CN108914197A - A kind of on-Line Monitor Device and its application - Google Patents
A kind of on-Line Monitor Device and its application Download PDFInfo
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- CN108914197A CN108914197A CN201811096518.4A CN201811096518A CN108914197A CN 108914197 A CN108914197 A CN 108914197A CN 201811096518 A CN201811096518 A CN 201811096518A CN 108914197 A CN108914197 A CN 108914197A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
- C25D21/14—Controlled addition of electrolyte components
Abstract
The present invention provides a kind of on-Line Monitor Device and its applications, the on-Line Monitor Device, including electroplating unit, dissolves unit and be connected to electroplating unit and dissolve the first conveying device between unit, the on-Line Monitor Device further includes analysis cell and controller, the analysis cell is connect with electroplating unit, described controller one end is connected with analysis cell, and the other end is connect with the first conveying device；The device can be used for the concentration of metal ion in real-time monitoring electroplate liquid, to adjust the concentration of metal ions in electroplate liquid, positive effect is generated to electroplating effect.
Description
Technical field
The present invention relates to field of electroplating, it is related to a kind of on-Line Monitor Device and its application.
Background technique
Suction of the ferric ion to the light of 302nm wavelength is utilized usually using photometry during electro-coppering liquid medicine
Receive, convert electric signal for ferric ion concentration, then by the corresponding electromechanical assembly of micro computer control, realize to ferric iron from
The On-line Control of sub- concentration；The method can only monitor ferric ion, to detect other ions then and must be further added by one layer it is other
The detection product of wavelength, and optical means haves the shortcomings that disturbing factor is more, to limit its application.
CN102081408A discloses a kind of ion concentration monitoring system, mentions the system comprises plating membrane cavity, to plating membrane cavity
For the gas supply device of mixed gas, electric vacuum pipe, optical fiber and gas flow controller；The intracavitary mixed gas of the plated film
Being discharged excitation is different ions；One end of the electric vacuum pipe is connected to plating membrane cavity, and the other end passes through optical fiber and gas stream
Amount controller is connected；The electric vacuum pipe excites mixed gas to generate emission spectrum, which is transmitted through the fiber to gas stream
Amount controller；The gas flow controller include presetting module for setting the concentration ratio value of the intracavitary different ions of plated film,
For analyzing emission spectrum to obtain the spectral analysis module of the actual concentrations ratio value of the intracavitary ion of plated film and for comparing
The ion concentration ratio value of setting control module compared with actual ions concentration ratio value；It is described relatively control module according to than
The gas supply flow of gas supply device is controlled compared with result the intracavitary ion concentration ratio of plated film is maintained setting value；The invention
The ion concentration of target material pollution optical fiber for detection, does not refer to and can be used for detecting the dense of metal ion in electroplating unit
Degree.
CN204203159U discloses a kind of online heavy metal monitor with pre- plated film function, including micro-injection
Pump, analysis cell, distilled water bottle, test bottom liquid bottle, water sample bottle, standard solution bottle, liquid parting bottle, coating liquid bottle, two peristaltic pumps,
Coating liquid recycling bin, two waste liquid barrels and ten two-bit triplet solenoid valves；Online heavy metal monitor described in the utility model
It is mainly used for monitoring the heavy metal ion in water, does not refer to the dense of the heavy metal ion that can be used in real-time monitoring electroplate liquid
Degree.
Therefore, developing a kind of device that metal ion in electroplating unit can be monitored online is highly desirable.
Summary of the invention
The purpose of the present invention is to provide a kind of on-Line Monitor Device and its application, the line monitoring device can be used in real time
The concentration of metal ion in electroplate liquid is monitored, to adjust the concentration of metal ions in electroplate liquid, electroplating effect is generated positive
Effect.
In order to achieve that object of the invention, the present invention uses following technical scheme：
One of the objects of the present invention is to provide a kind of on-Line Monitor Devices, including electroplating unit, dissolution unit and company
It is connected to electroplating unit and dissolves the first conveying device between unit, the on-Line Monitor Device further includes analysis cell and control
Device, the analysis cell are connect with electroplating unit, and described controller one end is connected with analysis cell, and the other end and the first conveying device connect
It connects.
The present invention provides a kind of on-Line Monitor Device, which includes analysis cell, controller and the first conveying
Chemical signal can be converted to electric signal by device, analysis cell, and controller can the gold according to corresponding to standard curve reading electric signal
The concentration for belonging to ion adjusts the concentration of metal ion in electroplating unit by control the first conveying device, thus effectively
Control electroplating effect.
In the present invention, the analysis cell is the cavity for conveying liquid, is inserted with electrode in the cavity.
In the present invention, the electrode includes working electrode, reference electrode and to electrode.
In the present invention, electrode may include working electrode, reference electrode and to electrode, and electrode can also be working electrode, reference
Electrode and electrode is integrally formed, forms a combination electrode.
In the present invention, the working electrode is platinum electrode.
Working electrode need to carry out electrochemical cleaning at measurement interval in the present invention, and electrochemical cleaning is to add on the working electrode (s
Add the current potential of a 1-2V, to aoxidize the hard-degraded substance adsorbed on working electrode.
In the present invention, the current potential refers to current potential of the working electrode relative to reference electrode.
In the present invention, the reference electrode is silver-colored silver chloride reference electrode or saturated calomel reference electrode.
In the present invention, described is platinum electrode, glass-carbon electrode, gold electrode, graphite electrode, Ti electrode, stainless steel to electrode
Any one in electrode or copper electrode.
In the present invention, the import of the analysis cell is connected by the first outlet of the second conveying device and electroplating unit bottom
It connects.
In the present invention, the extraction mouth of the analysis cell and the top of electroplating unit connect.
A circulation is formed between analysis cell and electroplating unit of the present invention, the second conveying device is defeated by the solution of electroplating unit
It send to analysis cell, is analyzed in real time, after analysis, solution is returned in electroplating unit, both can be monitored in real time so molten
Liquid concentration, and not will cause the waste of raw material.
In the present invention, the import that the second outlet of the electroplating unit bottom passes through the first conveying device and dissolution unit
Connection.
In the present invention, it is connect at the top of the top extraction mouth and electroplating unit of the dissolution unit.
A circulation is also formed between electroplating unit of the present invention and dissolution unit, the first supply unit will be in electroplating unit
Liquid is delivered in dissolution unit, and liquid reacts in dissolution unit with copper, and the liquid after reaction is returned in electroplating unit, ginseng
With electroplating process.
In the present invention, the electroplating unit includes power supply, cathode, anode and electroplate liquid.
In the present invention, the anode is coated titanium electrode.
In the present invention, the cathode is pcb board.
In the present invention, the first conveying device is pumping.
In the present invention, the second conveying device is pumping.
In the present invention, the controller is used to control the conveying speed of the first conveying device.
The second object of the present invention is to provide on-Line Monitor Device described in a kind of first purpose in concentration of metal ions
Application in on-line monitoring.
In the present invention, the method for the concentration of metal ions on-line monitoring includes the following steps：
(1) standard curve of concentration of metal ions and current strength is formulated；
(2) electroplate liquid after reacting electroplating unit is delivered to analysis cell, converts electricity for chemical signal in analysis cell
Signal is flowed, current signal is delivered to controller, controller obtains metal ion according to the size and standard curve of current signal
Concentration, start the Internal Control Procedure of controller, with control first conveying device to dissolution unit conveying speed, by metal
Ion concentration controls within the scope of preset concentration, realizes the on-line monitoring to concentration of metal ions.
In the present invention, the metal ion includes any one in ferrous ion, ferric ion or tetravalent vanadium ion
Kind or at least two combination.
A circulation is formed between analysis cell and electroplating unit of the present invention, the second conveying device is defeated by the solution of electroplating unit
It send to analysis cell, is analyzed in real time, after analysis, electroplating solution is returned in electroplating unit；Analysis cell is by electroplating unit
Electroplate liquid after middle reaction is analyzed, and converts electric signal for chemical signal, electric signal transmission passes through standard into controller
Curve obtains the concentration of corresponding metal ion by current strength, and molten copper slot is connected with electroplating bath in the device, works as electroplating bath
When middle ferrous ion, tetravalent vanadium ion concentration are lower or ferric ion concentration is higher, accelerate the defeated of the first conveying device
Speed is sent, electrolyte is quickly delivered in dissolution unit, ferric ion is converted into ferrous ion under the action of copper,
And it can also supplement copper ion；When ferrous ion, tetravalent vanadium ion concentration is higher in electroplating bath or ferric ion concentration
When lower, slow down the conveying speed of the first conveying device, react it in electroplating unit；Between electroplating unit and dissolution unit
Also a circulation is formed, the liquid in electroplating unit is delivered in dissolution unit by the first supply unit, and liquid is in dissolution unit
In reacted with copper, the liquid after reaction is returned in electroplating unit, participate in electroplating process.
In the present invention, the ferric ion concentration and the standard curve of current strength are in working electrode relative to ginseng
Current potential than electrode is to obtain under 0V and 0.5V checker, and 0V refers to the current potential that ferric ion can be reduced herein,
Its value is not limited to 0V, can between -0.2V~0.4V value, 0.5 V refers to ferric ion and ferrous ion herein
Equilibrium potential, both ferric ion cannot be reduced under this current potential, and ferrous ion can not be oxidized, and value is not limited to
0.5V, can between 0.4V~0.7V value, the composition of the selection of above-mentioned potential value and the type of reference electrode and electroplate liquid it is special
It is not that the concentration of sulfuric acid and copper sulphate has certain relationship, has offset by a small margin with the variation of above-mentioned condition.
In the present invention, the ferrous ion concentration and the standard curve of current strength be current potential be 0.5V and
It is obtained under 1.2V checker, herein the meaning of 0.5V and consistent above, 1.2V refers to the electricity that ferrous ion can be oxidized
Position, and the current potential that the vanadium ion of tetravalence can't be oxidized, value are not limited to 1.2V, can take in the range of 0.7V~1.3V
Value.
In the present invention, the standard curve of the tetravalent vanadium ion concentration and current strength be current potential be 1.2V and
It is obtained under 1.6V checker, herein the meaning of 1.2V and consistent above, 1.6V refers to the electricity that tetravalent vanadium ion can be oxidized
Position, value is not limited to 1.6V, can between 1.4V~1.8V value, it is too small to cross low current signal, it is excessively high easily cause it is serious
Oxygen evolution reaction influences accuracy.
When current potential is widely varied, electric current is controlled by diffusion, when one timing of electrolyte flow state, in constant potential
Under, electric current is directly proportional to concentration of metal ions；When current potential is in 0V and 0.5V checker, the three of various concentration can be can be visually seen
The electric current that valence iron ion responds under 0.5V current potential makees standard curve according to the concentration of electric current and ferric ion；When current potential exists
When 0.5V and 1.2V checker, the electric current that the ferrous ion of various concentration responds under 1.2V current potential, root can be can be visually seen
Concentration according to electric current and ferrous ion makees standard curve；When current potential checker between 1.2V and 1.6V, it is in current potential
When 1.2V, only ferrous ion can be electrolysed, and when current potential is 1.6V, ferrous ion and tetravalent vanadium ion can be electric
Solution, the difference of the two faradic currents then correspond to faradic currents when tetravalence vanadium is oxidized, according to electric current and tetravalent vanadium ion
Concentration makees standard curve.
Compared with the existing technology, the invention has the advantages that：
It includes analysis cell and controller that the present invention, which provides a kind of on-Line Monitor Device, and analysis cell is connect with electroplating unit, control
Device one end processed is connected with analysis cell, and the other end is connect with the first conveying device, can be used for monitoring on-line in electroplating unit metal from
The concentration of son, including ferrous ion concentration, ferric ion concentration and tetravalent vanadium ion concentration, control the first conveying device
To the conveying speed of dissolution unit, by concentration of metal ions control within the scope of preset concentration, thus effectively control plating
Effect.
Detailed description of the invention
Fig. 1 is the schematic diagram of on-line monitoring device in the embodiment of the present invention, wherein：1, electroplating unit；2, dissolve unit；
3, the first conveying device；4, analysis cell；5, controller；6, the second conveying device；
Fig. 2 is the schematic diagram of analysis cell in the embodiment of the present invention, wherein：41, cavity；42, working electrode；43, reference electricity
Pole；44, to electrode；45, import；46, produce mouth；
Fig. 3 is that current potential is in 0V and 0.5V checker in the embodiment of the present invention 1, ferric ion concentration and faraday's electricity
The standard curve of stream；
Fig. 4 is that current potential is in 0.5V and 1.2V checker in the embodiment of the present invention 1, ferrous ion concentration and faraday
The standard curve of electric current；
Fig. 5 is that current potential is in 1.2V and 1.6V checker in the embodiment of the present invention 1, tetravalent vanadium ion concentration and faraday
The standard curve of electric current.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.Those skilled in the art should be bright
, the described embodiments are merely helpful in understanding the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
The present embodiment provides a kind of on-Line Monitor Devices, as shown in Figure 1, including electroplating unit 1, dissolution unit 2, first
Convey device 3, analysis cell 4, controller 5 and the second conveying device 6；The analysis cell 4 is connect with electroplating unit 1；The control
5 one end of device is connected with analysis cell 4, and the other end is connect with the first conveying device 3；The second outlet of 1 bottom of electroplating unit is logical
It crosses the first conveying device 3 to connect with the import for dissolving unit 2, the top extraction mouth and electroplating unit 1 of the dissolution unit 2 push up
Portion's connection.
As shown in Fig. 2, analysis cell 4 is the cavity 41 for conveying liquid, electrode is inserted in the cavity；The electrode packet
Include working electrode 42, reference electrode 43 and to electrode 44；Wherein working electrode 42 is platinum electrode, and reference electrode 43 is silver-colored silver chlorate
Reference electrode is platinum electrode to electrode 44；The import 45 of analysis cell 4 passes through the second conveying device 6 and 1 bottom of electroplating unit
First outlet connection, the extraction mouth 46 of the analysis cell 4 are connect with the top of electroplating unit 1；Electroplate liquid to be measured is from analysis cell 4
45 feed liquor of import goes out liquid from extraction mouth 46.
The electroplating unit 1 includes power supply, cathode, anode and electroplate liquid；The anode is coated titanium electrode, the yin
Extremely with the pcb board of plated-through-hole；The electroplate liquid includes following component：2.5g/L tetravalent vanadium ion, 3.7g/L ferrous ion,
1.3g/L ferric ion, 140g/L cupric sulfate pentahydrate, 210g/L sulfuric acid and 60mg/L chloride.
The controller 5 is used to control the conveying speed of the first conveying device.
Application of the on-Line Monitor Device in concentration of metal ions on-line monitoring, the method for on-line monitoring include as follows
Step：
(1) standard curve of concentration of metal ions and current strength is formulated；
(2) electroplate liquid after reacting electroplating unit is delivered to analysis cell, converts electricity for chemical signal in analysis cell
Signal is flowed, current signal is delivered to controller, controller obtains metal ion according to the size and standard curve of current signal
Concentration, start the Internal Control Procedure of controller, with control first conveying device to dissolution unit conveying speed, by metal
Ion concentration controls within the scope of preset concentration, realizes the on-line monitoring to concentration of metal ions.
Fig. 3 is the standard curve of ferric ion concentration and faradic currents in the embodiment of the present invention, when current potential in 0V and
Between 0.5V when checker, the electric current that the ferric ion of various concentration responds under 0.5V current potential can be can be visually seen, according to
The concentration of electric current and ferric ion makees standard curve, obtains homing method y=-0.6819x-0.2912, is obtained by regression equation
To linearly dependent coefficient (R2) it is 0.9981, illustrate that the standard curve is linearly good；
Fig. 4 is the standard curve of ferrous ion concentration and faradic currents in the embodiment of the present invention, when current potential is in 0.5V
The electric current responded under 1.2V current potential with the ferrous ion that various concentration when checker, can be can be visually seen when 1.2V, according to
The concentration of electric current and ferrous ion makees standard curve, obtains homing method y=0.9271x+0.033, is obtained by regression equation
Linearly dependent coefficient (R2) it is 0.9998, illustrate that the standard curve is linearly good；
Fig. 5 is the standard curve of tetravalent vanadium ion concentration and faradic currents in the embodiment of the present invention, when current potential is in 1.2V
Between 1.6V when checker, when current potential is 1.2V, only ferrous ion can be electrolysed, sub- when current potential is 1.6V
Iron ion and tetravalent vanadium ion can be electrolysed, the difference of the two faradic currents, method when just corresponding tetravalence vanadium is oxidized
Electric current is drawn, standard curve is made according to electric current and tetravalent vanadium ion concentration, obtains homing method y=0.1568x+0.1186, by
Regression equation obtains linearly dependent coefficient (R2) it is 0.9924, illustrate that the standard curve is linearly good.
By current signal obtained in analysis cell and standard curve come metal ion in quantitative corresponding electroplate liquid
Concentration starts the Internal Control Procedure of controller when ferric ion concentration is higher than 1.43g/L in electroplate liquid, can accelerate the
The conveying speed of one conveying device；When ferric ion concentration is lower than 1.17 g/L in electroplate liquid, start the inside of controller
Program is controlled, the conveying speed of the first conveying device can be slowed down；When ferrous ion concentration is higher than 4.07g/L in electroplate liquid,
The Internal Control Procedure for starting controller, can slow down the conveying speed of the first conveying device；When with ferrous ion concentration be prison
When controlling index, when ferrous ion concentration is lower than 3.33g/L in electroplate liquid, starts the Internal Control Procedure of controller, can add
The conveying speed of fast first conveying device；When tetravalent vanadium ion concentration is higher than 2.75g/L in electroplate liquid, start the interior of controller
Portion controls program, can slow down the conveying speed of the first conveying device；When tetravalent vanadium ion concentration is lower than 2.25 g/L in electroplate liquid
When, start the Internal Control Procedure of controller, the conveying speed of the first conveying device can be accelerated.
Embodiment 2
The present embodiment provides a kind of on-Line Monitor Devices, as shown in Figure 1, including electroplating unit 1, dissolution unit 2, first
Convey device 3, analysis cell 4, controller 5 and the second conveying device 6；The analysis cell 4 is connect with electroplating unit 1；The control
5 one end of device is connected with analysis cell 4, and the other end is connect with the first conveying device 3；The second outlet of 1 bottom of electroplating unit is logical
It crosses the first conveying device 3 to connect with the import for dissolving unit 2, the top extraction mouth and electroplating unit 1 of the dissolution unit 2 push up
Portion's connection.
As shown in Fig. 2, analysis cell 4 is the cavity 41 for conveying liquid, electrode is inserted in the cavity；The electrode packet
Include working electrode 42, reference electrode 43 and to electrode 44；Wherein working electrode 42 is platinum electrode, and reference electrode 43 is saturation calomel
Reference electrode is glass-carbon electrode to electrode 44；The import 45 of analysis cell 4 passes through the second conveying device 6 and 1 bottom of electroplating unit
First outlet connection, the extraction mouth 46 of the analysis cell 4 are connect with the top of electroplating unit 1；Electroplate liquid to be measured is from analysis cell 4
45 feed liquor of import goes out liquid from extraction mouth 46.
The electroplating unit 1 includes power supply, cathode, anode and electroplate liquid；The anode is coated titanium electrode, the yin
The extremely band pcb board of partly filling out Microvia；The electroplate liquid includes following component：1g/L tetravalent vanadium ion, 5.2g/L ferrous iron from
Son, 0.8g/L ferric ion, 140g/L cupric sulfate pentahydrate, 210g/L sulfuric acid, 60mg/L chloride, 5mg/L levelling agent and
2g/L brightener.
The controller 5 is used to control the conveying speed of the first conveying device.
Application of the on-Line Monitor Device in concentration of metal ions on-line monitoring, the method for on-line monitoring include as follows
Step：
(1) standard curve of concentration of metal ions and current strength is formulated；
(2) electroplate liquid after reacting electroplating unit is delivered to analysis cell, converts electricity for chemical signal in analysis cell
Signal is flowed, current signal is delivered to controller, controller obtains metal ion according to the size and standard curve of current signal
Concentration, start the Internal Control Procedure of controller, with control first conveying device to dissolution unit conveying speed, by metal
Ion concentration controls within the scope of preset concentration, realizes the on-line monitoring to concentration of metal ions.
It is quantified according to current signal obtained in standard curve described in Fig. 3, Fig. 4 and Fig. 5 in embodiment 1 and analysis cell
The concentration of metal ion in electroplate liquid starts the interior of controller when ferric ion concentration is higher than 0.88g/L in electroplate liquid
Portion controls program, can accelerate the conveying speed of the first conveying device；When ferric ion concentration is lower than 0.72g/L in electroplate liquid
When, start the Internal Control Procedure of controller, the conveying speed of the first conveying device can be slowed down；When being with ferrous ion concentration
When monitor control index, when ferrous ion concentration is higher than 5.72g/L in electroplate liquid, start the Internal Control Procedure of controller, meeting
Slow down the conveying speed of the first conveying device；When ferrous ion concentration is lower than 4.68g/L in electroplate liquid, start controller
Internal Control Procedure can accelerate the conveying speed of the first conveying device；When tetravalent vanadium ion concentration is higher than 1.1g/L in electroplate liquid
When, start the Internal Control Procedure of controller, the conveying speed of the first conveying device can be slowed down；When tetravalent vanadium ion in electroplate liquid
When concentration is lower than 0.9g/L, starts the Internal Control Procedure of controller, the conveying speed of the first conveying device can be accelerated.
Embodiment 3
The present embodiment provides a kind of on-Line Monitor Devices, as shown in Figure 1, defeated including electroplating unit 1, dissolution unit 2, first
Send device 3, analysis cell 4, controller 5 and the second conveying device 6；The analysis cell 4 is connect with electroplating unit 1；The controller 5
One end is connected with analysis cell 4, and the other end is connect with the first conveying device 3；The second outlet of 1 bottom of electroplating unit passes through
First conveying device 3 is connect with the import for dissolving unit 2,1 top of top extraction mouth and electroplating unit of the dissolution unit 2
Connection.
As shown in Fig. 2, analysis cell 4 is the cavity 41 for conveying liquid, electrode is inserted in the cavity；The electrode packet
Include working electrode 42, reference electrode 43 and to electrode 44；Wherein working electrode 42 is platinum electrode, and reference electrode 43 is saturation calomel
Reference electrode is gold electrode to electrode 44；The import 45 of analysis cell 4 passes through the second conveying device 6 and 1 bottom of electroplating unit
First outlet connection, the extraction mouth 46 of the analysis cell 4 are connect with the top of electroplating unit 1；Electroplate liquid to be measured is from analysis cell 4
45 feed liquor of import goes out liquid from extraction mouth 46.
The electroplating unit 1 includes power supply, cathode, anode and electroplate liquid；The anode is coated titanium electrode, the yin
The extremely band pcb board of filling out Microvia；The electroplate liquid includes following component：2.5g/L tetravalent vanadium ion, 4.2g/L ferrous iron from
Son, 1.8g/L ferric ion, 210g/L cupric sulfate pentahydrate, 100g/L sulfuric acid, 60mg/L chloride, 3.5mg/L levelling agent and
2g/L brightener.
The controller 5 is used to control the conveying speed of the first conveying device.
Application of the on-Line Monitor Device in concentration of metal ions on-line monitoring, the method for on-line monitoring include as follows
Step：
(1) standard curve of concentration of metal ions and current strength is formulated；
(2) electroplate liquid after reacting electroplating unit is delivered to analysis cell, converts electricity for chemical signal in analysis cell
Signal is flowed, current signal is delivered to controller, controller obtains metal ion according to the size and standard curve of current signal
Concentration, start the Internal Control Procedure of controller, with control first conveying device to dissolution unit conveying speed, by metal
Ion concentration controls within the scope of preset concentration, realizes the on-line monitoring to concentration of metal ions.
It must be arrived according to current signal obtained in standard curve described in Fig. 3, Fig. 4 and Fig. 5 in embodiment 1 and analysis cell
The concentration of metal ion starts controller when ferric ion concentration is higher than 1.98 g/L in electroplate liquid in quantitative electroplate liquid
Internal Control Procedure, the conveying speed of the first conveying device can be accelerated；When ferric ion concentration is lower than in electroplate liquid
When 1.62g/L, start the Internal Control Procedure of controller, the conveying speed of the first conveying device can be slowed down；When with ferrous iron from
When sub- concentration is Con trolling index, when ferrous ion concentration is higher than 4.62g/L in electroplate liquid, start the internal control of controller
Program can slow down the conveying speed of the first conveying device；When ferrous ion concentration is lower than 3.78g/L in electroplate liquid, starting
The Internal Control Procedure of controller can accelerate the conveying speed of the first conveying device；When tetravalent vanadium ion concentration is high in electroplate liquid
When 2.75 g/L, start the Internal Control Procedure of controller, the conveying speed of the first conveying device can be slowed down；When in electroplate liquid
When tetravalent vanadium ion concentration is lower than 2.25g/L, starts the Internal Control Procedure of controller, the conveying of the first conveying device can be accelerated
Speed.
Embodiment 4
The present embodiment provides a kind of on-Line Monitor Devices, as shown in Figure 1, including electroplating unit 1, dissolution unit 2, first
Convey device 3, analysis cell 4, controller 5 and the second conveying device 6；The analysis cell 4 is connect with electroplating unit 1；The control
5 one end of device is connected with analysis cell 4, and the other end is connect with the first conveying device 3；The second outlet of 1 bottom of electroplating unit is logical
It crosses the first conveying device 3 to connect with the import for dissolving unit 2, the top extraction mouth and electroplating unit 1 of the dissolution unit 2 push up
Portion's connection.
As shown in Fig. 2, analysis cell 4 is the cavity 41 for conveying liquid, electrode is inserted in the cavity；The electrode packet
Include working electrode 42, reference electrode 43 and to electrode 44；Wherein working electrode 42 is platinum electrode, and reference electrode 43 is silver-colored silver chlorate
Reference electrode is graphite electrode to electrode 44；The import 45 of analysis cell 4 passes through the second conveying device 6 and 1 bottom of electroplating unit
First outlet connection, the extraction mouth 46 of the analysis cell 4 are connect with the top of electroplating unit 1；Electroplate liquid to be measured is from analysis cell 4
45 feed liquor of import goes out liquid from extraction mouth 46.
The electroplating unit 1 includes power supply, cathode, anode and electroplate liquid；The anode is coated titanium electrode, the yin
The extremely band pcb board of filling out Microvia；The electroplate liquid includes following component：12g/L ferrous ion, 3g/L ferric ion,
140g/L cupric sulfate pentahydrate, 210g/L sulfuric acid, 60mg/L chloride, 5mg/L levelling agent and 2g/L brightener.
The controller 5 is used to control the conveying speed of the first conveying device.
Application of the on-Line Monitor Device in concentration of metal ions on-line monitoring, the method for on-line monitoring include as follows
Step：
(1) standard curve of concentration of metal ions and current strength is formulated；
(2) electroplate liquid after reacting electroplating unit is delivered to analysis cell, converts electricity for chemical signal in analysis cell
Signal is flowed, current signal is delivered to controller, controller obtains metal ion according to the size and standard curve of current signal
Concentration, start the Internal Control Procedure of controller, with control first conveying device to dissolution unit conveying speed, by metal
Ion concentration controls within the scope of preset concentration, realizes the on-line monitoring to concentration of metal ions.
It must be arrived according to current signal obtained in standard curve described in Fig. 3 and Fig. 4 in embodiment 1 and analysis cell quantitative
The concentration of metal ion in electroplate liquid starts the inside of controller when ferric ion concentration is higher than 3.3g/L in electroplate liquid
Program is controlled, the conveying speed of the first conveying device can be accelerated；When ferric ion concentration is lower than 2.7g/L in electroplate liquid, open
The Internal Control Procedure of movement controller can slow down the conveying speed of the first conveying device；When using ferrous ion as monitor control index
When, when ferrous ion concentration is higher than 13.2g/L in electroplate liquid, starts the Internal Control Procedure of controller, first can be slowed down
Convey the conveying speed of device；When ferrous ion concentration is lower than 10.8g/L in electroplate liquid, start the internal control of controller
Program can accelerate the conveying speed of the first conveying device.
The Applicant declares that the foregoing is merely a specific embodiment of the invention, but protection scope of the present invention not office
It is limited to this, it should be clear to those skilled in the art, any to belong to those skilled in the art and take off in the present invention
In the technical scope of dew, any changes or substitutions that can be easily thought of, and all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of on-Line Monitor Device, including electroplating unit (1), dissolution unit (2) and it is connected to electroplating unit (1) and dissolution
The first conveying device (3) between unit (2), which is characterized in that the on-Line Monitor Device further includes analysis cell (4) and control
Device (5), the analysis cell (4) connect with electroplating unit (1), and described controller (5) one end is connected with analysis cell (4), the other end
It is connect with the first conveying device (3).
2. on-Line Monitor Device according to claim 1, which is characterized in that the analysis cell (4) is for conveying liquid
Cavity (41), is inserted with electrode in the cavity (41)；
Preferably, the electrode includes working electrode (42), reference electrode (43) and to electrode (44)；
Preferably, the working electrode (42) is platinum electrode；
Preferably, the reference electrode (43) is silver-colored silver chloride reference electrode or saturated calomel reference electrode；
Preferably, described is platinum electrode, glass-carbon electrode, gold electrode, graphite electrode, Ti electrode, stainless steel electrode to electrode (44)
Or any one in copper electrode.
3. on-Line Monitor Device according to claim 1 or 2, which is characterized in that the import (45) of the analysis cell (4) is logical
The second conveying device (6) is crossed to connect with the first outlet of electroplating unit (1) bottom；
Preferably, the extraction mouth (46) of the analysis cell (4) is connect with the top of electroplating unit (1)；
Preferably, the second outlet of electroplating unit (1) bottom by first conveying device (3) and dissolve unit (2) into
Mouth connection；
Preferably, it is connect at the top of the top extraction mouth and electroplating unit (1) of dissolution unit (2).
4. on-Line Monitor Device according to claim 1-3, which is characterized in that the electroplating unit (1) includes
Power supply, cathode, anode and electroplate liquid；
Preferably, the anode is coated titanium electrode；
Preferably, the cathode is pcb board.
5. on-Line Monitor Device according to claim 1-4, which is characterized in that first conveying device (3)
For pumping；
Preferably, second conveying device (6) is pumping.
6. on-line monitoring device according to claim 1-5, which is characterized in that the controller (5) is used to control
The conveying speed of system the first conveying device.
7. a kind of application for on-Line Monitor Device described in claim 1-6 in concentration of metal ions on-line monitoring.
8. application according to claim 7, which is characterized in that the method for the concentration of metal ions on-line monitoring includes such as
Lower step：
(1) standard curve of concentration of metal ions and current strength is formulated；
(2) electroplate liquid after reacting electroplating unit is delivered to analysis cell, converts electric current letter for chemical signal in analysis cell
Number, current signal is delivered to controller, controller obtains the dense of metal ion according to the size and standard curve of current signal
Degree, starts the Internal Control Procedure of controller, to control conveying speed of the first conveying device to dissolution unit, by metal ion
Concentration controls within the scope of preset concentration, realizes the on-line monitoring to concentration of metal ions.
9. application according to claim 7 or 8, which is characterized in that the metal ion includes ferrous ion, ferric iron
Any one in ion or tetravalent vanadium ion or at least two combination.
10. according to the described in any item applications of claim 7-9, which is characterized in that the ferric ion concentration and electric current are strong
The standard curve of degree is obtained in the case where current potential is 0V and 0.5V checker；
Preferably, it is 0.5V and 1.2V checker that the ferrous ion concentration and the standard curve of current strength, which are in current potential,
Under obtain；
Preferably, it is 1.2V and 1.6V checker that the standard curve of the tetravalent vanadium ion concentration and current strength, which is in current potential,
Under obtain.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811096518.4A CN108914197A (en) | 2018-09-19 | 2018-09-19 | A kind of on-Line Monitor Device and its application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811096518.4A CN108914197A (en) | 2018-09-19 | 2018-09-19 | A kind of on-Line Monitor Device and its application |
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| CN201811096518.4A Pending CN108914197A (en) | 2018-09-19 | 2018-09-19 | A kind of on-Line Monitor Device and its application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129869A (en) * | 2019-05-24 | 2019-08-16 | 江西景旺精密电路有限公司 | A kind of method and system automatically analyzing addition gold salt based on real-time online |
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