Nano-modified electrolyte correction method

FIELD: electrical engineering.

SUBSTANCE: method for correction of carbon nano-tubes (CNTs) concentration in an electrolyte for electrochemical sedimentation of metals involves measurement of the temperature of electrolyte in the plating bath, measurement of CNTs concentration and recovery of CNTs concentration in the electrolyte. Measurement of CNTs concentration in the electrolyte is performed by way of passing the electrolyte through the photometer optical system; relying on the photometer readings, the initial CNTs concentration is recovered by way of dosaged delivery of CNTs into the electrolyte that is subsequently passed through the disperser and returned to the plating bath.

EFFECT: measurement of CNTs concentration and recovery of initial CNTs concentration in the electrolyte in the process of plated coating application.

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The invention relates to electroplating and can be used in electrochemical and chemical treatment of metals using chemical methods.

Technologies for nanomodified electroplating allowed to get Nickel and chromium coatings with improved properties (high hardness, wear resistance, less uneven than traditional coatings) [1, 2]. The core of the process is the addition of electrolytes fullerenedoped carbon nanotubes (CNTS) - nanocarbon material registered under the trade mark "Taunit", produced by LLC "Nanocenter", Tambov. "Taunit" represents a carbon nanoscale filamentary formations predominantly cylindrical shape with an internal channel. The number of graphene layers not more than 30, the diametrical size of from 10 to 60 nm and a length not less than 2 μm. The number of structured carbon material "Taunit" not less than 95% [3]. Low concentrations of carbon nanotubes "Taunit in the electrolyte substantially change as the properties of the electrolyte, and properties of the coatings. One of the most important tasks in the organization galvanic processes is the measurement of the concentration of CNTS in the electrolyte and, consequently, its stabilization. CNT "Taunit" is a new material and at the present time what I'm missing sensors and methods of measurement of its concentration in the electrolyte. Based on the opacity of polycrystalline graphite, the inventors propose to measure the concentration of carbon nanotubes by optical methods.

When electroplating the concentration of carbon nanotubes "Taunit" decreases due to the fact that "Taunit" hits the floor. Periodically measuring the concentration of CNTS using device KLF-3.

When the concentration of CNTS lower threshold values produce dosing the right amount of CNTS using dispenser[1, 2, 3].

There is a method of regenerating exhausted chromate solutions for chromate zinc and cadmium, comprising adjusting the pH of the solution in the range of 5-9, the introduction of the flocculating agent is polyacrylamide, decanting the solution from the precipitate, the acidification of the solution with sulfuric acid to working pH and the addition of chromate salt solution to adjust the solution of the bichromate of sodium [4].

However, this method is not applicable in the electroplating processes in which the process is not directly connected with the power consumption and the temperature of the electrolyte, and changes the concentration of the nanomaterial used in electroplating.

Also known method [5] adjustment of the composition of the electrolyte upon receipt of zirconium, including monitoring the amount of electricity and electrolyte composition, calculation Velich is to download the source salts porcelanato and potassium chloride, and load them into the machine - electrolysis, in which before loading measure the temperature of the electrolyte, and the calculation load of the original salts are the formulas:

PK2ZrF6=AZrQ-BZr(CZr-C Zr)+DZr(T-T');

PKCl=AClQ-BCl(CCl-C Cl)+DCl(T-T'),

where PK2ZrF6, PCl - a number of salts of porcelanato and potassium chloride, which is loaded in the current period, kg;

Q - the amount of electricity over the past period, kA·h;

CZr, CCl - content of zirconium and chlorine in the electrolyte in the last period, wt.%;

T - the result of measuring the temperature of the electrolyte before downloading °C;

C Zr, C Cl - specified values of the content of zirconium and chlorine in the electrolyte, wt.%;

T - the set-point temperature of the electrolyte °C;

AZr, BZr, DZr, ACl, BCl, DCl - defined coefficients AZr=1,6-2,0, BZr=2-40, DZr=1,4-3,7, ACl=1,3-3,1; BCl=10-30, DCl=0.8 to 2.6.

However, this method allows to increase the output of zirconium current by increasing the accuracy of the composition of the electrolyte, but is not applicable in galvanic processes, such as electroplating, in which the consumption of reagents is not directly associated with the power consumption and the temperature of the electrolyte.

Adopted as the prototype of the method of automatic adjustment of the electrolyte in the electroplating baths of the line [6], which includes information input by the operator on the initial concentration of the components of the electrolyte, the current measurement in the tub and number of suspensions with what seliami, passed through the bath, the calculation based on the obtained information of the current component concentration of the electrolyte, the comparison of the current concentration with predetermined acceptable values, correction of electrolyte if the current value of the concentration is less than acceptable, provide measurements of the space of products of each suspension, the multiplication values of the area on specific ablation of the electrolyte and the conversion current value of the component concentration of the electrolyte.

This method allows to carry out the adjustment of the solution, which ensures the production of high quality coatings. However, this method cannot be used in the electroplating process, in which the consumption of reagents is not directly associated with the power consumption and the temperature of the electrolyte.

The problem solved by the invention is the development of technologies for the measurement of the concentration of the CNTS and the restoration of the initial concentration of the CNTS in the electrolyte during electroplating coating.

The task is implemented because, according to the method of correction of electrolyte composition, including the control of the electrolyte composition, the calculation load of the component and loading it in electroplating apparatus, in which before loading measure the temperature of the electrolyte, the adjustment of the concentration of the CNTS in the electroplating bath is carried out by passing the electrolyte through the optical system of the photometer, according to the indications which include dosing CNTS in the electrolyte, which is then passed through the disperser and return in the galvanic bath.

The content of CNTS in the electroplating solution is determined at the working temperature of the solution depending on its optical density and the magnitude of the transmission coefficient.

To adjust the concentration of the CNTS in the electroplating bath by passing the electrolyte through the optical system of the photometer according to the indications which include dosing CNTS in the electrolyte, which is then passed through the disperser and return in the galvanic bath, provides the performance comparison of current concentration with predetermined acceptable values, adjusting the concentration of the electrolyte if the current value of the concentration is below limit, and maintaining the concentration of CNTS within the specified limits, which ensures the production of high quality coatings.

The determination of the content of CNTS in the electroplating solution at the operating temperature of the solution depending on its optical density at the magnitude of the transmission coefficient of the electrolyte provides the necessary accuracy of measurement of the concentration of the CNT with respect to temperature of the solution affects the optical properties of the electrolyte and in the presence in the solution brightening agent EXT is the SAI.

Studies were conducted using a photometer KLF-3. Analyzed the optical properties of the following electrolytes: standard electrolyte plating, bestiality electrolyte silvering 07-CR (SPE "ECOMET"), the alkaline electrolyte of the zinc with the addition of Zn-1 (LLC Galvanic technology"), a Nickel plating electrolyte watts with the addition of Likonda Ni-A and Likonda Ni-B (LLC Galvanic technology"). All electrolytes are not only color, but also by the concentration of various substances, including brightening agent and additives. Substances included in the composition of the electrolyte, and a brightening agent additives absorb light differently. Obviously, clean, lapped electrolytes have an optical density, non-operated contaminated metal oxides. Adding to the electrolyte opaque materials further increases the optical density. In turn, the optical density depends on the wavelength of light. Therefore, for proper research necessary to determine the operating wavelength of each of the electrolyte.

Before electroplating coating in the electrolyte is injected CNT "Taunit". The resulting electrolyte is a colloidal solution of multilayer carbon nanotubes. A known method of determining the content of colloidal particles in aqueous solutions, based on measured and transmittance of transparent liquid solutions and determining the concentration of a substance at a pre-constructed calibration curve. In the proposed method this method is based, but its use is complicated by the optical properties of the electrolyte and the presence of the brightening agent additives.

Dosing the initial amount of carbon nanotubes "Taunit in the electrolyte is carried out, for example, using the QUANTOS dosing. CNT "Taunit" may be in powder form or in the form of effervescent tablets. With the introduction of CNTS in the form of a powder, the powder is subjected to dispersion, for example, using a flow-through ultrasonic disperser IL 100-6/9. To do this, arrange the circulation loop, in which the electrolyte is pumped from the bath via a flow disperser and return to the bath. This path for a number of processes already exist, for example, Nickel plating, where you need continuous filtration of the electrolyte. In this case, the existing circuit inserts a flow disperser.

The invention is illustrated by the following examples.

Example 1. The electrolyte galvanizing

Prepared a set of samples of pure electrolyte having a working temperature of 20°C. Held optical measurement from the beginning of the range of the instrument (350 nm) with a step of 50 nm (table 1).

Table 1
The dependence of the optical density E of the electrolyte zinkovani is of wavelength λ
λ, nm350400450500550600650700750800
E, B0,7030,2720,0800,0580,0420,0270,0180,0120,0040,000

The table shows that the maximum value of F occurs at λ=350 nm. Setting a wavelength of 350 nm, made measurements for different samples of electrolytes. In the experiments varied the concentration of CCNTnanoglide "Taunit" in electrolytes and measured the optical density E and the transmission coefficient P. the Results are presented in table 2.

Table 2
Experimental data for electrolyte galvanizing
The electrolyteWithCNT mg/lE, BP %
123AVG.123AVG.
Net00,0040,0040,0010,00398,6of 99.199,299,0
With the addition of CNTS500,2640,2640,261to 0.26354,7of 54.855,154,9
With the addition of CNTS700,3820,3750,3750,37742,642,642,842,7
With the addition of the HT 1000,6000,5850,5690,58527,628,128,027,9

According to table 2 are the graphs of dependences of optical density E and transmittance of PCNT(Fig 1 and 2), where figure 1 shows the dependence of the optical density of the electrolyte, the zinc concentration of the CNTS;

figure 2 - dependence of the transmission coefficient of the electrolyte, the zinc concentration of the CNTS.

From the graphs clearly shows that the dependence is close to linear, so they were fitted by a polynomial of the first order.

Found approximate expression:

E=0,SCNT- 0,009,

R2=0,994,

P=-0,SCNT+95,76,

R2=0,979,

where R is the coefficient of determination is calculated by the formula:

where- full sum of the squares of the differences between the mean values ofexperimental data yi;

- the residual sum of squares, which characterizes the deviation of the experimental data yifrom theoretical.

Note that when R2 =1, the full correlation of the model with experimental data.

Example 2. Electrolytes Nickel plating

In the process of working with electrolytes Nickel plating, there was a significant effect of electrolyte temperature on the optical density due to the potential for crystallization of salts of Nickel at lower temperature (table 3)

Significant differences of the optical density at different temperatures of the electrolyte leads to the conclusion that it is advisable to measure optical density or transmittance in solutions having a working temperature. Under the working temperature is understood to be the temperature range of the electrolyte recommended to obtain high-quality electroplating. The optimum temperature galvanic Nickel plating in accordance with the technology is 52°C. Maintaining the specified temperature value, we performed further measurements to determine the working wavelength. The example graph shown in figure 3.

The method of selection of the operating wavelength (maximum value), it follows that the measurement should be carried out at λ=700 nm. However, it was observed volatility readings in almost all measurements. Values for the same samples differed by 10-20%. Exploring the sample at wavelength λ=400 nm (the second peak in figure 3), also p who were given erratic readings. Performing measurements over the entire range of experimentally found that stable readings are obtained at a wavelength of λ=800 nm. Obviously there are some factors that do not allow to apply the standard method for determining the working wavelengths. Perhaps this is due to the color of the electrolyte or its chemical composition. Figure 3. shows the definition of the working wavelength of the electrolyte plating with brightening agent additive Likonda Ni-A.

Setting a wavelength of 800 nm, made measurements for different samples of electrolytes and obtained the following data (table 4).

Table 4
Experimental data for Nickel plating electrolyte with brightening agent additive Likonda Ni-A
The electrolyteWithCNT,
mg/l
E, BP %
123AVG.123AVG.
Net0 strength of 0.1590,1630,1600,16170,170,370,1to 70.2
With the addition of CNTS500,3590,3610,3600,36044,244,144,744,3
With the addition of CNTS700,5720,5690,5700,57026,826,727,026,8
With the addition of CNTS1000,7050,6950,6980,69919,620,420,320,1

The graphs of dependences of absorbance and transmittance of the electrolyte plating with brightening agent additive Likonda Ni-A con is entrale CNTS shown in Figure 4 and 5.

The correct wavelength is indirectly confirmed by the appearance of the graphs. Figure 4. the dependence of optical density of the electrolyte plating with brightening agent additive Likonda Ni-A concentration of CNTS. Figure 5 - dependence of the transmission coefficient of the electrolyte plating with brightening agent additive Likonda Ni-A concentration of CNTS.

The electrolyte plating also has multiextremal function of optical density and requires experimental choice of operating wavelength.

Below are the results of research.

The silver plating electrolyte: a solution temperature of 20°C, λ=350 nm.

The function of optical density:

E=0,SCNT+0,078,

R2=0,996

and transmittance:

P=-0,SCNT+81,44,

R2=0,952.

The Nickel plating electrolyte with additive Likonda Ni-A: the solution temperature 52°C, λ=800 nm.

Simplified function of optical density:

E=0,SCNT+0,142

and transmittance:

P=-0,523CNT+69,14

The magnitude of the accuracy of the approximation R2in the first case 0,967, in the second 0,969.

Functions obtained using TableCurve 2D are of the form:

when R2=0,982,

when R2=0,999.

The Nickel plating electrolyte with additive Likonda Ni-B: the solution temperature 52°C, λ=600 nm.

Aproxen the e function of optical density:

E=0,SCNT+0,119

and transmittance:

P=-0,SCNT+70,25

The magnitude of the accuracy of the approximation R2in the first case 0,957, in the second 0,941.

Functions obtained using TableCurve 2D are of the form:

when R2=0,990,

when R2=0,999.

The electrolyte plating: temperature of the solution 52°C, λ=600 nm.

Simplified function of optical density:

E=0,SCNT+0,532

and transmittance:

P=-0,SCNT+27,95

The magnitude of the accuracy of the approximation R2in the first case 0,949, in the second 0,973.

Functions obtained using TableCurve 2D are of the form:

when R2=0,996,

when R2=0,999.

The electrolyte of the zinc with the addition of Zn-1: the solution temperature of 20°C, λ=350 nm.

Simplified function of optical density:

E=0,SCNT+0,009

and transmittance:

P=-0,SCNT+95,76

The magnitude of the accuracy of the approximation R2in the first case 0,994, in the second 0,979.

Functions obtained using TableCurve 2D are of the form:

when R2=0,999,

when R2=0,999.

Thus electrolytes for electrochemical deposition of metals distributed in them CNTS is Taunit" can be considered a highly dispersed colloidal systems with a liquid dispersion medium. The concentration of the CNTS and the temperature of the electrolyte affects the optical properties of electrolytes.

Experimental determination of the working wavelength perform on the basis of the stability of the readings, because not all electrolytes suitable standard method of determining the operating wavelength.

Mathematical models E(SWNT) and P(SWNT) take into account the degree of exploitation of the electrolyte, its operating temperature and resistance readings at the working wavelength.

These models can be applied, for example, regulators concentrations of CNTS, galvanic bath - optical system - dispenser - dispenser - galvanic bath.

It should be noted that the exact formula is only functional in the studied concentration range from 0 to 100 mg/l outside of range of their behavior is unpredictable and requires further investigation.

LITERATURE

1. Litovka J.V., Tkachev A.G. Kuznetsov O.A., Dyakov I.A. Getting nanomodified composite Nickel electroplating // electroplating and surface treatment, 2010, volume XVIII, No. 1, p.17-21.

2. Litovka J.V., Tkachev A.G. Kuznetsov O.A., Dyakov IA, carpenter, R.A., Development of technology for nanomodified electroplating // proc. Dokl. 7 international. proc. "Coatings and surface treatment". M., 2010, p.55-56.

3. Misen what about the SV, Tkachev A.G. Carbon nanomaterials. Production, properties, applications. - M.: Mashinostroenie, 2008, 297 S.

4. Patent of great Britain No. 1538656, IPC C23F 9/00, 1979.

5. The copyright certificate of the Russian Federation No. 1741476, IPC SS 3/26, 2000

6. The copyright certificate of the Russian Federation No. 1650795, IPC C25D 21/13, 1991

1. The method of adjusting the concentration of carbon nanotubes (CNTS) in the electrolyte electrochemical deposition of metals, including the measurement of the temperature of the electrolyte in the electroplating bath, the measurement of the concentration of CNTS and restore the concentration of CNTS in the electrolyte, characterized in that the measurement of the concentration of CNTS in the electrolyte is carried out by passing the electrolyte through the optical system of the photometer according to the indications of which shall restore the initial concentration of CNTS dosed supply of CNTS in the electrolyte, which is then passed through the disperser and return in the galvanic bath.

2. The method according to claim 1, characterized in that the content of CNTS in the electrolyte is determined at the operating temperature of the electrolyte, depending on its optical density and the magnitude of the transmission coefficient.



 

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Proportioner // 2248030

FIELD: machine engineering, namely aircrafts, possibly fuel system devices for regulating and feeding fuel components to engine.

SUBSTANCE: apparatus includes housing, supplying and discharging pipelines and mechanisms for regulating relation and flow rate of components. Housing is in the form of set of sleeves with lids whose number is equal to number of controlled components. Movable and stationary partitions with flow-through windows are placed in said sleeves. Partitions divide cavity of sleeves by inlet and outlet chambers. Sleeves are provided with supplying and discharging pipelines respectively. Movable partitions are spring-loaded and they are mounted in splines of central sleeve in the form of cylinder. Said cylinder is placed in central zones of sleeves and lids and it is mounted in boundary lids. Each stationary partition includes rigidly secured to it lever for setting relation of fuel components. Said lever is fixed to housing by means of ball fixing member.

EFFECT: possibility for regulating total flow rate of components at keeping necessary mutual relation of them.

2 dwg

FIELD: automation of processes for transporting oil with different quality parameters through different pipelines.

SUBSTANCE: systems may include at least two oil pipelines designed for transporting oil flows and oil pipeline designed for mixed oil flow. System includes shutters mounted in oil conduits and designed for controlling respective oil flows, devices for measuring density, flow rate, content of sulfur or chlorides and water content. Said devices are connected with units for calculating parameters and determining relation of said parameters in each flow relative to mixed flow. System also includes microprocessor designed for comparing measured and calculated parameters with preset ones and for generating signals for regulating shutter position in respective flows according to comparison results.

EFFECT: possibility for controlling oil compounding process according to several quality parameters.

1 dwg

FIELD: petroleum processing and petrochemistry.

SUBSTANCE: process comprises heating additives, pumping and mixing them with oil components. Oil components and additives are mixed by synchronously feeding them into collecting channel provided with static mixer. Synchronization is provided by frequency changers, employed in automated control system, to control speed of rotation of pump motors. Oil components are controlled by means of Coriolis-type flowmeters.

EFFECT: reduced oil preparation time, reduced power and expensive materials consumption, and increased component dispensing accuracy.

3 cl, 1 dwg

FIELD: engineering of automation systems.

SUBSTANCE: method for compounding oil includes continuous measurements of sulfur content in mixed oil flow and source flow of sulfurous oil and adjusting feeding thereto of highly sulfurous oil for providing required sulfur content in mixed oil flow. Adjustment is performed by evening out oscillations of sulfur content in mixed flow, for which purpose reservoir or reservoir park is used, connected to flow of highly sulfurous oil, in case when sulfur content in mixed flow drops below acceptable levels, a portion of highly sulfurous oil is fed thereto, enough to provide for required sulfur content in mixed flow, in case when sulfur content in mixed flow exceeds required value, feeding of highly sulfurous oil from reservoir or reservoir park to mixing point is halted, when reservoir or reservoir park is overflowed, flow of highly sulfurous oil is sent to mixing point with flow value equal to flow value of highly sulfurous oil entering aforementioned reservoir or reservoir park.

EFFECT: maintained stability and evenness of mixing.

2 cl, 3 dwg, 3 tbl

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