阅读说明：本技术 Ic载板通孔填埋电镀整平剂的分析方法 (Analysis method of through hole filling electroplating leveling agent of IC carrier plate ) 是由 曾琳 丁惠萍 于 2020-06-05 设计创作，主要内容包括：本发明公开了一种IC载板通孔填埋电镀整平剂的分析方法,包括以下步骤：配置标准溶液；配制电解液；制作标准曲线；验证校正因子：将所述电解液放置在所述分析仪的电极下方,将标准溶液放置到所述分析仪的自动进样口,通过分析仪得到一个标准溶液的整平剂的浓度,将此浓度与标准溶液整平剂的浓度比较；样品分析：将所述电解液放置在所述分析仪的电极下方,将样品放置到所述分析仪的自动进样口,启动分析仪进行分析,同时记录电位图。其电位差值明显,分析结果稳定。(The invention discloses an analysis method of an electroplating leveling agent for through hole landfill of an IC carrier plate, which comprises the following steps: preparing a standard solution; preparing an electrolyte; making a standard curve; and verifying the correction factor: placing the electrolyte below an electrode of the analyzer, placing a standard solution at 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; 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 potential difference value is obvious, and the analysis result is stable.)

1. An analysis method of an electroplating leveling agent for through hole filling of an IC carrier is characterized by comprising the following steps:

preparing a standard solution: adding a brightening agent, a wetting agent and a leveling agent into the basic solution to obtain a mixed solution, and preparing the mixed solution into 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;

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;

and verifying the correction factor: placing the electrolyte below an electrode of the analyzer, placing the 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 carrying out the next operation if the error is within 1-10%; if the error exceeds 10%, repeating the steps to manufacture a standard curve;

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 of claim 1, wherein the calibration factor is determined by adding standard sample in an amount of 0.2ml each time for 3-6 times, and the obtained standard curve has a starting point of 1 and an ending point of 0.93.

3. The method of claim 1, wherein the base solution comprises 75g/l copper sulfate, 230g/l sulfuric acid and 75ppm hydrochloric acid.

4. The method of claim 1 wherein said analyzer is a CIE lift off analyzer.

5. The method for analyzing the through-hole landfill plating leveling agent of the IC carrier of claim 1, wherein the electrodes of the analyzer comprise a platinum electrode, an auxiliary electrode and a reference electrode, the reference electrode of the platinum electrode has an inner solution of 3M potassium chloride solution and an outer solution of 1M potassium nitrate solution; the auxiliary electrode is a stainless steel electrode.

6. The method of claim 1, wherein the analyzer has a positive analysis voltage of 1.25V-1.75V.

7. The method of claim 1, wherein the negative limit of the analysis voltage of the analyzer is from-0.175V to-0.3V.

8. The method of claim 1, wherein the rotation speed of the working electrode of the analyzer is 1000r/min-3000 r/min.

9. The method of claim 1, wherein the method further comprises: a first electrode activation, which is performed before the step of preparing the standard curve; the electrode activation is that the electrode is placed under an electrode by using a basic solution before the instrumental analysis, and the electrode activation is carried out for 10-15 times.

10. The method of claim 1, wherein the method further comprises: activating the second electrode, wherein the second electrode activation analysis is carried out after the second electrode activation analysis is finished and before the second electrode activation analysis is carried out again; the electrode activation is that the electrode is placed under an electrode by using a basic solution before the instrumental analysis, and the electrode activation is carried out for 10-15 times.

Technical Field

The invention relates to the field of leveling agent analysis, in particular to an analysis method of an electroplating leveling agent for through hole landfill of an IC carrier plate.

Background

The mademe company develops a process for directly electroplating copper to bury the through holes of the IC carrier plate, and solves the problems that the hole plugging is not full due to the air bubbles in the hole of the traditional resin plug hole, the resin and a copper layer are easy to separate, the thermal conductivity of the resin is not high, the number of components is increased, and the like.

The main components of the electrolytic copper plating liquid medicine comprise: copper sulfate, sulfuric acid, chloride ions, a brightening agent, a wetting agent and a leveling agent.

The leveling agent influences the potential difference of high and low positions, the concentration of the leveling agent is too high, the performance of a pulse electroplating process section can not be fully exerted, the copper aggregation of the middle section of the hole is not enough, and the subsequent process is influenced; the concentration of the leveling agent is too low, and during direct current electroplating, copper on the upper layer of the hole is not smooth enough, so that the through hole cannot be leveled during electroplating, and therefore, the concentration of the leveling agent needs to be analyzed.

The traditional leveling agent analysis method mostly adopts an RC (stress current) mode, the basic components of the electrolyte are analyzed, the concentration of the basic components is the same as that of the bath solution, a corresponding standard curve is drawn by adding 4-6 times of leveling agents with the same concentration, then the bath solution is tested again, and the corresponding concentration is found on the standard curve. The method has the disadvantages that the concentration of the additive is too high, so that the analysis electrode is not easy to clean, the analysis liquid is polluted to influence the analysis result, the analysis result is unstable, the reproducibility is poor, and the service life of the electrode is shortened.

Disclosure of Invention

In order to overcome the defects in the prior art, the embodiment of the invention provides an analysis method of an IC carrier through hole filling electroplating leveling agent, and the analysis result is stable.

In order to achieve the above object, the embodiment of the present application discloses an analysis method for an IC carrier through-hole burying electroplating leveling agent, which includes the following steps:

preparing a standard solution: adding a brightening agent, a wetting agent and a leveling agent into the basic solution to obtain a mixed solution, and preparing the mixed solution into 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;

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;

and verifying the correction factor: placing the electrolyte below an electrode of the analyzer, placing the 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 carrying out the next operation if the error is within 1-10%; if the error exceeds 10%, repeating the steps to manufacture a standard curve;

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, the addition amount of the standard sample for determining the correction factor is 0.2ml each time, the addition times are 3-6 times, and the starting point and the ending point of the obtained standard curve are 1 and 0.93 respectively.

Preferably, the basic solution comprises 75g/l of copper sulfate, 230g/l of sulfuric acid and 75ppm of hydrochloric acid.

Preferably, the analyzer is a cyclic circuit stripping analyzer.

Preferably, the electrodes of the analyzer comprise a platinum electrode, an auxiliary electrode and a reference electrode, wherein the reference electrode internal solution of the platinum electrode is a 3M potassium chloride solution, and the external solution is a 1M potassium nitrate solution; the auxiliary electrode is a stainless steel electrode.

Preferably, the positive analysis voltage limit 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 rotating speed of the working electrode of the analyzer is 2600 r/min.

The invention has the following beneficial effects:

1. the invention uses DT (dilution migration) mode to analyze, the analysis electrolyte is changed into low-concentration copper sulfate and additive, the low-concentration copper and additive enable the cleaning of the electrode to be easier, 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 the potential difference obtained in the analysis process is obvious, the potential performance is stable, the verification of the correction factor is simpler and clearer, and the reproducibility of the analysis result is good.

3. The DT mode is less sensitive to the influence of the operating environment, the application range of the operating temperature and the operating humidity is wide, and the field management and control of a factory are facilitated.

4. According to the invention, through the comparison test of the standard solution and the DT analysis method, the deviation between the analysis result and the standard value can be reduced to about 2%, and the analysis result is stable, so that the control on the leveler is facilitated, and the performance of the liquid medicine can be brought into the best state.

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 graph of a standard addition of a sample according to example 1 of the present invention;

FIG. 2 is a graph of the measured electric quantity of a sample of example 1 of the present invention;

FIG. 3 is a graph of standard additions to samples of example 2 of the present invention;

FIG. 4 is a graph of the measured electric quantity of a sample of 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 the description of the present invention, it should be noted that the terms "upper", "lower", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature.

In order to achieve the above object, the present invention provides an analysis method for an electroplating leveling agent for through hole filling of an IC carrier, comprising the following steps:

preparing a standard solution: adding 1ml/l of brightening agent, 30ml/l of wetting agent and 1.5ml/l of leveling agent into the base solution to obtain a mixed solution, and setting the mixed solution to be 100ml to obtain a standard sample;

preparing an electrolyte: the electrolyte comprises 75g/l of copper sulfate, 230g/l of sulfuric acid, 75g/l of chloride ions, 0.75ml/l of brightening agent and 2.5ml/l of wetting agent;

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;

and verifying the correction factor: placing the electrolyte below an electrode of the analyzer, placing the 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 carrying out the next operation if the error is within 1-10%; if the error exceeds 10%, repeating the steps to manufacture a standard curve;

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.