CN114858897A - Method for analyzing leveling agent of acid copper plating process of semiconductor - Google Patents
Method for analyzing leveling agent of acid copper plating process of semiconductor Download PDFInfo
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- CN114858897A CN114858897A CN202111623680.9A CN202111623680A CN114858897A CN 114858897 A CN114858897 A CN 114858897A CN 202111623680 A CN202111623680 A CN 202111623680A CN 114858897 A CN114858897 A CN 114858897A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/4163—Systems checking the operation of, or calibrating, the measuring apparatus
Abstract
The invention discloses an analysis method of an acid copper plating process leveling agent of a semiconductor, which comprises the following steps: preparing a standard solution: adding 2mL of brightener stock solution SC R1, 0.6mL of wetting agent stock solution SC R2A and 0.6mL of leveling agent stock solution SC R2B to the base solution to obtain a mixed solution, and preparing the mixed solution into 100mL to obtain a standard sample; preparing an electrolyte: the electrolyte comprises 40g/L of copper metal, 140g/L of sulfuric acid and 50mg/L of chloride ions, 40mL/L of SC R1 and 20mL/L of SC R2A; making a response curve: placing the electrolyte below an electrode of the analyzer, placing the standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor; and (3) sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample into an automatic sample inlet of the analyzer, starting the analyzer for analysis, and simultaneously recording a potential diagram. 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 a leveling agent for an acid copper plating process of a semiconductor.
Background
The mcdenmei company developed microcrystalline SC-40 technology specifically designed for high speed, columnar and copper stud/UBM applications. It provides unique within-wafer, in-mold, and within-feature uniformity. The series of liquid medicines are also approved by a plurality of customers and are applied on line. As the feature size of the line width of the chip becomes smaller and smaller, customers require high flatness of the surface of the copper plating layer, which becomes a key factor restricting the increase of the transmission speed of the integrated circuit. The purification and chemical system of the copper plating solution directly determines the surface morphology of the copper pillar or copper wiring layer. The selection and optimization of plating conditions is critical, with the chemistry of the plating solution playing a critical role.
The chemical components typically used in acid copper plating include the basic plating solution (metal ions, sulfuric acid, chloride ions) and organic additives. Which is decisive for the surface morphology of the electroplated layers, can generally be divided into suppressors (or wetting agents), levelers and brighteners (or accelerators). In the prior art, the control of the surface appearance and smoothness of a copper electroplating layer is mainly realized by the conditions of the electroplating process and the addition of different chemical systems (namely different additive systems).
The main components of the electrolytic copper plating liquid medicine comprise: the copper metal concentration of SC 40MU is 40g/L, sulfuric acid (reagent or semiconductor grade) 135-145g/L, chloride ion (reagent grade) 40-60mg/L, SC R1 (brightener and inhibitor mixture) 16-20mL/L, SC R2(R2A plus R2B)10-14mL/L, leveling agent (R2B)2-7 mL/L.
The leveling agent influences the potential difference of high and low positions, the concentration of the leveling agent is too high, the copper in the middle section of the circuit is not sufficiently accumulated, the surfaces of two ends of the circuit are too rough, the concentration of the leveling agent is too low, the copper of the circuit is not flat enough, and the surface of the circuit is convex when electroplating is caused. Influencing subsequent processes
A general leveling agent analysis method mostly adopts a cyclic voltammetry stripping method CVS mode, an influence curve RC method is adopted, a corresponding standard curve is made by adding 4-6 times of leveling agents with known concentrations into proper electrolytic base liquid, then tank liquid is measured back, and the corresponding concentrations are found on the standard curve. The method has the defects that the stable circulation of the electric quantity of the electrolytic base solution is too long (deviation change is 1%), the stripping peak area measured at the position of the Pt disk electrode is influenced, the temperature rise of the electrolytic base solution influences the large electric quantity change of the electrolyte, the influence on the analysis result is unstable, and the repeatability is poor.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides an analysis method of a leveling agent for an acid copper plating process of a semiconductor, and the analysis result is stable.
In order to achieve the purpose, the embodiment of the application discloses an analysis method of a leveling agent of an acid copper plating process of a semiconductor, which comprises the following steps:
preparing a standard solution: adding 2mL of 20mL/L brightener SC R1, 6mL of 6mL/L wetting agent SC R2A and 6mL of 6mL/L leveling agent SC R2B to the base solution to obtain a mixed solution, and making the mixed solution into 100mL to obtain a standard sample;
preparing an electrolyte: the electrolyte comprises 40g/L copper metal, 140g/L sulfuric acid and 50mg/L chloride ions, 40mL/L SC R1 and 20mL/L SC R2A;
making a response curve: placing the electrolyte below an electrode of the analyzer, placing the standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor;
and (3) sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample into an automatic sample inlet of the analyzer, starting the analyzer for analysis, and simultaneously recording a potential diagram.
Preferably, when a response curve is prepared, the amount of the SC R2B sample added per time is 0.4ml, the number of times of addition is 12, and the starting point of the curve is 1, thereby obtaining a response curve.
Preferably, the SC R2B is Madeim (422669MICROFAB SC R2-B).
Preferably, the SC R1 is a blend of brightener and inhibitor, and the SC R1 is Maidemed (421514MICROFAB SC R1).
Preferably, the SC R2A is mademe (422695MICROFAB SC R2-a).
Preferably, the analyzer is a cyclic circuit stripping (CVS) analyzer.
Preferably, the working electrode is a platinum electrode, the reference electrode inner solution is a 3M potassium chloride solution, the outer solution is a 1M potassium nitrate solution, and the auxiliary electrode is a platinum electrode.
Preferably, the positive value of the analytical voltage is 1-2V.
Preferably, the negative limit is-0.5-1V.
Preferably, the working electrode rotation speed is 500-.
The invention has the following beneficial effects: through the comparison test of the standard solution, the analysis result is stable by adopting the RC analysis method of CPVS. This facilitates the handling of the leveler, which also optimizes the performance of the chemical.
In order to make the aforementioned and other objects, features and advantages of the invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a standard graph of example 1 of the present invention;
FIG. 2 is a graph of a standard solution known from the re-test preparation of example 1 of the present invention;
FIG. 3 is a graph of the capacity of a sample test of a customer;
FIG. 4 is a standard curve chart of example 2 of the present invention;
FIG. 5 is a graph of a standard solution prepared by a re-test in example 2 of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to achieve the above object, the present invention provides a method for analyzing a leveler for an acid copper plating process of a semiconductor, comprising the steps of:
preparing a standard solution: adding 40g/L copper metal, 140g/L sulfuric acid, 50mg/L chloride ions, 40mL/L SC R1 and 20mL/L SC R2A to obtain a mixed solution, and preparing the mixed solution into 100mL to obtain a standard sample;
preparing an electrolyte: the electrolyte comprises 40g/L of copper metal, 140g/L of sulfuric acid and 50mg/L of chloride ions, 40mL/L of SC R1 and 20mL/L of SC R2A;
making a standard curve: placing the electrolyte below an electrode of the analyzer, placing the standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor;
and (3) sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample into an automatic sample inlet of the analyzer, starting the analyzer for analysis, and simultaneously recording a potential diagram.
Further, when the correction factor is determined, the amount of the sample of SC R2B added each time is 0.2ml, the number of times of addition is 12, the starting point of the curve is 1, and the ending point is 0.93, so as to obtain the correction factor.
Further, the SC R2B
Further, the SC R1 is a mixture of a brightener and a suppressor, and the SC R1 is Mideam
Further, said SC R2A is
Further, the analyzer is a cyclic circuit stripping (CVS) analyzer.
Furthermore, the working electrode is a platinum electrode, the reference electrode inner solution is 3M potassium chloride solution, the outer solution is 1M potassium nitrate solution, and the auxiliary electrode is a stainless steel electrode.
Further, the positive value of the analysis voltage is 1-2V.
Further, the negative limit value is-0.5-1V.
Further, the rotating speed of the working electrode is 500-1500 rpm.
Furthermore, through a comparative test on the standard solution, an RC analysis method of CPVS is adopted, and the analysis result is stable. This facilitates the handling of the leveler, which also optimizes the performance of the chemical.
Example 1
Instruments and conditions:
CVS instrument: a Switzerland full-automatic 797CVS analyzer;
a working electrode: 2 mm platinum electrodes;
electrode rotation speed: 1000 revolutions per minute;
electrolyte solution: 40g/L copper metal, 140g/L sulfuric acid and 50mg/L chloride ion, 40mL/L SC R1 and 20mL/L SC R2A;
working temperature: 23 deg.C
RC analysis method of CPVS (chlorinated polyvinyl chloride) mode
Analysis of stripping positive voltage: 0.25V;
step length time: 5sec
Analyzing the negative voltage of electroplating: 0.18V;
step length time: 4sec
And (3) an analysis step:
before instrumental analysis, electrode activation was performed 10-15 times with a blank VMS solution placed under the electrode.
Preparing an electrolyte: the electrolyte comprises 40g/L of copper metal, 140g/L of sulfuric acid and 50mg/L of chloride ions, 40mL/L of SC R1 and 20mL/L of SC R2A
Preparing a standard solution: 40g/L copper metal, 140g/L sulfuric acid and 50mg/L chloride ion, 40mL/L SC R1 and 12mL/L SC R2 were added to obtain a mixed solution, and the mixed solution was made to 100mL to obtain a standard sample.
Making a standard curve: and (3) placing the electrolyte in a cup below an electrode of the analyzer, placing the standard solution in a sample inlet of a liquid adding unit of the analyzer, cleaning and filling a pipeline, and starting a response curve method of the analyzer to obtain a response curve, wherein the response curve is shown in figure 4.
And (3) verifying the standard solution: and placing the electrolyte in a cup below an electrode of the analyzer, starting a sample analysis method of the analyzer, emptying the electrolyte after obtaining an electrolyte signal value, and pouring a standard solution. Obtaining the concentration of the leveling agent of a standard solution through an analyzer, comparing the concentration with the concentration of the standard solution, and carrying out the next operation if the error is within 1-10%; if the error exceeds 10%, the steps are repeated to make a standard curve, as shown in FIG. 5.
And (3) sample analysis: the electrolyte was placed in a cup under the electrodes of the analyzer, the sample analysis method of the analyzer was started, after obtaining the electrolyte signal value, the electrolyte was drained, the sample solution was poured (the concentration of R1 and R2A was adjusted to be consistent with the concentration values of R1 and R2A of the base solution), and the leveler concentration of one sample was obtained by the analyzer, see fig. 3.
After the instrument was used, a blank VMS solution was placed under the electrode and 10-15 electrode activations were performed.
As can be seen from FIG. 1, the amount of sample added was 12 times, each addition of 0.4mL, the starting area was 1.82mc, the product after the addition of 0.4mL of R2B was 1.77mc, the product after the addition of 0.4mL of R2B was 1.73mc, the product after the addition of 0.4mL of R2B was 1.69mc, the product after the addition of 0.4mL of R2B was 1.65mc, the addition of 0.4mL of R2B was 1.61mc, the product after the addition of 0.4mL of R2B was 1.58mc, the product after the addition of 0.4mL of R2B was 1.54mc, the product after the addition of 0.4mL of R2B was 1.51mc, the product after the addition of 0.4mL of R2B was 1. B mc, the product after the addition of 0.4mL of R2 was 1.48mc, the addition of 0.4mL of R2B was 1.51mc, the product after the addition of 0.9 mL of R2 was 1.48mc, the product after the addition of 0.5 mL of R2 was 1.5 mL, the addition of the first 4mL of R2 was 1.25 mc, and the response of the product after the addition of the first R2 m1.25 m5 mL of the first R2 mC was 1.25 mC.
As can be seen from FIG. 2, the initial area Q (0) obtained after pouring the electrolyte was 1.77mc, the electrolyte was drained, the standard solution was poured to obtain a sample area Q of 1.56mc, and the leveling agent standard concentration was obtained by calculating the Q/Q (0) correspondence curve.
As can be seen from FIG. 3, the initial area Q (0) obtained after pouring the electrolyte was 1.79mc, the electrolyte was drained, the sample solution was poured to obtain a sample area Q of 1.69mc, and the Q/Q (0) correspondence curve was calculated to obtain the sample leveler concentration.
Example two:
instruments and conditions:
CVS instrument: a Switzerland full-automatic 797CVS analyzer;
a working electrode: 2 mm platinum electrodes;
electrode rotation speed: 2600 rpm;
electrolyte solution: 40g/L copper metal, 140g/L sulfuric acid and 50mg/L chloride ion, 40mL/L SC R1 and 20mL/L SC R2A;
working temperature: 23C;
RC analysis method of CVS mode
Analysis of positive voltage: 1.625V;
analysis of negative voltage: 0.18V;
and (3) an analysis step:
before instrumental analysis, electrode activation was performed 10-15 times with a blank VMS solution placed under the electrode.
Preparing an electrolyte: the electrolyte comprises 40g/L of copper metal, 140g/L of sulfuric acid and 50mg/L of chloride ions, 40mL/L of SC R1 and 20mL/L of SC R2A
Preparing a standard solution: 40g/L copper metal, 140g/L sulfuric acid and 50mg/L chloride ion, 40mL/L SC R1 and 12mL/L SC R2 were added to obtain a mixed solution, and the mixed solution was made to 100mL to obtain a standard sample.
Making a standard curve: and (3) placing the electrolyte in a cup below an electrode of the analyzer, placing the standard solution in a liquid adding unit sample inlet of the analyzer, cleaning and filling a pipeline, and starting a response curve method of the analyzer to obtain a response curve, wherein the response curve is shown in figure 4.
And (3) verifying the standard solution: and placing the electrolyte in a cup below an electrode of the analyzer, starting a sample analysis method of the analyzer, emptying the electrolyte after obtaining an electrolyte signal value, and pouring a standard solution. The leveling agent concentration of a standard solution was obtained by the analyzer, as shown in fig. 5.
After the instrument was used, a blank VMS solution was placed under the electrode and 10-15 electrode activations were performed.
As can be seen from FIG. 4, the amount of sample added was 12 times, each addition of 0.4mL, the initial area was 624.35uC, the product was 624.35uC after the addition of 0.4mL R2B for the 1 st time, the product was 601.88uC after the addition of 0.4mL R2B for the 2 nd time, the product was 578.07uC after the addition of 0.4mL R2B for the 3 rd time, the product was 556.69uC after the addition of 0.4mL R2B for the 4 th time, the product was 536.83uC after the addition of 0.4mL R2B for the 5 th time, the product was 516.41uC after the addition of 0.4mL R2B for the 6 th time, the product was 5uC after the addition of 0.4mL R2B for the 7 th time, the product was 483.23uC after the addition of 0.4mL R2B for the 8 th time, the product was 466.79 th after the addition of 0.4mL R2B, the 10 th time, the addition of the sample was 5732 uC, and the response curve was 82B uC.
As can be seen from FIG. 5, the initial area Q (0) obtained after pouring the electrolyte was 651.69c, the electrolyte was drained, the standard solution was poured to obtain a sample area Q of 609.36uC, and the leveling agent concentration was 2.9mL/L, which was not matched with the prepared standard concentration of 6mL/L, by calculating the Q/Q (0) correspondence curve.
According to the analysis result, the standard solution obtained by the RC analysis method in the CVS mode does not accord with the preparation concentration, and the analysis result is influenced due to small electric quantity of the electrolyte and small difference of the electric quantity. In the CPVS mode RC analysis method, the electric quantity is large, the difference of the electric quantity is large, the polarization time is short and irreversible adsorption on the surface of the platinum electrode can be avoided due to the fact that the electric quantity of the electrolyte is large and the electric quantity is large when the same amount of additives are added.
Because the semiconductor wafer acid copper plating does not have an analysis method of the leveling agent at present, the analysis method for finding the leveling agent capable of providing the semiconductor wafer acid copper plating in the existing analysis technology has stable analysis results.
The principle and the implementation mode of the invention are explained by applying specific embodiments in the invention, and the description of the embodiments is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. An analysis method of a leveling agent of an acid copper plating process of a semiconductor is characterized by comprising the following steps:
preparing a standard solution: adding 2mL of brightener stock solution SC R1, 0.6mL of wetting agent stock solution SC R2A and 0.6mL of leveling agent stock solution SC R2B to the base solution to obtain a mixed solution, and preparing the mixed solution into 100mL to obtain a standard sample;
preparing an electrolyte: the electrolyte comprises 40g/L of copper metal, 140g/L of sulfuric acid and 50mg/L of chloride ions, 40mL/L of SC R1 and 20mL/L of SC R2A;
making a response curve: placing the electrolyte below an electrode of the analyzer, placing the standard solution into an automatic sample inlet of the analyzer, and starting the analyzer to obtain a standard curve and a correction factor;
and (3) sample analysis: and placing the electrolyte below an electrode of the analyzer, placing a sample into an automatic sample inlet of the analyzer, starting the analyzer for analysis, and simultaneously recording a potential diagram.
2. The method for analyzing leveling agent for acid copper plating process of semiconductor as claimed in claim 1, wherein the response curve is obtained by adding SC R2B sample 0.4ml each time, adding 12 times, and starting point of the curve is 1.
3. The method of analyzing an acidic copper plating process leveler for semiconductors of claim 1, wherein the SC R2B is mademe (422669MICROFAB SC R2-B).
4. The method of analyzing an acid copper plating process leveler for semiconductors of claim 1, wherein the SC R1 is a mixture of brightener and suppressor, and the SC R1 is mademe (421514MICROFAB SC R1).
5. The method of analyzing an acidic copper plating process leveler for semiconductors of claim 1, wherein the SC R2A is mademe (422695MICROFAB SC R2-a).
6. The method of analyzing an acidic copper plating process leveler for semiconductors of claim 1, wherein the analyzer is a cyclic circuit stripping (CVS) analyzer.
7. The method of analyzing an acidic copper plating process leveler for semiconductors of claim 1, wherein the working electrode is a platinum electrode, the reference electrode has an inner solution of 3M potassium chloride solution, the outer solution is a 1M potassium nitrate solution, and the auxiliary electrode is a platinum electrode.
8. The method for analyzing an acid copper plating process leveler for semiconductors of claim 1, wherein the analytical voltage positive value is 1-2V.
9. The method for analyzing an acid copper plating process leveler for semiconductors of claim 1, wherein the negative limit value is-0.5 to 1V.
10. The method as claimed in claim 1, wherein the rotation speed of the working electrode is 500-1500 rpm.
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2021
- 2021-12-28 CN CN202111623680.9A patent/CN114858897A/en active Pending
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| JP2001073183A (en) * | 1999-08-31 | 2001-03-21 | Ebara Corp | Method for measuring leveler concentration in copper sulfate plating liquid |
| US20040000484A1 (en) * | 2002-06-27 | 2004-01-01 | Applied Materials, Inc. | Methods in electroanalytical techniques to analyze organic components in plating baths |
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