CN101481809A - Method for controlling electroforming velocity of nickel by pulse parameter - Google Patents
Method for controlling electroforming velocity of nickel by pulse parameter Download PDFInfo
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- CN101481809A CN101481809A CNA2008102467060A CN200810246706A CN101481809A CN 101481809 A CN101481809 A CN 101481809A CN A2008102467060 A CNA2008102467060 A CN A2008102467060A CN 200810246706 A CN200810246706 A CN 200810246706A CN 101481809 A CN101481809 A CN 101481809A
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Abstract
The invention relates to a method for controlling the electroforming speed of nickel by pulse parameters, belonging to the electroforming preparation field. The electroforming speed of a clad layer is freely controlled by regulating the parameters of impulse current. In the method, the electroforming speed is calculated by steps such as distributing electroforming solutions-cathode material, electrolytic nickel anode pretreatment-electroforming-cathode demoulding-quality measurement and the like. The electroforming speed is the added value of the thickness of the clad layer in a certain time. As the quality equals to the cathode area*the thickness of the clad layer*the density of the clad layer, the area and the density are known; therefore, the thickness of the clad layer can be figured out; and finally the electroforming speed can be obtained by the thickness of the clad layer divided by the time used by the electroforming. The method has the advantages that the influence of the pulse parameters on the electroforming speed of the cast layer of the nickel is found out; the thickness of the cast layer of the nickel can be conveniently controlled by regulating the pulse parameters and time.
Description
Technical field
The invention belongs to the electroforming preparation field, a kind of method of the time control cast layer electroforming velocity for preparing the pure nickel cast layer in the single nickel salt electroforming solution is provided, can freely control the electroforming velocity of cast layer by the parameter of adjusting pulsed current.
Background technology
China has also had the history of five more than ten years in research aspect the plating, has also obtained more achievement in research for electroplating technology, but for the research of electroforming then the time very short, also do not carry out careful research for a lot of problems in the electroforming field.In China, the pulse galvanoplastics was risen gradually from the nineties.In general, the pulse electroforming is than the common good cast layer of the easier obtained performance of direct current electroforming.The direct current electroforming has only a strength of current parameter to regulate, and pulsed electrical is cast with electric current, pulse-repetition, three customized parameters of dutycycle, the bidirectional pulse adjustable parameter is more, thereby can regulate processing parameter more flexible and changeablely, to obtain better tissue and performance.
The research of paired pulses electroforming is more rare, and also the no one furthers investigate the influence of the variation of extra pulse parameter to electroforming velocity.For electroforming rather than plating, the electroforming velocity Research Significance is very big, often require in the production electroformed layer very thick, require electroforming velocity very fast, can obtain our desired cast layer thickness by the research of electroforming velocity accurately being controlled electroforming parameter and time, also can understand how to accelerate electroforming velocity by it.
Through a large amount of tests, various parameters changed the rule that influences to electroforming velocity when we had drawn a cover pulse electroformed nickel.
The patent of present domestic electroforming aspect is considerably less, yet there are no the patent of pulse electroformed nickel aspect.
Summary of the invention
Utilize the adjustment of pulse parameter to control the method for electroforming velocity when the object of the present invention is to provide a kind of electroformed nickel, solve the unmanageable problem of thickness of coating.
A kind of method of utilizing the electroforming velocity of pulse parameter control nickel, processing step is:
(1) joins electroforming solution: the deionized water that in the electrotyping bath that cleans up with deionized water, adds electrotyping bath volume about 1/2, be heated to 45-55 ℃, insulation 1-2h, in electrotyping bath, add 250-450g/L six hydration nickel sulfate, 25-65g/L nickelous chloride successively, 0.1-10g/L asccharin, or replace the asccharin of prescription in one jointly with N-501A and two kinds of additives of N-501B, and the concentration of N-501A is 2-10mL/L, the concentration of N-501B is 0.5-4mL/L.
The deionized water that adds electrotyping bath volume 1/5-2/5 again in the Glass Containers that cleans up with deionized water, be stirred and heated to boiling, add 25-65g/L boric acid and boil 20-40min, add the 0.05-1g/L sodium lauryl sulphate then, after treating that sodium lauryl sulphate is fully dissolved, the liquid for preparing in the Glass Containers is poured in the electrotyping bath.The deionized water that reinjects is filled it up with electrotyping bath.Fully stir, be incubated 1-14h at 45-55 ℃.
(2) cathode material, the pre-treatment of electrolytic nickel anode: the negative electrode stainless steel plate is through 200#, 400#, 600#, 800#, 1000# silicon carbide waterproof abrasive paper polishing → deionization washing → nitric acid passivation → deionization washing → drying; The electrolytic nickel anode cleans in boiling water → deionization washing → hydrochloric acid activation → deionization washing with brush.
(3) electroforming: the sulphuric acid soln with 3-8% is regulated pH=3.5-5, and anode electrolysis nickel plate is put into the anode basket and connected circuit, regulates current density 1-10A/dm
2, regulating the positive negative sense dutycycle of bidirectional pulse electric current, the dutycycle in electric current dead band, the frequency 100-5000 of regulating impulse keeps the negative electrode maximum current density constant, carries out electroforming 3-80h.
(4) the negative electrode demoulding: the demoulding → deionization washing → drying.
(5) measure quality: the electroform product that obtains under various electroforming process high-precision electronic balance measurement quality.
(6) calculate electroforming velocity: electroforming velocity is the increased value of thickness of coating in certain hour just.Because quality=cathode area * thickness of coating * coating density, area and density are known, so can calculate thickness of coating (if directly measuring thickness of coating then error ratio is bigger with vernier callipers).Can try to achieve electroforming velocity with thickness of coating divided by the used time of electroforming at last, the result is accurate to behind the radix point 4.
Find after deliberation, utilizing unidirectional or during bidirectional pulse technology electroformed nickel, pulse parameter and electroforming velocity have following relation:
(1) as seen from Figure 2, when the unidirectional pulse electroformed nickel,,, dutycycle constantly increases along with increasing electroforming velocity when prescription, frequency, when maximum cathode current density processing condition are constant.
(2) as can be seen, when the unidirectional pulse electroformed nickel, when prescription, dutycycle, when maximum cathode current density processing condition are constant, do not have evident regularity between electroforming velocity and the frequency by Fig. 3,4.
(3) as seen from Figure 5, when the unidirectional pulse electroformed nickel, when prescription, dutycycle, when the frequency processing condition are constant, along with the increase electroforming velocity of maximum cathode current density constantly increases.
(4) as seen from Figure 6, when the bidirectional pulse electroformed nickel, when prescription, frequency, maximum cathode current density, when negative-going pulse dutycycle processing condition are constant, along with the increase electroforming velocity of direct impulse dutycycle constantly increases.
By processing parameters such as control prescription, frequency, dutycycle, maximum cathode current density, can control electroforming velocity.
The invention has the advantages that: found the influence rule of pulse parameter, aborning can be easily control the thickness of nickel cast layer by adjusting pulse parameter and time to the electroforming velocity of nickel.
Description of drawings
Fig. 1 is the interior oscillogram of single cycle of bidirectional pulse electric current.
A1%+a2%+a3%+a4%=100%, 100% is exactly a recurrence interval, and a1 is the direct impulse interval, and a3 is the reverse impulse interval, and a2 and a4 are that the dead band is that electric current is zero zone.Being dc waveform when a1=100, is the bidirectional pulse waveform when 0＜a1, a3＜100, is unidirectional pulse when 0＜a1＜100 and a3=0.The length in each cycle equals 1/f, and f is a frequency.Maximum cathode current density Y=Imax/ cathode area.
Fig. 2 is the graph of a relation of two kinds of prescriptions electroforming velocity and dutycycle when the unidirectional pulse electroforming.
Fig. 3 is the graph of a relation of prescription one electroforming velocity and frequency when the unidirectional pulse electroforming.
Fig. 4 is the graph of a relation of prescription two electroforming velocity and frequency when the unidirectional pulse electroforming.
Fig. 5 is the graph of a relation of two kinds of prescriptions electroforming velocity and maximum cathode current density when the unidirectional pulse electroforming.
Fig. 6 is the graph of a relation of two kinds of prescriptions electroforming velocity and dutycycle when the bidirectional pulse electroforming.
Embodiment
Embodiment 1,
1. single nickel salt electroforming solution preparation: the volume that calculates electrotyping bath earlier, the concentration that multiply by single nickel salt, nickelous chloride, asccharin, sodium lauryl sulphate, boric acid with volume obtains required drug weight respectively, electrotyping bath adds 1/3-2/3 volumetrical deionized water, be heated to 45-55 ℃, add all required single nickel salt, nickelous chloride, asccharin successively, stir and insulation 1-2h.Other gets 1000mL beaker deionized water rinsing, drying, add the 200-400mL deionized water, be stirred and heated to boiling, add required boric acid and boil half an hour, add required sodium lauryl sulphate then, after treating that sodium lauryl sulphate is fully dissolved, it is slowly poured in the six hydration nickel sulfate solution, add deionized water again to the electrotyping bath volume.Fully stir, at 45-55 ℃ of insulation 1-14h.
2. the pre-treatment of negative electrode, anode material: used negative electrode stainless steel plate is polished with 200#, 400#, 600#, 800#, 1000# silicon carbide waterproof abrasive paper, rinse well with deionized water, put into concentrated nitric acid and carried out surface passivation in 10 minutes, and then wash with deionized water, dry then.Anode electrolysis nickel plate with the careful clean surface of toothbrush, is put into sheet nickel hydrochloric acid then and made its surface active in 15 minutes, use washed with de-ionized water then.
3. electroforming: the sulphuric acid soln with 5% is regulated pH=3.5-5, then the negative electrode stainless steel plate source negative pole that Connects Power, with electric adhesive tape non-electroforming zone on the steel plate is clung, anode electrolysis nickel plate is put into the anode basket and connected circuit, the adjusting current density is 1-10A/dm
2, mix up required pulse parameter and frequency, electroforming 3-80h.
4. the demoulding: take out negative electrode and carry out the demoulding, to gained electroformed nickel sample clean, drying.
5. measurement quality: the electroform product that obtains under the various electroforming process with high-precision electronic balance measurement quality, is accurate to 2 significant digits.
6. calculating electroforming velocity: electroforming velocity is the increased value of thickness of coating in certain hour just.With quality divided by cathode area (40cm
2) again divided by density (8.9g/cm
3) can calculate thickness of coating, be scaled a millimeter unit, can try to achieve electroforming velocity with thickness of coating divided by the used time of electroforming (min of unit), the unit of electroforming velocity is mm/min, mapping for convenience enlarges 1000 times to data, obtain the increased value of the thickness in 1000 minutes, be accurate to behind the radix point 4, electroforming velocity unit becomes mm/1000min.
Embodiment 2,
Change a kind of prescription, (this is two kinds of additive trades mark of Wuhan sail electroplating additive company with N-501A and N-501B, N-501A is the agent that walks, N-501B is a brightening agent) these two kinds of additives replace the asccharin of prescription in one jointly, the concentration of N-501A is 2-10mL/L, the concentration of N-501B is 0.5-4mL/L, utilize with the identical processing condition of filling a prescription and test once more, obtain similar electroforming velocity rule, can control the thickness of nickel cast layer aborning easily by adjustment pulse parameter and time.
Claims (1)
1. method of utilizing the electroforming velocity of pulse parameter control nickel is characterized in that the technology that the electroforming nickel dam uses is:
(1) joins electroforming solution: the deionized water that in the electrotyping bath that cleans up with deionized water, adds electrotyping bath volume about 1/2, be heated to 45-55 ℃, insulation 1-2h, in electrotyping bath, add 250-450g/L six hydration nickel sulfate, 25-65g/L nickelous chloride successively, 0.1-10g/L asccharin, or replace the asccharin of prescription in one jointly with N-501A and two kinds of additives of N-501B, and the concentration of N-501A is 2-10mL/L, the concentration of N-501B is 0.5-4mL/L;
The deionized water that adds electrotyping bath volume 1/5-2/5 again in the Glass Containers that cleans up with deionized water, be stirred and heated to boiling, add 25-65g/L boric acid and boil 20-40min, add the 0.05-1g/L sodium lauryl sulphate then, after treating that sodium lauryl sulphate is fully dissolved, the liquid for preparing in the Glass Containers is poured in the electrotyping bath, and the deionized water that reinjects is filled it up with electrotyping bath, fully stirs, is incubated 1-14h at 45-55 ℃;
(2) cathode material, the pre-treatment of electrolytic nickel anode: the negative electrode stainless steel plate is through 200#, 400#, 600#, 800#, 1000# silicon carbide waterproof abrasive paper polishing → deionization washing → nitric acid passivation → deionization washing → drying; The electrolytic nickel anode cleans in boiling water → deionization washing → hydrochloric acid activation → deionization washing with brush;
(3) electroforming: the sulphuric acid soln with 3-8% is regulated pH=3.5-5, and anode electrolysis nickel plate is put into the anode basket and connected circuit, regulates current density 1-10A/dm
2, regulating the positive negative sense dutycycle of bidirectional pulse electric current, the dutycycle in electric current dead band, the frequency 100-5000 of regulating impulse keeps the negative electrode maximum current density constant, carries out electroforming 3-80h;
(4) the negative electrode demoulding: the demoulding → deionization washing → drying;
(5) measure quality: the electroform product that obtains under various electroforming process high-precision electronic balance measurement quality;
(6) calculate electroforming velocity: electroforming velocity is the increased value of thickness of coating in certain hour just; Because quality=cathode area * thickness of coating * coating density, area and density are known, so can calculate thickness of coating, can try to achieve electroforming velocity with thickness of coating divided by the used time of electroforming at last;
Finding after deliberation has following relation between the electroforming velocity of cast layer and pulse parameter:
(1) with the unidirectional pulse electroformed nickel time, when prescription, frequency, when maximum cathode current density processing condition are constant, improve the duty specific energy and improve electroforming velocity;
(2) when the unidirectional pulse electroformed nickel, electroforming velocity is not subjected to frequency influence;
(3) when the unidirectional pulse electroformed nickel,, improve maximum cathode current density and can improve electroforming velocity when prescription, dutycycle, when the frequency processing condition are constant;
(4) when using the bidirectional pulse electroformed nickel, when prescription, frequency, maximum cathode current density, when negative-going pulse dutycycle processing condition are constant, improve direct impulse duty specific energy and improve electroforming velocity.
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| CNA2008102467060A CN101481809A (en) | 2008-12-30 | 2008-12-30 | Method for controlling electroforming velocity of nickel by pulse parameter |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556192A (en) * | 2013-10-09 | 2014-02-05 | 北京航空航天大学 | Method for preparing electroformed nickel layer with high mechanical properties by using bidirectional pulse power supply |
| CN109943872A (en) * | 2019-04-11 | 2019-06-28 | 广西大学 | It is a kind of for melting the preparation method for the composite coating that stainless steel containing Cr in fluoride salt protects |
| CN110158120A (en) * | 2019-05-28 | 2019-08-23 | 合肥铜冠国轩铜材有限公司 | Foil machine on-line monitoring system and its monitoring method |
| CN113502510A (en) * | 2021-06-07 | 2021-10-15 | 北京保利微芯科技有限公司 | Manufacturing method of integrated micro-column array metal mold and metal mold thereof |
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2008
- 2008-12-30 CN CNA2008102467060A patent/CN101481809A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556192A (en) * | 2013-10-09 | 2014-02-05 | 北京航空航天大学 | Method for preparing electroformed nickel layer with high mechanical properties by using bidirectional pulse power supply |
| CN103556192B (en) * | 2013-10-09 | 2016-03-30 | 北京航空航天大学 | A kind of bidirectional pulse power supply that adopts prepares the method with strong mechanical performance electroforming nickel dam |
| CN109943872A (en) * | 2019-04-11 | 2019-06-28 | 广西大学 | It is a kind of for melting the preparation method for the composite coating that stainless steel containing Cr in fluoride salt protects |
| CN110158120A (en) * | 2019-05-28 | 2019-08-23 | 合肥铜冠国轩铜材有限公司 | Foil machine on-line monitoring system and its monitoring method |
| CN110158120B (en) * | 2019-05-28 | 2021-12-17 | 合肥铜冠电子铜箔有限公司 | Online monitoring system and method for foil forming machine |
| CN113502510A (en) * | 2021-06-07 | 2021-10-15 | 北京保利微芯科技有限公司 | Manufacturing method of integrated micro-column array metal mold and metal mold thereof |
| CN113502510B (en) * | 2021-06-07 | 2024-02-02 | 北京保利微芯科技有限公司 | Manufacturing method of integrated micro-column array metal mold and metal mold thereof |
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Open date: 20090715 |