SU1444406A1 - Apparatus for automatic monitoring and controlling of composition of solution in copper chemical plating bath - Google Patents

Abstract

The invention relates to chemical coating equipment. The purpose of the invention is the expansion of technological capabilities, increasing the accuracy of control and regulation of the concentration of sodium hydroxide and formalin in a solution of chemical copper. The device consists of a sampling circulating pump 1, to the outlet of which under

Description

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the first channel of the peristaltic pump 2 is connected, the output of which is connected to the flow-through light-transparent cell of the photocrystal 3 connected to the flow-through electrolytic cell 4 connected to the flow-through electrolytic cell 5 through the peristaltic pump 6. In addition, the device has a capacity of 7 sulfuric acid solution and a capacity of 8 sulphi, t, and sodium, unit 9 for controlling the concentration of copper, to the output of which the metering pump 10 is connected through. software relay P. In cell 4, a pH electrode 12 and a comparison electrode 13 are installed, connected to a unit 14 for measuring and adjusting sodium hydroxide concentration, the output of which is connected to the metering pump 15 and the solenoid valve 16 via a time relay T7

Cell 5 contains measuring pH electrode 18 and comparison electrode 19 associated with a formalist concentration measuring and control unit 20, the output of which is connected to a metering pump 21 and a solenoid valve 22 via program time relay 23. The device also contains a capacity of 24 distilled water, a capacity of 25 concentrated sulfuric acid, a capacity of 26 copper sulfate corrective solution, a capacity of 27 sodium hydroxide corrective solution, a capacity of 28 corrective formalin solution. The expansion of techno - logical capabilities is achieved by the introduction of three software time relays into this device, a capacity of distilled water, a tank of concentrated sulfuric acid and

two solenoid valves, 1 Il.

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The invention relates to chemical coating equipment, namely, devices for controlling and regulating the composition of solutions of chemical copper baths.

The purpose of the invention is the expansion of technological capabilities; Increasing. The accuracy of controlling and regulating the concentration of sodium hydroxide and formalin in a solution of chemical copper.

The drawing shows a block diagram of this device.

The device consists of a sampling circulating pump 1, the output of which is connected to the first channel of the peristaltic pump 2, the output of which is connected to the flow-through translucent cell of the photocolorimeter 3 connected by means of a hose to a flow-through electrolytic cell 4 connected to the second flow-through electrolytic cell 5, through the second peristaltic pump 6. Cells 4 and 5 are connected to a tank — Z of sulfuric acid solution and capacity of 8 sodium sulfite solution

through pumps 2 and 6 respectively. The output of photocolorimeter 3 is electrically connected with the copper concentration control unit, to the output of which the metering pump 10 is electrically connected via a program relay of time II, type 24 PB.

Cell 4 has a measuring pH electrode 12 and a comparison electrode 13, electrically connected to the sodium hydroxide measuring and control unit 14,

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its course is electrically connected with

metering pump 15 and the solenoid valve 16 through the program time relay 17.

: Cell 5 contains measuring pH electrode 18 and comparison electrode 19, electrically connected to the formalin concentration measuring and control unit 20, the output of which is electrically connected to the pump 5 by metering unit 21 and the solenoid valve 22 via time program relay 23.

To the tank 7 by means of a vshang and a solenoid valve 16, a tank 24 of distilled water is connected, positioned above the tank 7.

A capacitor 25 of concentrated sulfuric acid is connected to the capacitor 8 of the sodium sulfite solution by means of the α-hose and the electromagnetic valve 22.

The inlets of the metering pumps 10, 15 and 21 are connected via hoses to a tank 26 of copper sulfate correction solution, a tank of 27 sodium hydroxide correction solution, 28 tank of the formalin corrective section, respectively, and the outlets of these pumps are connected to the chemical bath 29 medneni.

Blocks 14 and 20 for measuring and adjusting the concentration of sodium hydroxide and formalin consist of two blocks: measuring block 30, legs according to the industrial P-201 converter circuit, and adjustment block 31, performed according to the BAT-5 automatic titration block scheme.

The device works as follows.

Before the start of automatic control and adjustment, pre-prepared corrective solutions of copper sulfate, sodium hydroxide and formalin are poured into the vessel 26-28. Capacity 7 for 2/3 of the volume is filled with a solution of sulfuric acid, prepared in such a way that when mixing one volume of chemical copper solution containing the maximum possible concentration of sodium hydroxide and one volume of solution of sulfuric acid, a mixture of pH 11.5 The container 24 is filled with distilled water and placed above the container 7. The container 8 by 3/4 of the volume is filled with a solution of sodium sulphite with concentrations of 100 g / l. The container 25 is filled with concentrated sulfuric acid and placed above the container 8. Then the device is turned on for heating.

After applying voltage to the device, a circulation pump 1, peristaltic pumps 2 and 6, and also program relays 11, 17 and 3 are turned on. At the same time, a sample of a solution of chemical copper from the bath 29 by the circulation pump 1 is fed to the inlet of the peristaltic pump 2 and

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then it enters the flow-through light-perceptible cuvette of the photocolorimeter 3, after which, mixing with a solution of sulfuric acid from the tank 7 in a 1: 1 ratio, is fed into the electrolytic cell 4. From the cell 4, the resulting mixture of a solution of a chemical copper bath with a solution of sulfuric acid by a peristaltic pump 6 is mixed with a sodium sulfite solution in a 1: 1 volume ratio and fed to an electrolytic cell 5, from where it is discharged through overflow,

At the end of the time required for the device to warm up, the software time relay 17 electrically connects the output of the unit 14 to the solenoid valve 16 to automatically bring the concentration of the sulfuric acid solution to the optimum value by diluting with distilled water from the tank 24 to the CAPACITY 7 by gravity through the electromagnet. valve 16, controlled by block 14.

The optimum concentration of the sulfuric acid solution is adjusted so that when the chemical copper solution from the bath 29 is mixed with the sulfuric acid solution in a volume ratio of 1: 1, the pH of the mixture obtained in the Electrolytic cell 4 is 11,, 2, which ensures maximum accuracy in controlling concentration deviations sodium hydroxide in the process of chemical copper from the initial value.

The time of connecting the solenoid valve 16 to the unit 14, by setting the program time relay 17, is selected based on the dilution of the initial solution of sulfuric acid in the tank 7 to a concentration corresponding to the minimum permissible concentration of sodium hydroxide in the solution of chemical copper, at which the mixing A single Q volume of a solution of chemical copper with a single volume of sulfuric acid gives a mixture with a pH of 11.5. The activation of the solenoid valve 16 is carried out by the unit 14 controlling and regulating the concentration of sodium hydroxide at a pH of 4 .. in the cell: below 11.5. This value is the trigger threshold for

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the settings of the sodium hydroxide concentration control unit 31.

At the end of the time for automatically bringing the concentration of the sulfuric acid solution to the optimum value, the program relay i 7 of time switches off the output of block 14 from the solenoid valve 16, and the program relay of time 23 electrically connects the output of block 20 to the solenoid valve 22 acidifying the sodium sulfite solution to an optimum value by adding concentrated sulfuric acid from tank 25 to tank 8 by gravity through a solenoid valve 22, controlled by block 20, ptimalnoe acidification

of sodium sulfite solution is selected 20 29, From flowing translucent

so that when mixing a mixture of solution from cell 4 with an acidified solution of sodium sulfite in a volume ratio of 1: 1, the pH of the resulting mixture in an electrolytic cell, 5 and the gel has a value of 11.5.10.2, which ensures maximum accuracy in controlling deviations of formalin concentration in a chemical solution copper from the original.

The timing of the connection of the electromagnetic valve 22 to the block 20, specified by the programmable time relay 23, is selected in the calculation of acidification of the initial solution of sodium sulfite in the tank 8 to mt & degree, so that when mixing one volume of the chemical mediating solution containing the maximum the formalin concentration, with one volume of the resulting acidified solution of sodium sulfite, formed a mixture with a pH of 1.5,

The solenoid valve 22 is turned on by block 20 with a pH value in the cell of 5 nyuke 11.5,. This value is the trigger value for setting the formalin concentration adjusting unit 31.

At the end of the time for automatically bringing the degree of acidification of sodium sulfite solution to the optimum value, the program relay 23

Electrical signals from glass pH electrodes 12.3 and 18.19 are fed to measurement and control units 14 and 20, where they are compared with threshold values for triggering the controllers, respectively, time off from the output of unit 20 from. g.

solenoid valve 22 and electrification pH 11, 5. Parametrically connects the output of the block 20 with B to the process of the bath with a chemical dosing pump 21 "At this moment of copper plaster, programmed turnips I and 17 time sodium hydroxide concentrations occur in it

electrically connect the outputs of the blocks 9 and 14 to the metering pumps 10 and 15, respectively, transferring the device to the mode of automatic control and regulation of the composition of the chemical copper bath 29.

At the same time, a sample of the chemical copper solution from the bath 29 enters the flow-through light-transparent cell of the photocolorimeter 3, which analyzes the sample for copper content. When the copper concentration deviates from a given value, the control unit 9 generates and delivers a control electrical signal to the dosing pump Sho When the electric signal arrives, the pump 10 pushes the correction liquid from the tank 26 into the bath

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The cuvettes of the photocolorimeter 3 sample the solution of the chemical copper plating into the electrolytic cell 4, where the peristaltic pump 2 from the tank 7 feeds the solution of sulfuric acid for mixing with the sample of the chemical copper plating solution in a volume ratio of 1: 1. The glass pH electrodes 12 and 13 installed in the electrolytic cell 4 create an electrical power proportional to the pH value, which depends on the concentration of sodium hydroxide, on the mixture from cell 4, using calcium 6, is mixed with acidified sodium sulfite solution in the V1 ratio and fed in cell 5 located in it. a pair of glass pH electrodes 18 and 19s in which the reaction results in a replacement of formalin with sodium sulfite

 therefore, -1- (oH) -so:; + OH, resulting in the formation of additional OH groups, C3 mmar, whose effect on the change in pH of the mixture is proportional to the concentration of formalin.

Electric signals from glass pH-electrodes 12.3 and 18.19 are fed to blocks 14 and 20 of measurement and control, where they are compared with the threshold values of the triggering of the regulators, respectively. g.

pH of 11, 5. In the process of operation of a chemical formalin bath, leading to a decrease in pH in cells D and 5. When H decreases below 11.5, blocks 14 and 20 produce and send control signals to the metering pumps 15 and 21, and the latter turn on and serve in the bath 29 correction solutions from from tanks 27 and 28. Upon reaching the. In the cells 4 and 5, the pH values of 11.5, the adjustment blocks 14 and 20, turn off the dosing pumps 15 and 21.

When carrying out the next cycle of monitoring and adjusting the composition of the solution of a chemical bath, the preparation and operation of the device occurs in the sequence described.

This device has advanced technological capabilities, as it provides automatic control and regulation of chemical copper solutions with any ratio of the concentrations of the main components, allows you to control and regulate the concentrations of copper, sodium hydroxide and formalin with an accuracy of 10.2 g / l, as well as to increase the percent yield of suitable products from 3% due to a more stable maintenance of the initial concentrations of the components of the solution of a chemical copper bath.

Claims (1)

Invention Formula A device for automatically controlling and adjusting the composition of the chemical bathing bath solution in a two-flow electrochemical cell consisting of a copper concentration control unit, the output of which is electrically connected to a concentrated sulfuric acid copper dosing pump, and the input - with a photocolorimeter - an innovative translucent flow cell, connected through a hose and a first peristaltic pump with a sampling circulating pump, a measuring and regulating unit ontsentratsii sodium hydroxide whose output RE VNIIPI Order 6461/30 Random polygons pr-tie, Uzhgorod, st. Project, 4 with 0 5 o five d 0 It is connected to a metering pump: a concentrated sodium hydroxide solution, and an input is connected to a reference electrode and pH measuring electrode, located in the first flow electrolytic cell connected by a peristaltic pump with a flow-through transparent solution and a capacitance of sulfuric acid solution, a unit for measuring and regulating formalin concentration the output of which is electrically connected to the formalin dosing pump, and the input to the comparison electrode and the pH measuring electrode located in. A second flow electrolytic cell connected by a second peristaltic pump with a first electrolytic cell and a capacity of sodium sulfite solution, characterized in that, in order to expand technological capabilities, improve the accuracy of monitoring and controlling the concentration of sodium hydroxide and formalin in a chemical copper sizing solution, it is equipped with three software time relay, capacity of distilled water, capacity of concentrated sulfuric acid and two electromagnetic valves, one of oryh, electric; It is connected through the first software time relay to the sodium hydroxide concentration and control unit, and the other via the second software time relay to the formalin concentration and concentration control unit, while the sodium hydroxide concentration and formalin control unit and the copper concentration controllers are connected to metering pumps through the appropriate software time relays, the distilled water tank through the first solenoid valve is connected to the solution oh acid and concentrated sernstsr acid capacitance through a second solenoid valve connected to tank solution of sodium sulfite. Circulation 622 Subscription