CN105628755A - Method for detecting plating uniformity of plating solution in double-anode mode - Google Patents
Method for detecting plating uniformity of plating solution in double-anode mode Download PDFInfo
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Abstract
The invention discloses a method for detecting plating uniformity of a plating solution in a double-anode mode. According to the method, the plating solution is detected through two anode electrodes of different areas and a cathode electrode; different currents generated by the same cathode electrode and the anode electrodes of different areas are detected respectively under the cathode electrode, wherein the smaller the current difference is, the better the plating uniformity of the plating solution is. The method can be used for the aspect of additive qualitative analysis of the plating solution and the like. The ratio of the specific area of the small anode to the specific area of the large anode is 1:5 to 1:200. The surface area of the small anode is 5-20 times of the surface area of the cathode. The position of the cathode electrode is opposite to the positions of the two anode electrodes. The two anode electrodes are in the same direction. According to the method, information of the plating uniformity of the plating solution is obtained through the two anodes of different areas and the same cathode under different currents, the method is rapid, effective, easy and convenient to use and feasible, and cost can be reduced.
Description
Technical field
The present invention relates to a kind of detection method, specifically, it relates to the method for the equal plating property of a kind of double anode detection plating liquid.
Background technology
In electroplating process, plated item is placed in negative electrode. Due to the effect of the factors such as plating piece shape, plating piece position, the different positions plating speed of different plating piece is had any different. Usually it is desirable that this kind of difference is the smaller the better. The index weighing this performance is called as all platings of plating liquid, is called for short COP.
COP is required higher by electronics finishing. Because the density that design reasons needs the lines of plating, convex point etc. has very big gap often, and electronics finishing is very strict to the requirement of thickness of coating homogeneity. Therefore the COP performance of plating liquid is one of salient features index of electronics finishing liquid.
Present detection method is production standard sheet with photoresist on silicon chip, measures after plating, to determine to plate the COP performance of liquid. The method and production technique are close, good reliability, are applicable to using the supplied materials detection of producer. But cost height, speed is slow, inadaptable plating liquid R&D work. Urgently need to improve.
Summary of the invention
It is an object of the invention to provide a kind of method of COP performance for detecting plating liquid, can fast and effeciently detect while the electrode area of restriction anode.
In order to achieve the above object, the present invention provides the method for a kind of double anode detection plating equal plating property of liquid, and wherein, the method adopts the anode electrode of two different area and a cathode electrode to be detected by plating liquid; Detecting the different electric currents that it produces from different area anode electrode under same cathode electrode respectively, electric current gap is more little, and all platings of plating liquid are more good.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described anode electrode, the surface-area of primary anode and big anode is than being 1:5 ~ 1:200.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described primary anode surface-area is the 1/10 ~ 1 of cathodic surface area.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described big anode surface area is 5 ~ 20 times of cathodic surface area.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described electrode position is fixed, and two anode electrodes are less than 1:1.2 to the ratio of distances constant of cathode electrode.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described cathode electrode is relative with the position of two anode electrodes, and two described anode electrodes are in the same way. The position of cathode electrode and two anode electrodes generally has three kinds: in the same way, its Detection results is worst for anode and cathode; Anode and cathode is vertical, and it has certain Detection results; Anode and cathode is relative, and its Detection results is best.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described anode electrode is noble electrode or non-inert electrode, needs cleaning anode electrode surface when detecting different plating liquid. Concrete cleaning solution to be groped to determine according to type of electrodes and sort of plating solution. Preferably, adopting a ultrapure water to clean, twice polishing, once once uses polishing powder with sand paper. Lose liquid with copper every day and process 1 minute.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described cathode electrode is noble electrode, needs cleaning cathode electrode surface when detecting different plating liquid; Concrete cleaning solution to be groped to determine according to type of electrodes and sort of plating solution. Preferably, adopt cold concentrated nitric acid to soak 3 minutes, after cleaning, clean 5 minutes with 5%, 0.6 volt, sulfuric acid 75%-hydrogen peroxide. But need to determine according to additive types, as additive adsorptivity is not bery strong, it is possible to simpler. Described cathode electrode adopts rotating electrode, and when detecting, rotating speed is higher than 50 revs/min. Adopting other whipped form data stability poor, stir as cancelled, data and actual plating liquid COP gap are big.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described bath temperature is stablized, and in testing process, temperature variation is less than less than 1 DEG C.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described method adopts potentiostatic method or CV curve method detection data to be processed; Described potentiostatic method is under identical potential condition, relatively different anode electrode and same cathode electrode, the total electricity passed through within the identical time, and all plating property is more good for the more little plating liquid of total electricity gap; Described CV curve method draws the different anode electrode CV curve different with same cathode electrode, draws the current ratio of different anode electrode, and all plating property is more good for the more little plating liquid of electric current gap. The data processing of potentiostatic method is simple, and the information of CV curve method is more.
The method of the equal plating property of above-mentioned double anode detection plating liquid, wherein, described method can also be used for plating the aspects such as the additive qualitative analysis of liquid.
The method of the double anode provided by the invention detection plating equal plating property of liquid has the following advantages:
The present invention provides a kind of special detection method, it is possible to the COP performance of detection plating liquid fast, the electrode area of restriction anode, and utilizes the anode of two different area. By detecting the electric current of different area anode, obtain the information of plating liquid COP performance. In traditional detection, detecting electrode is negative electrode. For ensureing the repeatability that electrode data is good, meeting matching standard electrode usually, thus need to provide enough big annode area. And in the method, cancel standard electrode and reduce annode area, make the electrode area of anode relevant with the electrochemical data of plating liquid. The anode utilizing two areas different, obtains the COP information of plating liquid by the different electric current under same negative electrode, fast effectively, simple and easy to do, and can reduce costs.
Accompanying drawing explanation
Fig. 1 be the double anode detection plating equal plating property of liquid method in the schematic diagram of the identical setting of electrode direction.
Fig. 2 be the double anode detection plating equal plating property of liquid method in the vertically disposed schematic diagram of electrode direction.
Fig. 3 be the double anode detection plating equal plating property of liquid of the present invention method in the schematic diagram that is oppositely arranged of electrode direction.
Fig. 4 be the double anode detection plating equal plating property of liquid of the present invention method in potentiostatic method data plot.
Fig. 5 be the double anode detection plating equal plating property of liquid of the present invention method in CV graphic representation.
Fig. 6 be the double anode detection plating equal plating property of liquid of the present invention method in the CV graphic representation of two anodes.
Fig. 7 be the double anode detection plating equal plating property of liquid of the present invention method in CV graphic representation after process.
Fig. 8 be the double anode detection plating equal plating property of liquid of the present invention method in the COP figure that draws of CV curve method.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is further described.
The method of the double anode provided by the invention detection plating equal plating property of liquid, wherein, the method adopts the anode electrode of two different area and a cathode electrode to be detected by plating liquid; Detecting the different electric currents that it produces from different area anode electrode under same cathode electrode respectively, electric current gap is more little, and all platings of plating liquid are more good. The method can also be used for plating the aspects such as the additive qualitative analysis of liquid.
Bath temperature needs to keep stable, and in testing process, temperature variation is less than less than 1 DEG C.
In two anode electrodes, the surface-area of primary anode and big anode is than being 1:5 ~ 1:200. Primary anode surface-area is the 1/10 ~ 1 of cathodic surface area. Big anode surface area is 5 ~ 20 times of cathodic surface area.
Electrode position is fixed, and two anode electrodes are less than 1:1.2 to the ratio of distances constant of cathode electrode.
Cathode electrode is relative with the position of two anode electrodes, and two anode electrodes are in the same way. The position of cathode electrode and two anode electrodes generally has three kinds: in the same way, its Detection results is worst, shown in Figure 1 for anode and cathode; Anode and cathode is vertical, and it has certain Detection results, shown in Figure 2; Anode and cathode is relative, and its Detection results is best, shown in Figure 3.
Anode electrode is noble electrode or non-inert electrode, needs cleaning anode electrode surface when detecting different plating liquid. Concrete cleaning solution to be groped to determine according to type of electrodes and sort of plating solution. Preferably, adopting a ultrapure water to clean, twice polishing, once once uses polishing powder with sand paper. Lose liquid with copper every day and process 1 minute.
Cathode electrode is noble electrode, needs cleaning cathode electrode surface when detecting different plating liquid; Concrete cleaning solution to be groped to determine according to type of electrodes and sort of plating solution. Preferably, adopt cold concentrated nitric acid to soak 3 minutes, after cleaning, clean 5 minutes with 5%, 0.6 volt, sulfuric acid 75%-hydrogen peroxide. But need to determine according to additive types, as additive adsorptivity is not bery strong, it is possible to simpler. Cathode electrode adopts rotating electrode, and when detecting, rotating speed is higher than 50 revs/min. Preferably, the rotating speed adopting rotating electrode to stir is 1000 revs/min. Adopting other whipped form data stability poor, stir as cancelled, data and actual plating liquid COP gap are big.
The method can adopt potentiostatic method or CV curve method detection data to be processed.
Potentiostatic method is under identical potential condition, relatively different anode electrode and same cathode electrode, the total electricity passed through within the identical time, and all plating property is more good for the more little plating liquid of total electricity gap. CV curve method draws the different anode electrode CV curve different with same cathode electrode, draws the current ratio of different anode electrode, and all plating property is more good for the more little plating liquid of electric current gap. The data processing of potentiostatic method is simple, and the information of CV curve method is more.
By the following examples embodiments of the present invention are described in detail.
Embodiment 1
Anode electrode and a cathode electrode of two different area is adopted to be detected by plating liquid; The different electric currents that it produces from different area anode electrode are detected respectively under same cathode electrode.
The surface-area of primary anode and big anode is than being 1:10. Primary anode surface-area is equal with cathodic surface area. Big anode surface area is 10 times of cathodic surface area.
Electrode position is fixed, and two anode electrodes are 1:1.1 to the ratio of distances constant of cathode electrode.
Cathode electrode is relative with the position of two anode electrodes, and two anode electrodes are in the same way.
Anode electrode is non-inert electrode, needs cleaning anode electrode surface when detecting different plating liquid. Adopting a ultrapure water to clean, twice polishing, once once uses polishing powder with sand paper. Lose liquid with copper every day and process 1 minute.
Cathode electrode is noble electrode, needs cleaning cathode electrode surface when detecting different plating liquid; Adopt cold concentrated nitric acid to soak 3 minutes, after cleaning, clean 5 minutes with 5%, 0.6 volt, sulfuric acid 75%-hydrogen peroxide.
Cathode electrode adopts rotating electrode, and the rotating speed adopting rotating electrode to stir is 1000 revs/min.
Plating liquid adopts the low acid ultrapure copper electrolyte of VMS of the low copper containing 40ppm trimethyl-glycine.
Adopting potentiostatic method detection data to be processed, result is shown in Figure 4.
Under identical potential condition, relatively different anode and same negative electrode, the total comparision of quantity of electricity passed through within the identical time. Total electric quantity change is smaller is good. The concrete value of electropotential is scaled and obtain by concrete plating condition, with simulated field as far as possible. Certainly value can also obtain data arbitrarily. And have certain guidance meaning.
Embodiment 2
The surface-area of primary anode and big anode is than being 1:30. Primary anode surface-area is the 1/2 of cathodic surface area. Big anode surface area is 15 times of cathodic surface area.
Electrode position is fixed, and two anode electrodes are 1:1.2 to the ratio of distances constant of cathode electrode.
Testing process is identical with above-described embodiment 1.
Adopting CV curve method detection data to be processed, result is shown in Figure 5.
Draw the CV curve that different anode is different with same negative electrode, then utilize the instruments such as Excel to process. The comparison of two anodes is shown in Figure 6.
CV graphic representation after Excel process is as shown in Figure 7.
COP after process and size anodic current are than the graphic representation relative to electropotential as shown in Figure 8.
The ratio available potential condition can be compared from the COP figure of difference plating liquid, thus draw the COP character quality of different plating liquid. Available current potential is calculated by concrete electroplating technique condition to be determined, the COP numerical value under other potential condition, only Research Significance is without actual meaning.
Different according to ratio diagram shape, it is possible to the additive types added in conjecture plating liquid. Portions additive can produce specified shape by correlative value figure.
Embodiment 3 ~ 41
Research cathode electrode difference stirs rotation mode, and electrode position arranges the impact on detected result.
Two kinds of plating liquid A and B, all adopt common magnetic agitation, and result is as shown in table 1. Can finding out that data fluctuations is big, namely all degree of plating liquid of the same race are bigger than gap.
Table 1: the data using magnetic agitation.
Adopting rotating-disk, and secure electrode position, in the same way, result is as shown in table 2 for electrode direction.
Visual data fluctuation reduces, and namely all degree of plating liquid of the same race reduce than gap, but A, B plating liquid difference is not obvious.
Wherein, the surface-area of primary anode and big anode is than being 1:120. Primary anode surface-area is the 1/10 of cathodic surface area. Big anode surface area is 12 times of cathodic surface area.
Table 2: the data using rotating-disk.
Electrode direction being set to vertically, result is as shown in table 3. Comparing in the same way with electrode direction, all platings of identical plating liquid are less than fluctuation, and all platings of different plating liquid are bigger than difference.
Table 3: the vertically disposed data of electrode.
Electrode direction being set to relatively, effect is best, and result is as shown in table 4. Electrode position is fixed, and two anode electrodes are equal to the distance of cathode electrode. Therefrom distinguishing the COP of different plating liquid, the COP fluctuation ratio plating liquid B of plating liquid A is little, therefore plates liquid A and is better than plating liquid B.
Table 4: the data that electrode is oppositely arranged.
The method of the double anode provided by the invention detection plating equal plating property of liquid, it is also possible to for assessment of additive add-on. For a kind of additive A-2, result is as shown in table 5. The add-on of additive A-2 can be preferably 8 ~ 12 (ml/L), and under this add-on, the COP fluctuation of plating liquid is minimum.
Table 5: additive add-on is on the impact of plating liquid COP.
The method can also for assessment of different additive, and for another two kinds of additive P-9 and C-62, result is as shown in table 6. Can find out that additive P-9 adds rear COP fluctuation and is greater than C-62.
Table 6: additive types is on the impact of plating liquid COP.
The method of the double anode provided by the invention detection plating equal plating property of liquid, cancels standard electrode and also reduces annode area, makes the electrode area of anode and plate the electrochemical data of liquid relevant. The anode utilizing two areas different, obtains the COP information of plating liquid by the different electric current under same negative electrode.
Although the content of the present invention has made detail by above preferred embodiment, but it should recognize that above-mentioned description is not considered as limitation of the present invention. After those skilled in the art have read foregoing, multiple amendment for the present invention and replacement will be all apparent. Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. the method for the equal plating property of double anode detection plating liquid, it is characterised in that, the method adopts the anode electrode of two different area and a cathode electrode to be detected by plating liquid; Detecting the different electric currents that it produces from different area anode electrode under same cathode electrode respectively, electric current gap is more little, and all platings of plating liquid are more good.
2. the method for the equal plating property of double anode detection plating liquid as claimed in claim 1, it is characterised in that, described anode electrode, the surface-area of primary anode and big anode is than being 1:5 ~ 1:200.
3. the method for the equal plating property of double anode detection plating liquid as claimed in claim 2, it is characterised in that, described primary anode surface-area is the 1/10 ~ 1 of cathodic surface area.
4. the method for the equal plating property of double anode detection plating liquid as claimed in claim 2, it is characterised in that, described big anode surface area is 5 ~ 20 times of cathodic surface area.
5. the method for the equal plating property of double anode detection plating liquid as claimed in claim 1, it is characterised in that, described electrode position is fixed, and two anode electrodes are less than 1:1.2 to the ratio of distances constant of cathode electrode.
6. the method for the equal plating property of double anode detection plating liquid as claimed in claim 5, it is characterised in that, described cathode electrode is relative with the position of two anode electrodes, and two described anode electrodes are in the same way.
7. the method for the equal plating property of double anode detection plating liquid as claimed in claim 6, it is characterised in that, described anode electrode is noble electrode or non-inert electrode, needs cleaning anode electrode surface when detecting different plating liquid.
8. the method for the equal plating property of double anode detection plating liquid as claimed in claim 6, it is characterised in that, described cathode electrode is noble electrode, needs cleaning cathode electrode surface when detecting different plating liquid; Described cathode electrode adopts rotating electrode, and when detecting, rotating speed is higher than 50 revs/min.
9. the method for the equal plating property of double anode detection plating liquid as claimed in claim 1, it is characterised in that, described bath temperature is stablized, and in testing process, temperature variation is less than less than 1 DEG C.
10. the method for the equal plating property of double anode detection plating liquid as claimed in claim 1, it is characterised in that, described method adopts potentiostatic method or CV curve method detection data to be processed; Described potentiostatic method is under identical potential condition, relatively different anode electrode and same cathode electrode, the total electricity passed through within the identical time, and all plating property is more good for the more little plating liquid of total electricity gap; Described CV curve method draws the different anode electrode CV curve different with same cathode electrode, draws the current ratio of different anode electrode, and all plating property is more good for the more little plating liquid of electric current gap.
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Cited By (1)
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| CN109030605A (en) * | 2018-08-30 | 2018-12-18 | 武汉钢铁有限公司 | The determination method of chrome plating surface metal chromium content height |
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