A kind of method that the copper plate hardness shelf-life is tested using square Hull cell
Technical field
The present invention relates to electroplating technology, and in particular to one kind utilizes the Hull cell device to test copper plate hardness shelf-life
Method.
Background technology
Domestic and international gravure plate-making hard copper plating mostly uses acidiccopper plating, and the process components are simple, and cost is low, are easy to control
System.And requirement of the gravure plate-making for copper plate hardness is stricter, the wherein layers of copper hardness shelf-life is one critically important
Index.However, the test for the shelf-life is a very intractable job.Most of plate-making factory test layers of copper hardness shelf-life
Method is, a roller is plated under its current manufacturing condition, tests the change of hardness observation numerical value daily to determine to guarantee the quality
Phase, although this method can accurately determine the shelf-life, test period is long, it is impossible to adapts to wanting for modern industrial process
Ask.
The content of the invention
The technical problem to be solved in the present invention is the defects of being directed to prior art, there is provided one kind can be determined rapidly and accurately
Holding phase, the method simple to operate that the copper plate hardness shelf-life is tested using square Hull cell.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:One kind utilizes the test copper facing of square Hull cell
The method of layer hardness shelf-life, it is characterised in that:Carry out according to the following steps,
1), sample, before sampling, be first sufficiently stirred plating solution, and plating solution is sampled from the different parts of coating bath, make after mixing
With;
2), test piece is handled, and the overlay film that test piece needs plating one side is removed, using 3000# fine sandpapers or scouring pad along one
Individual direction polishes stainless steel test piece totally, standby;Electroplating surface is not touched after being disposed, in order to avoid being stained with greasy dirt, is caused
Coating bubbles;
3), the plating solution of sampling is inserted in square Hull cell, plating solution is heated to technological temperature during production, heating process
In, open air stirring or using mechanical agitation, electric current 4.5A;
4), test when, first by 500ml plating solutions be heated to than production when technological temperature it is high 2-3 DEG C, heat while
Stirring, avoids hot-spot from causing additive to decompose, and can not react the reset condition of plating solution after otherwise even cooling down comprehensively;
5), phosphorus-copper anode is inserted in the anode slot among square Hull cell, positive source is connected to phosphorus-copper anode, bears
Pole is connected to stainless test piece, tracheae insertion air pipe interface, the electricity of needs is inputted on power-supply controller of electric, and source current is revolved
Button adjusting is to minimum;
6), power-on and air pump, and electric current is progressively transferred to rated current, and opening time controller in time;
7), in test process, bath temperature situation of change is observed, if temperature is in rising trend in test process,
Anode is moved toward in the anode slot of negative electrode, so that tank voltage reduces, and reduces the caloric value of plating solution;If testing
During temperature it is on a declining curve, then anode so that tank voltage just raises, is improved toward moving in the anode slot away from negative electrode
The caloric value of plating solution, ensure that test temperature is consistent with normal technological temperature;
Because electroplating time is longer, the poor phosphorus-copper anode generation anode film of use quality is thicker, voltage can be caused to raise.
If voltage quickly raises, anode can be changed rapidly.
8), to the scheduled time, power supply is closed, test piece is taken out and rinses well, be put into 30-50g/L potassium bichromate solution
The 5-20 seconds are passivated, and should not be too high by the water stain drying of strip, temperature with hot hair dryer, otherwise easily oxidation, influences to survey
Test result;
9), test piece is put into boiling water, is kept for some minutes of seething with excitement, to the scheduled time after take out test piece, naturally cool to
Hardness is tested after room temperature, such repeated several times, selects point test hardness number different in test piece (minimum 5 tools of selection every time
Representational position), then average.
Further, the inside of the square Hull cell is provided with two pieces of dividing plates, centre will be separated into inside cell body respectively
Square tank house and the square fluid reservoir positioned at tank house both sides, some convection holes are provided with dividing plate by fluid reservoir and tank house phase
It is intercommunicated;Negative electrode slot and some anode slots are provided with tank house, negative electrode slot and anode slot are parallel to each other, and negative electrode is inserted
Enter in negative electrode slot, phosphorus-copper anode is inserted in a wherein anode slot.
Further, stirring stomata is provided with the bottom of tank house, stirring stomata passes through the inlet channel in cell body
Connected with air pipe interface, by tracheae toward inflating in tank house, and the stirring to plating solution is realized by stirring stomata outlet.
Further, the heating to plating solution is completed by being arranged on the heating rod of tank house bottom, can be facilitated plating solution
Technological temperature is risen to, to improve the degree of accuracy of test result.
Further, the test piece time to boil water is respectively 15 minutes, 30 minutes, 45 minutes and 60 minutes, after the completion of to boil water
Immediately the average hardness measured and time to boil water are contrasted with the hardness shelf-life table of comparisons.
Further, during electroplating experiments the temperature control of plating solution in the range of 38-40 DEG C.
Further, the test piece plating area of square Hull cell is 0.25dm2, current density 18A/dm2, so as to reach
4.5A electric current.
The present invention, as test equipment, corresponding survey is designed according to the characteristic of square Hull cell by using square Hull cell
Method for testing, the standard summarized on the basis of lot of experiments time to boil water and the hardness shelf-life table of comparisons are incorporated in, can quickly be tested
The hardness of copper plate is kept for the phase, has the characteristics of easy to operate, speed is fast, the degree of accuracy is high.
Brief description of the drawings
Fig. 1 is the square Hull cell dimensional structure diagram that the present invention uses;
Fig. 2 is the square Hull cell schematic top plan view that the present invention uses.
In figure, 1 is cell body, and 2 be negative electrode slot, and 3 be stirring stomata, and 4 be thermometer, and 5 be fluid reservoir, and 6 be anode slot,
7 be heating rod, and 8 be air pipe interface, and 9 be convection holes, and 10 be dividing plate, and 11 be tank house.
Embodiment
In the present embodiment, referring to Figures 1 and 2, the method that the copper plate hardness shelf-life is tested using square Hull cell,
Carry out according to the following steps,
1), sample, before sampling, be first sufficiently stirred plating solution, and plating solution is sampled from the different parts of coating bath, make after mixing
With;
2), test piece is handled, and the overlay film that test piece needs plating one side is removed, using 3000# fine sandpapers or scouring pad along one
Individual direction polishes stainless steel test piece totally, standby;Electroplating surface is not touched after being disposed, in order to avoid being stained with greasy dirt, is caused
Coating bubbles;
3), the plating solution of sampling is inserted in square Hull cell, plating solution is heated to technological temperature during production, heating process
In, open air stirring or using mechanical agitation, electric current 4.5A;
4), test when, first by 500ml plating solutions be heated to than production when technological temperature it is high 2-3 DEG C, heat while
Stirring, avoids hot-spot from causing additive to decompose, and can not react the reset condition of plating solution after otherwise even cooling down comprehensively;
5), phosphorus-copper anode is inserted in the anode slot among square Hull cell, positive source is connected to phosphorus-copper anode, bears
Pole is connected to stainless test piece, tracheae insertion air pipe interface, the electricity of needs is inputted on power-supply controller of electric, and source current is revolved
Button adjusting is to minimum;
6), power-on and air pump, and electric current is progressively transferred to rated current, and opening time controller in time;
7), in test process, bath temperature situation of change is observed, if temperature is in rising trend in test process,
Anode is moved toward in the anode slot of negative electrode, so that tank voltage reduces, and reduces the caloric value of plating solution;If testing
During temperature it is on a declining curve, then anode so that tank voltage just raises, is improved toward moving in the anode slot away from negative electrode
The caloric value of plating solution, ensure that test temperature is consistent with normal technological temperature;
Because electroplating time is longer, the poor phosphorus-copper anode generation anode film of use quality is thicker, voltage can be caused to raise.
If voltage quickly raises, anode can be changed rapidly.
8), to the scheduled time, power supply is closed, test piece is taken out and rinses well, be put into 30-50g/L potassium bichromate solution
The 5-20 seconds are passivated, and should not be too high by the water stain drying of strip, temperature with hot hair dryer, otherwise easily oxidation, influences to survey
Test result;
9), test piece is put into boiling water, is kept for some minutes of seething with excitement, to the scheduled time after take out test piece, naturally cool to
Hardness is tested after room temperature, such repeated several times, selects point test hardness number different in test piece (minimum 5 tools of selection every time
Representational position), then average.
And square Hull cell includes cell body 1, cell body 1 is square structure, by the dividing plate 10 of left and right two by cell body 1 in it
Part is divided into the tank house 11 of centre and the fluid reservoir 5 positioned at the both sides of tank house 11, and some convection holes 9 will be provided with dividing plate 10 to be stored up
Liquid room 5 is interconnected with tank house 11, and in the course of work, the plating solution in tank house 11 can generate heat in electric current after, density meeting
Change, can be swapped by the convection holes 9 on dividing plate 10 with the plating solution in fluid reservoir 5;Inserted in tank house 10 provided with negative electrode
Groove 2 and some anode slots 6, negative electrode slot 2 and anode slot 6 are parallel to each other, and negative electrode (test piece) is inserted in negative electrode slot 2,
Phosphorus-copper anode is inserted in a wherein anode slot 6.
Stirring stomata 3 is provided with the bottom of tank house 11, stirring stomata 3 passes through the inlet channel and gas in cell body 1
Interface tube 8 connects, and by tracheae toward inflation in tank house 11, and realizes the stirring to plating solution by the outlet of stirring stomata 3.
Heating rod 7 is provided with the bottom of tank house 11, the heating to plating solution is completed by heating rod 7, will conveniently can be plated
Liquid rises to technological temperature, to improve the degree of accuracy of test result.
Thermometer 4 can be set at dividing plate 10, thermometer 4 can so react the change of bath temperature conscientiously close to plating solution
Change, reduce inertia.
Cell body 1 is made of transparent PVC material, anticorrosion, resistance to conventional plating process temperature;Block dividing plate 10 is mutually flat
OK, the tank house 11 and fluid reservoir 5 being divided into are square structure.
The test piece time to boil water is respectively 15 minutes, 30 minutes, 45 minutes and 60 minutes, will be measured immediately after the completion of to boil water
Average hardness and the time to boil water contrasted with the hardness shelf-life table of comparisons.Time to boil water and the hardness shelf-life table of comparisons are as follows
Table:
The temperature control of plating solution is in the range of 38-40 DEG C during electroplating experiments.
The test piece plating area of square Hull cell is 0.25dm2, current density 18A/dm2, so as to reach 4.5A electricity
Stream.
The present invention is described in detail above, described above, only the preferred embodiments of the invention, when can not
Limit the scope of the present invention, i.e., it is all to make equivalent changes and modifications according to the application scope, it all should still belong to covering scope of the present invention
It is interior.