CN111650249B - Analysis method of electroplating leveling agent for filling through hole of IC carrier plate - Google Patents
Analysis method of electroplating leveling agent for filling through hole of IC carrier plate Download PDFInfo
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Abstract
The invention discloses an analysis method of an electroplating leveling agent for filling through holes of an IC carrier plate, which comprises the following steps: preparing a standard solution; preparing electrolyte; manufacturing a standard curve; verifying correction factors: placing the electrolyte below an electrode of the analyzer, placing a standard solution to an automatic sample inlet of the analyzer, obtaining the concentration of a leveling agent of the standard solution through the analyzer, and comparing the concentration with the concentration of the leveling agent of the standard solution; sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample on an automatic sample inlet of the analyzer, starting the analyzer for analysis, and recording a potential diagram. The potential difference is obvious, and the analysis result is stable.
Description
Technical Field
The invention relates to the field of leveling agent analysis, in particular to an analysis method of an electroplating leveling agent for filling through holes of an IC carrier plate.
Background
The Maidemar company develops a process for directly electroplating copper to fill the through holes of the IC carrier plate, and solves the problems that the holes of the traditional resin are not full, the resin and the copper layer are easy to separate, the thermal conductivity of the resin is not high, the components are increased, overload is easy to occur, and the like.
The main components of the copper electroplating liquid medicine comprise: copper sulfate, sulfuric acid, chloride ions, brightening agents, wetting agents and leveling agents.
The leveling agent influences the potential difference at the high and low positions, the concentration of the leveling agent is too high, the performance of the pulse electroplating process section can be insufficient, copper aggregation at the middle section of the hole is insufficient, and the subsequent process is influenced; the concentration of the leveler is too low, and copper on the upper layer of the hole is not flat enough during direct current plating, so that the through hole cannot be filled during plating, and therefore, the concentration of the leveler needs to be analyzed.
The traditional leveling agent analysis method mostly adopts a RC (Response Curve) mode, the basic components of the electrolyte are analyzed to have the same concentration as the bath solution, a corresponding standard curve is drawn by adding the leveling agent with the same concentration for 4-6 times, then the bath solution is returned, and the corresponding concentration is found on the standard curve. The disadvantage of this method is that the concentration of the additive is too high, which results in an analysis electrode that is not easy to clean, so that the contamination of the analysis liquid affects the analysis result, which is unstable, has poor reproducibility and a shortened electrode lifetime.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides an analysis method of an electroplating leveling agent for filling through holes of an IC carrier plate, and the analysis result is stable.
To achieve the above objective, an embodiment of the present application discloses an analysis method of an IC carrier board via-hole landfill electroplating leveling agent, including the following steps:
preparing a standard solution: adding a brightening agent, a wetting agent and a leveling agent into a base solution to obtain a mixed solution, and fixing the volume of the mixed solution to 100ml to obtain a standard sample;
preparing an electrolyte: the electrolyte comprises copper sulfate, sulfuric acid, chloride ions, a brightening agent and a wetting agent;
and (3) making a standard curve: placing the electrolyte below an electrode of the analyzer, placing a standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor;
verifying correction factors: placing the electrolyte below an electrode of the analyzer, placing a standard solution into an automatic sample inlet of the analyzer, obtaining the concentration of a leveling agent of the standard solution through the analyzer, comparing the concentration with the concentration of the leveling agent of the standard solution, and performing the next operation, wherein the error is within 1-10%; if the error exceeds 10%, repeating the steps to manufacture a standard curve;
sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample on an automatic sample inlet of the analyzer, starting the analyzer for analysis, and recording a potential diagram.
Preferably, the addition amount of the standard sample for determining the correction factor is 0.2ml each time, the addition times are 3-6 times, the starting point of the obtained standard curve is 1, and the ending point is 0.93.
Preferably, the base solution comprises a mixture of 75g/l copper sulfate, 230g/l sulfuric acid and 75ppm hydrochloric acid.
Preferably, the analyzer is a cyclic stripping analyzer.
Preferably, the electrodes of the analyzer comprise a platinum electrode, an auxiliary electrode and a reference electrode, wherein the reference electrode inner liquid of the platinum electrode is 3M potassium chloride solution, and the outer liquid is 1M potassium nitrate solution; the auxiliary electrode is a stainless steel electrode.
Preferably, the positive limit value of the analysis voltage of the analyzer is 1.625V.
Preferably, the negative limit of the analysis voltage of the analyzer is-0.175 to-0.3V.
Preferably, the working electrode rotation speed of the analyzer is 2600r/min.
The beneficial effects of the invention are as follows:
1. according to the invention, DT (Dilution Titration) mode is used for analysis, the analysis electrolyte is changed into low-concentration copper sulfate and additive, and the low-concentration copper and additive enable the electrode to be cleaned more easily, so that the service life of the electrode is prolonged, and the analysis cost is saved.
2. Compared with the traditional RC analysis mode, the DT analysis mode has the advantages that potential difference obtained in the analysis process is obvious, potential performance is stable, verification of correction factors is simpler and clearer, and reproducibility of analysis results is good.
3. The DT mode is insensitive to the influence of the operation environment, has wide application range of the operation temperature and the humidity, and is beneficial to the management and control of the factory site.
4. According to the invention, through the comparison test of the standard solution, the deviation between the analysis result and the standard value can be reduced to about 2% by adopting the DT analysis method, and the analysis result is stable, thereby being beneficial to the control of the leveler and further enabling the performance of the liquid medicine to be exerted to the optimal state.
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular description of preferred embodiments, as illustrated in the accompanying drawings.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a sample standard addition chart of example 1 of the present invention;
FIG. 2 is a graph of the electrical quantity of the sample test of example 1 of the present invention;
FIG. 3 is a sample standard addition chart of example 2 of the present invention;
FIG. 4 is a graph of the electrical test of the sample of example 2 of the present invention;
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it should be noted that the positional or positional relationship indicated by the terms such as "upper", "lower", "bottom", "inner", "outer", etc. are based on the positional or positional relationship shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first", "a second", etc. may include one or more of the feature, either explicitly or implicitly.
In order to achieve the above-mentioned object, the present invention provides an analysis method of a leveling agent for filling and plating through holes of an IC carrier, comprising the following steps:
preparing a standard solution: adding 1ml/l brightening agent, 30ml/l wetting agent and 1.5ml/l leveling agent into the basic solution to obtain a mixed solution, and fixing the volume of the mixed solution to 100ml to obtain a standard sample;
preparing an electrolyte: the electrolyte comprises 75g/l copper sulfate, 230g/l sulfuric acid, 75g/l chloride ion, 0.75ml/l brightening agent and 2.5ml/l wetting agent;
and (3) making a standard curve: placing the electrolyte below an electrode of the analyzer, placing a standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor;
verifying correction factors: placing the electrolyte below an electrode of the analyzer, placing a standard solution into an automatic sample inlet of the analyzer, obtaining the concentration of a leveling agent of the standard solution through the analyzer, comparing the concentration with the concentration of the leveling agent of the standard solution, and performing the next operation, wherein the error is within 1-10%; if the error exceeds 10%, repeating the steps to manufacture a standard curve;
sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample on an automatic sample inlet of the analyzer, starting the analyzer for analysis, and recording a potential diagram.
Example 1
Instrument and conditions:
CVS instrument: switzerland ten thousand full-automatic 894CVS analyzer;
working electrode: a platinum electrode;
electrode rotation speed: 2600 rpm;
an electrolyte;
operating temperature: 23 DEG C
Analyzing positive voltage: 1.625V;
negative voltage analysis: 0.175V;
the analysis step:
first electrode activation: before instrument analysis, a blank VMS solution is placed under the electrode, and electrode activation is carried out for 15 times, so that the potential difference of the electrode after two continuous activations is ensured to be less than 0.2%.
And (3) making a standard curve: and placing 20ml of electrolyte below an electrode of the analyzer, placing 5ml of standard solution at an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor.
Verifying correction factors: placing the 20ml electrolyte below an electrode of the analyzer, placing 5ml standard solution at an automatic sample inlet of the analyzer, obtaining the concentration of the leveling agent of one standard solution by the analyzer, wherein the concentration is 1.55ml/l, the concentration is 1.35-1.65ml/l, the error is 1-10%, and the next operation can be performed.
Sample analysis: and placing the 20ml electrolyte below an electrode of the analyzer, placing 5ml of sample to be analyzed on an automatic sample inlet of the analyzer, starting the analyzer for analysis, and recording a potential diagram at the same time, wherein the result is shown in fig. 1 and 2.
Second electrode activation: and placing the base solution under the electrode for 15 times of electrode activation, and ensuring that the potential difference of the electrode after two continuous activations is less than 0.2%.
As can be seen from FIG. 1, the amounts of the added samples were 4 times, 0.2ml,0.4ml,0.6ml and 0.8ml, respectively. The standard addition amount of the sample is 0.2ml each time, the test curve reaches the end point after 4 times of addition, the curve is in a linear descending trend, each data is close to the curve, no obvious offset exists, and the method is reasonable. In the prior art, 6 standard additions are usually carried out, the time consumption is long, and the phenomenon of test point drift often occurs.
As can be seen from FIG. 2, the initial area was 5.50mc, the area after adding 0.2ml of the sample was 5.42mc, the area after adding 0.4ml of the sample was 5.35mc, the area after adding 0.6ml of the sample was 5.27mc, and the area after adding 0.8ml of the sample was 5.19mc.
As can be seen from the result of the electric quantity analysis, each 0.2ml of additive is added to inhibit the electric quantity, and the inhibition quantity is basically the same and is 0.08mc, so that the reproducibility of the analysis result can be proved to be better. In the prior art, because the concentration of the electrolyte is high, the inhibition is insufficient when the additive with the same amount is added, and the difference value of electric quantity is small, so that the judgment of a machine is affected, and the situation that an analysis result cannot be given often occurs.
Example 2
Instrument and conditions:
CVS instrument: switzerland ten thousand-pass full-automatic 894CVS analyzer
Working electrode: platinum electrode
Electrode rotation speed: 2600 rpm
Electrolyte solution: 75g/l copper sulphate, 230g/l sulphuric acid, 75g/l chloride ion, 0.75ml/l brightening agent and 2.5ml/l wetting agent
Operating temperature: 23 ℃;
analyzing positive voltage: 1.625V;
negative voltage analysis: 0.3V;
the analysis step:
first electrode activation: before instrument analysis, a blank VMS solution is placed under the electrode, and electrode activation is carried out for 15 times, so that the potential difference of the electrode after two continuous activations is ensured to be less than 0.2%.
And (3) making a standard curve: and placing 20ml of electrolyte below an electrode of the analyzer, placing 5ml of standard solution at an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor.
Verifying correction factors: placing the 20ml electrolyte below an electrode of the analyzer, placing 5ml standard solution at an automatic sample inlet of the analyzer, obtaining the concentration of the leveling agent of one standard solution by the analyzer, wherein the concentration is 1.45ml/l, the concentration is 1.35-1.65ml/l, the error is 1-10%, and the next operation can be performed.
Sample analysis: and placing the 20ml electrolyte below an electrode of the analyzer, placing 5ml of sample to be analyzed on an automatic sample inlet of the analyzer, starting the analyzer for analysis, and recording a potential diagram at the same time, wherein the result is shown in fig. 1 and 2.
Second electrode activation: and placing the base solution under the electrode for 15 times of electrode activation, and ensuring that the potential difference of the electrode after two continuous activations is less than 0.2%.
As can be seen from FIG. 3, the amounts of the added samples were 4 times, 0.2ml,0.4ml,0.6ml and 0.8ml, respectively. The standard addition amount of the sample is 0.2ml each time, the test curve reaches the end point after 4 times of addition, the curve is in a linear descending trend, each data is close to the curve, no obvious offset exists, and the method is reasonable. In the prior art, 6 standard additions are usually carried out, the time consumption is long, and the phenomenon of test point drift often occurs.
As can be seen from FIG. 4, the initial area was 27.32mc, the area after adding 0.2ml of the sample was 26.97mc, the area after adding 0.4ml of the sample was 26.60mc, the area after adding 0.6ml of the sample was 26.24mc, and the area after adding 0.8ml of the sample was 25.87mc.
As can be seen from the result of the electric quantity analysis, the change of the analysis negative voltage can affect the electric quantity value, but the inhibition effect of the additive added with 0.2ml on the electric quantity is basically the same, and is 0.37mc, the analysis result can not be affected, and meanwhile, the reproducibility of the analysis result can be proved to be good. In the prior art, because the concentration of the electrolyte is high, the inhibition is insufficient when the additive with the same amount is added, and the difference value of electric quantity is small, so that the judgment of a machine is affected, and the situation that an analysis result cannot be given often occurs.
The principles and embodiments of the present invention have been described in detail with reference to specific examples, which are provided to facilitate understanding of the method and core ideas of the present invention; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in accordance with the ideas of the present invention, the present description should not be construed as limiting the present invention in view of the above.
Claims (7)
1. The analysis method of the electroplating leveling agent for the through hole landfill of the IC carrier plate is characterized by comprising the following steps of:
preparing a standard solution: adding a brightening agent, a wetting agent and a leveling agent into a base solution to obtain a mixed solution, and fixing the volume of the mixed solution to 100ml to obtain a standard sample; the components of the basic solution are a mixed solution of copper sulfate of 75g/l, sulfuric acid of 230g/l and hydrochloric acid of 75 ppm;
preparing an electrolyte: the electrolyte comprises copper sulfate, sulfuric acid, chloride ions, a brightening agent and a wetting agent;
first electrode activation: placing the base solution under the electrode, and performing 10-15 times of electrode activation;
second electrode activation: placing the base solution under the electrode, and performing 10-15 times of electrode activation;
and (3) making a standard curve: placing the electrolyte below an electrode of an analyzer, placing a standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor;
verifying correction factors: placing the electrolyte below an electrode of an analyzer, placing a standard solution into an automatic sample inlet of the analyzer, obtaining the concentration of a leveling agent of the standard solution through the analyzer, comparing the concentration with the concentration of the leveling agent of the standard solution, and performing the next operation, wherein the error is within 1-10%; if the error exceeds 10%, repeating the steps to manufacture a standard curve;
sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample on an automatic sample inlet of the analyzer, starting the analyzer for analysis, and recording a potential diagram.
2. The method for analyzing the leveling agent for the through hole landfill of the IC carrier board according to claim 1, wherein the standard sample addition amount for determining the correction factor is 0.2ml each time, the number of addition times is 3 to 6, and the starting point of the obtained standard curve is 1 and the ending point is 0.93.
3. The method of analyzing an IC carrier via landfill electroplating leveler according to claim 1, wherein the analyzer is a cyclical circuit strip analyzer.
4. The method for analyzing the through hole landfill electroplating leveling agent of the IC carrier plate according to claim 1, wherein the electrodes of the analyzer comprise a platinum electrode, an auxiliary electrode and a reference electrode, wherein the reference electrode inner liquid of the platinum electrode is 3M potassium chloride solution, and the outer liquid is 1M potassium nitrate solution; the auxiliary electrode is a stainless steel electrode.
5. The method of analyzing an IC carrier via landfill electroplating leveler according to claim 1, wherein the analyzer has an analysis voltage threshold of 1.25V to 1.75V.
6. The method of analyzing an IC carrier via landfill electroplating leveler according to claim 1, wherein the analyzer has an analysis voltage negative of-0.175V to-0.3V.
7. The method of analyzing an IC carrier via landfill electroplating leveler of claim 1, wherein the analyzer has a working electrode rotation speed of 1000r/min to 3000r/min.
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Effective date of registration: 20230822 Address after: 29 chuhua North Road, Fengxian District, Shanghai, 201417 Patentee after: COOKSON ENTHONE CHEMISTRY (SHANGHAI) CO.,LTD. Address before: No.23 Longtan Road, Suzhou Industrial Park, Jiangsu Province Patentee before: MACDERMID TECHNOLOGY (SUZHOU) Co.,Ltd. |