new material that just progressively grows up at late 1980s, the beginning of the nineties.After this notion forms, cause common people's close attention, peculiar property that it had such as unusual mechanics electrical properties, good chemical activity, high characteristics such as physical strength make it have a wide range of applications at electronics such as flat-panel monitor, light source, microwave amplifier, millimetric wave device and field of optoelectronic devices.Nano-carbon material such as carbon nano-tube, Graphene, carbon nano-fiber and fullerene owing to its most advanced and sophisticated nano level radius-of-curvature and lower work function, are 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.The direct growth method needs higher growth temperature (about 600～1000 ℃), has limited the application of backing materials such as glass; The nano-carbon material of being grown simultaneously contains the impurity that is difficult for removal, influences 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, influences the field emission performance of nano-carbon material to a certain extent, needs certain subsequent treatment could improve its field emission performance.Electrophoretic deposition technology 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 the cryogenic conditions.
Generally, in the process of electrophoretic deposition nano-carbon material, there are a preferable concentration range in ionophore in the nano-carbon material electrophoretic deposition liquid and nano-carbon material, the ionophore ion that ionization goes out in solution is attached on the nano-carbon material powder, ion is subjected to electric field action nano-carbon material is deposited on electrode surface, forms one deck nano-carbon material film.But prolongation along with electrophoresis time, the 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 the electrophoretic deposition process, make prepared nano-carbon material film quality descend.Therefore for the quality of the nano-carbon material film that improves the electrophoretic deposition preparation, be necessary to adjust the electrophoretic deposition process parameter or change electrophoretic deposition liquid or additional in good time solute, 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,, can cause that electrolysis of electrophoretic deposition liquid solvent or burning or prepared nano-carbon material uniformity of film are relatively poor as improving voltage or electric current or increasing electrophoresis time; As replenish 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 that a kind of sxemiquantitative of 03116185.5 explanation characterizes carbon nano tube suspension stability.This patent was drawn the dilution of the upper strata stillness of night and is measured for 10 times again every 0.5 hour, but just because extension rate is too high, moment changes density between the solution carbon nano-tube significantly, cause that the acting force between the carbon nano-tube alters a great deal in the suspending liquid, therefore to carbon nano-tube dispersiveness in the suspending liquid is exerted an influence.And on September 12nd, 2007 disclosed Chinese invention patent application number be 200610056306.6 according to voltage in the electrophoresis process or electric current change with solution in assist the concentration of salt to be directly proportional characteristic, set up the regression function of electric current and time, prediction and adjustment electrophoretic liquid concentration.But because its regretional analysis, analytic process is comparatively loaded down with trivial details, need learn the part by weight of carbon nano-tube and magnesium nitrate in addition earlier, therefore fails the concentration of carbon nano-tube and magnesium nitrate is carried 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.This method is an analysis means with electrical conductivity method and infra-red sepectrometry, the conductivity of utilizing the nano-carbon material electrophoretic deposition liquid is with the absorbance of the Changing Pattern of ionophore concentration and the nano-carbon material electrophoretic deposition liquid Changing Pattern with nano-carbon material concentration, the concentration change of monitoring and quantitative test nano-carbon material electrophoretic deposition liquid intermediate ion carrier and nano-carbon material in real time.
The present invention implements by following technical solution:
A kind of nano-carbon material electrophoretic deposition liquid concentration monitoring and analytical approach are wherein monitored and are analyzed two kinds of component concentrations in the 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, treat the ionophore concentration of test sample according to the Conductivity Calculation of typical curve equation and electrophoretic deposition liquid to be measured conductivity.
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, calculate the nano-carbon material concentration for the treatment of test sample according to the absorbance of typical curve equation and electrophoretic deposition liquid to be measured to absorbance.
Described nano-carbon material is the 1-dimention nano material with carbon element.
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 in magnesium nitrate, aluminium nitrate, indium nitrate, zinc nitrate, silver nitrate, lanthanum nitrate, magnesium chloride, aluminum chloride, the inidum chloride any one or a few.
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, the 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 the 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 easy and simple to handle, reliability is high, on-line monitoring, cost is low, the time is brief advantage, can monitor ionophore concentration and nano-carbon material concentration with quantitative test nano-carbon material electrophoretic deposition liquid in real time.
Description of drawings
Fig. 1 is the test curve of embodiment of the 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 invention nano-carbon material electrophoretic deposition liquid infra-red sepectrometry, and wherein horizontal ordinate is nano-carbon material concentration (g/L), and ordinate is an absorbance.
Embodiment
The present invention is an analysis means with electrical conductivity method and infra-red sepectrometry, the conductivity of utilizing the nano-carbon material electrophoretic deposition liquid is with the absorbance of the Changing Pattern of ionophore concentration and the nano-carbon material electrophoretic deposition liquid Changing Pattern with nano-carbon material concentration, the quantitative test and the real-time concentration change of monitoring nano-carbon material electrophoretic deposition liquid intermediate ion carrier and nano-carbon material, and then survey the concentration of system ionophore and nano-carbon material according to its situation of change.
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, treat the ionophore concentration of test sample according to the Conductivity Calculation of typical curve equation and electrophoretic deposition liquid to be measured conductivity.
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, calculate the nano-carbon material concentration for the treatment of test sample according to the absorbance of typical curve equation and electrophoretic deposition liquid to be measured to absorbance.
Described nano-carbon material is the 1-dimention nano material with carbon element.
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 in magnesium nitrate, aluminium nitrate, indium nitrate, zinc nitrate, silver nitrate, lanthanum nitrate, magnesium chloride, aluminum chloride, the inidum chloride any one or a few.
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, the 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 the 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 the specific operation process and the concentration difference of nano-carbon material, give corresponding magnitude of recruitment or change electrophoretic deposition liquid, realize monitoring and the purpose of analyzing.
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 the 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.
See also Fig. 1, in the present embodiment electrical conductivity method, the carbon nano-tube electrophoretic deposit fluid that quantitative magnesium nitrate is added certain carbon nano-tube concentration, ultrasonic dispersion, measure the conductivity value of carbon nano-tube electrophoretic deposit fluid under the room temperature again with conductivity meter, repeating above work afterwards is 2.5g/L up to the magnesium nitrate concentration of carbon nano-tube electrophoretic deposit fluid, wherein carbon nano-tube electrophoretic deposit fluid carbon nano-tube concentration remains unchanged, thereby determines the pairing 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 match.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 the solution, unit is;
Be electrical conductivity of solution, unit is,
With
Be 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 the 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 decided according to instrument situation and nano material kind.Preferentially, the mensuration characteristic absorption wave number of present embodiment infra-red sepectrometry nano-carbon material carbon nano-tube concentration is 1630cm
-1
See also Fig. 2, the specific implementation process of present embodiment infra-red sepectrometry is that carbon nano-tube and magnesium nitrate are added in the isopropanol solvent, the carbon nano-tube electrophoretic deposit fluid that it is 0.03～0.35g/L that ultrasonic dispersion is prepared into a series of carbon nano-tube concentration, wherein electrophoretic deposition liquid magnesium nitrate concentration keeps the same.The present embodiment infra-red sepectrometry is reference with the isopropyl alcohol, is that the carbon nano-tube electrophoretic deposit fluid of 0.03～0.35g/L carries out infrared absorption spectrum analysis to carbon nano-tube concentration.Its corresponding carbon nano-tube concentration of resulting carbon nano-tube electrophoretic deposit fluid absorbance is carried out match, thus the calibration curve of the carbon nano-tube electrophoretic deposit fluid absorbance corresponding of the carbon nano-tube concentration that settles the standard with it.The test curve equation of the carbon nano-tube electrophoretic deposit fluid absorbance corresponding with it of carbon nano-tube concentration is a formula 2:
Wherein
Be carbon nano-tube concentration in the solution, unit is;
Be solution absorbance,
With
It is fitting parameter.
The 3rd, described electrical conductivity method and infra-red sepectrometry are surveyed system magnesium nitrate concentration, carbon nano-tube concentration in real time 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 respectively.It all is that the carbon nano-tube electrophoretic deposit fluid of definite value is the standard electrophoretic deposition liquid that 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 the carbon nano-tube concentration is the ionophore concentration of best carbon nano-tube film depositing and the carbon nano-tube electrophoretic deposit fluid of carbon nano-tube concentration.Calculate difference between the magnesium nitrate of electrophoretic deposition liquids to be measured and standard electrophoretic deposition liquid and the carbon nano-tube concentration according to the formula 1 of present embodiment, formula 2, additional again and in time magnesium nitrate and carbon nano-tube or replacing electrophoretic deposition liquid make its electrophoretic deposition liquid solute concentration that is near the mark, and more help electrophoretic deposition work next time.
Described nano-carbon material is a 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 a 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 the typical curve equation.
Described step 2) mid-infrared spectral characteristic absorption wave number is 1605cm
-1
More than not mentioned part identical with specific embodiment 1.
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 the typical curve equation.
Described step 2) mid-infrared spectral characteristic absorption wave number is 1620cm
-1
More than not mentioned part identical with specific embodiment 1.
The above only is preferred embodiment of the present invention, and all equalizations of being done according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (9)
1. nano-carbon material electrophoretic deposition liquid concentration monitoring and analytical approach are wherein monitored and are analyzed two kinds of component concentrations in the described electrophoretic deposition liquid, and 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, treat the ionophore concentration of test sample according to the Conductivity Calculation of typical curve equation and electrophoretic deposition liquid to be measured conductivity;
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, calculate the nano-carbon material concentration for the treatment of test sample according to the absorbance of typical curve equation and electrophoretic deposition liquid to be measured to absorbance.
2. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and analytical approach is characterized in that: described nano-carbon material is the 1-dimention nano material with carbon element.
3. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and 2 and analytical approach is characterized in that: described nano-carbon material is any one or a few of carbon nano-tube, Graphene, carbon nano-fiber, fullerene, sodium rice porous carbon.
4. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and analytical approach is characterized in that: described step 1) and step 2) in ionophore be in magnesium nitrate, aluminium nitrate, indium nitrate, zinc nitrate, silver nitrate, lanthanum nitrate, magnesium chloride, aluminum chloride, the inidum chloride any one or a few.
5. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and analytical approach is characterized in that: described step 1) and step 2) in the solvent that is dissolved with nano-carbon material, solvent is water or organic solvent.
6. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 5 and analytical approach is characterized in that: described organic solvent is any one or a few in ethanol, isopropyl alcohol, ethylene glycol, propyl alcohol, the butanols.
7. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and analytical approach is characterized in that: the concentration of the typical curve equation intermediate ion carrier of described step 1) is 0～5g/L.
8. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and analytical approach is characterized in that: nano-carbon material concentration 0～0.35g/L in the typical curve equation described step 2).
9. a kind of nano-carbon material electrophoretic deposition liquid concentration monitoring according to claim 1 and analytical approach is characterized in that: described step 2) mid-infrared spectral characteristic absorption wave number is 1605～1630cm
-1
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| 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 |
| CN104589459A (en) * | 2015-01-05 | 2015-05-06 | 中国东方电气集团有限公司 | Weight control method for electrophoretic deposition ceramic green body |
| CN108137340A (en) * | 2015-10-07 | 2018-06-08 | Sms集团有限公司 | Particularly it is used to prepare the on-line analysis by means of near-infrared spectrum analysis NIR of polyaluminium chloride hydroxide |
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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 |
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