Integrated circuit nickel plating solution on-line analysis system and method

Abstract

The application discloses an integrated circuit nickel plating electrolyte online analysis system and method, and relates to the technical field of electrolyte analysis.The system comprises a sampling unit, a liquid delivery unit, a reaction cup, a wetting agent analysis unit, a detection instrument and a control and data processing unit.The reaction cup is used as a titration reaction site for boric acid analysis and chloride ion analysis, and is internally provided with a stirrer.The wetting agent analysis unit comprises a separately arranged beaker, a weighing sensor below the beaker and a liquid drop sensing sensor above the beaker.The liquid delivery unit comprises a first peristaltic pump, a second peristaltic pump, a third peristaltic pump, a first injection pump, a second injection pump and a third injection pump.The detection instrument comprises a spectrometer, a pH electrode, a silver electrode and an ICP analyzer.The application realizes full-automatic online analysis of nickel ions, chloride ions, boric acid, 110AD3 additives, copper ion impurities and wetting agents in the nickel plating electrolyte, and has the advantages of high analysis efficiency, saving of manpower, good process stability and the like.

Description

Technical Field

[0001] This invention relates to the field of nickel plating solution analysis technology, and in particular to an online analysis system and method for nickel plating solutions used in integrated circuits. Background Technology

[0002] Nickel plating is a process that deposits a nickel layer on the surface of a metallic or non-metallic substrate through electrolysis. Its purpose is to impart properties such as corrosion resistance and wear resistance to the substrate material. In integrated circuit manufacturing, nickel plating is widely used for surface treatment of components such as lead frames and packaging substrates. The quality of the plating directly affects the reliability and lifespan of integrated circuit devices.

[0003] The stability of the electroplating bath composition is a core element in ensuring plating quality. Key parameters in the nickel plating bath, such as nickel ion concentration, chloride ion concentration, boric acid concentration, 110AD3 additive concentration, copper ion impurity content, and wetting agent concentration, directly determine the thickness, uniformity, adhesion, and microstructure of the plating layer. Therefore, accurate detection of the concentrations of each component in the nickel plating bath is a crucial step in ensuring plating quality.

[0004] Currently, the analysis of nickel plating solutions mainly relies on manual, timed sampling. Operators periodically take samples from the plating bath, analyzing the concentrations of nickel ions and 110AD3 additive using colorimetry, copper ion impurities using ICP (inductively coupled plasma atomic emission spectrometry), chloride ions and boric acid using titration, and wetting agents using gravimetric analysis. However, this traditional manual analysis method has the following significant drawbacks: (i) Data lag and inability to provide real-time feedback. Manual analysis has a long cycle and the data is severely outdated, failing to reflect real-time changes in the plating solution. When the composition of the plating solution fluctuates, it is difficult to detect and adjust in a timely manner, resulting in untimely adjustments to process parameters and unstable coating quality.

[0005] (ii) Large operational errors and low analytical accuracy. Manual analysis relies on the experience and skills of the operators, and human error is inevitable, resulting in unstable analytical data, poor reproducibility, and difficulty in meeting the stringent requirements of integrated circuit manufacturing for coating quality.

[0006] (iii) Time-consuming and labor-intensive. Manual analysis requires sampling, pretreatment and detection of multiple components separately. A single complete analysis takes a long time, is labor-intensive and has high labor costs.

[0007] (iv) Low analysis frequency makes it difficult to ensure process stability. Due to the limited efficiency of manual operation, the analysis frequency cannot be significantly increased. When the parameters of the plating bath fluctuate greatly, real-time data cannot be obtained in a timely manner, making it difficult to ensure the long-term stability of the nickel plating process. Summary of the Invention

[0008] According to an embodiment of the present invention, an online analysis system for nickel plating solution of integrated circuits is provided, comprising: The sampling unit (which belongs to the prior art) is used to circulate samples from the nickel plating tank to obtain nickel plating solution samples; The liquid delivery unit includes multiple peristaltic pumps and syringe pumps with measurable volumes for quantitatively delivering nickel plating solution samples and various chemicals to the corresponding analysis locations; The reaction cup is used for titration and colorimetric reactions in boric acid and chloride ion analysis. The reaction cup is equipped with a stir bar driven by a motor. The wetting agent analysis unit includes a beaker, a weighing sensor, and a droplet sensor. The beaker is an independent container for wetting agent analysis. The weighing sensor is located below the beaker, and the droplet sensor is located above the beaker. The testing instruments include a spectrometer, pH electrode, silver electrode, and ICP analyzer; The control and data processing unit is electrically connected to the sampling unit, liquid delivery unit, detection instrument and wetting agent analysis unit, and is used to control the operation of each unit and collect analytical data; Among them, the pH electrode is used to detect the endpoint of boric acid titration, the silver electrode is used to detect the endpoint of chloride ion titration, the spectrometer is used to detect the absorbance of nickel ions and additives, the ICP analyzer is used to detect the signal intensity of copper ions, and the weighing sensor and the droplet sensing sensor work together to perform the drop weight method analysis of wetting agent.

[0009] Furthermore, the liquid delivery unit includes: The first peristaltic pump is used to deliver mannitol into the reaction vessel; The second peristaltic pump is used to deliver pure water into the reaction vessel; The third peristaltic pump is used to deliver ammonia water into the reaction vessel; The first syringe pump is used to draw sodium hydroxide solution and titrate it in a reaction vessel. The second syringe pump is used to draw silver nitrate standard solution and titrate it in the reaction vessel; The third syringe pump is used for quantitative sampling and droplet analysis of the wetting agent in the beaker.

[0010] Furthermore, in the wetting agent analysis unit, the third injection pump drips the sample into the beaker at a uniform rate through a glass dropper.

[0011] According to another embodiment of the present invention, an online analysis method for nickel plating solution of integrated circuits is also provided, comprising the online analysis system for nickel plating solution of integrated circuits of the previous embodiment, and including the following steps: Step S1: Samples are circulated from the nickel plating tank using the sampling unit, and the sample is obtained after filtration. Step S2: Quantitatively distribute the sample to each analysis position using the liquid delivery unit; Step S3: Perform the following analysis operations: Boric acid analysis: The sample is placed in a reaction vessel, mannitol is added for complexation, and then titrated with sodium hydroxide standard solution. The titration endpoint is detected by pH electrode, and the boric acid concentration is calculated. Chloride ion analysis: The sample is placed in a reaction vessel and titrated with silver nitrate standard solution. The titration endpoint is detected by a silver electrode, and the chloride ion concentration is calculated. Nickel ion analysis: The diluted sample is passed through a spectrometer to measure the absorbance at a characteristic wavelength and the nickel ion concentration is calculated. Additive analysis: The diluted sample was passed through a spectrometer to measure the absorbance at characteristic wavelengths and the concentration of 110AD3 additive was calculated. Copper ion analysis: The sample is sent to an ICP analyzer to measure the copper signal intensity and calculate the copper ion concentration; Wetting agent analysis: The sample is quantitatively sampled by a syringe pump and dripped into a beaker at a constant rate through a glass dropper. The total number of drops is recorded by a droplet sensor located above the beaker and the total weight is recorded by a weighing sensor located below the beaker. The average weight of a single drop is calculated, and the wetting agent concentration is then analyzed. Step S4: The control and data processing unit collects the detection data, calculates and outputs the concentration results of each component.

[0012] Furthermore, the specific steps of boric acid analysis in step S3 are as follows: a quantitative sample of nickel plating solution is placed in a reaction vessel, and mannitol solution is drawn into the reaction vessel using a first peristaltic pump to allow mannitol to undergo a complexation reaction with boric acid in the sample; sodium hydroxide standard solution is added dropwise to the reaction vessel using a first syringe pump, while the pH value of the reaction solution is monitored in real time using a pH electrode; when the pH value changes abruptly, the titration endpoint is determined to have been reached, and the amount of sodium hydroxide standard solution consumed is recorded, thereby calculating the boric acid concentration in the sample.

[0013] Furthermore, the specific steps of chloride ion analysis in step S3 are as follows: a quantitative sample of nickel plating solution is placed in a reaction cup, and silver nitrate standard solution is added dropwise to the reaction cup through a second injection pump to allow silver ions to react with chloride ions in the sample to form silver chloride precipitate; the concentration change of silver ions in the reaction solution is monitored in real time through a silver electrode; when the concentration of silver ions changes abruptly, the titration endpoint is determined to have been reached, the amount of silver nitrate standard solution consumed is recorded, and the concentration of chloride ions in the sample is calculated.

[0014] Furthermore, the specific steps for nickel ion analysis and additive analysis in step S3 are as follows: take a nickel plating solution sample, dilute it with deionized water to a predetermined ratio, mix it well, and then pass it into a spectrometer. Measure the absorbance at the characteristic absorption wavelength of nickel ions and at the characteristic absorption wavelength of the 110AD3 additive. Then calculate the concentrations of nickel ions and additives in the sample.

[0015] Furthermore, the specific steps of the wetting agent analysis in step S3 are as follows: A sample of the nickel plating solution is quantitatively extracted using a third injection pump; the sample is then dripped dropwise into a beaker at a constant speed using a glass dropper; the total number of droplets N is automatically recorded by a droplet sensor located above the beaker; and the total weight W_total of the droplets is recorded by a weighing sensor located below the beaker; the average weight per drop is then calculated. The concentration of wetting agent in the sample is calculated based on the pre-established standard curve of average weight of a single drop versus concentration of wetting agent.

[0016] The online analysis system and method for nickel plating solution of integrated circuits according to embodiments of the present invention realize fully automatic, real-time, online quantitative analysis of multiple components such as nickel ions, chloride ions, boric acid, 110AD3 additive, copper ion impurities and wetting agents in nickel plating solution, thereby improving analysis efficiency, reducing labor costs and ensuring process stability.

[0017] It should be understood that both the foregoing general description and the following detailed description are exemplary and intended to provide further illustration of the claimed technology. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the sampling and analysis steps of the nickel plating solution according to an embodiment of the present invention. Detailed Implementation

[0019] The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, further illustrating the present invention.

[0020] First, combine Figure 1 This invention describes an online analysis system for nickel plating solutions used in integrated circuits, which has a wide range of applications.

[0021] like Figure 1 As shown, the online analysis system for nickel plating solution of integrated circuits according to an embodiment of the present invention includes: The sampling unit is used to circulate samples from the nickel plating bath to obtain nickel plating solution samples; The liquid delivery unit includes multiple peristaltic pumps and syringe pumps with measurable volumes for quantitatively delivering nickel plating solution samples and various chemicals to the corresponding analysis locations; The reaction cup is used for titration and colorimetric reactions in boric acid and chloride ion analysis. The reaction cup is equipped with a stir bar driven by a motor. The wetting agent analysis unit includes a beaker, a weighing sensor, and a droplet sensor. The beaker is an independent container for wetting agent analysis. The weighing sensor is located below the beaker, and the droplet sensor is located above the beaker. The testing instruments include a spectrometer, pH electrode, silver electrode, and ICP analyzer; The control and data processing unit is electrically connected to the sampling unit, liquid delivery unit, detection instrument and wetting agent analysis unit, and is used to control the operation of each unit and collect analytical data; Among them, the pH electrode is used to detect the endpoint of boric acid titration, the silver electrode is used to detect the endpoint of chloride ion titration, the spectrometer is used to detect the absorbance of nickel ions and additives, the ICP analyzer is used to detect the signal intensity of copper ions, and the weighing sensor and the droplet sensing sensor work together to perform the drop weight method analysis of wetting agent.

[0022] Furthermore, such as Figure 1 As shown, in this embodiment, the liquid delivery unit includes: The first peristaltic pump is used to deliver mannitol into the reaction vessel; The second peristaltic pump is used to deliver pure water into the reaction vessel; The third peristaltic pump is used to deliver ammonia water into the reaction vessel; The first syringe pump is used to draw sodium hydroxide solution and titrate it in a reaction vessel. The second syringe pump is used to draw silver nitrate standard solution and titrate it in the reaction vessel; The third syringe pump is used for quantitative sampling and droplet analysis of the wetting agent in the beaker.

[0023] Furthermore, such as Figure 1 As shown, in this embodiment, in the wetting agent analysis unit, the third injection pump drips the sample into the beaker at a uniform rate through a glass dropper.

[0024] According to another embodiment of the present invention, an online analysis method for nickel plating solution of integrated circuits is also provided, comprising the online analysis system for nickel plating solution of integrated circuits of the previous embodiment, and including the following steps: Step S1: Samples are circulated from the nickel plating tank using the sampling unit, and the sample is obtained after filtration. Step S2: Quantitatively distribute the sample to each analysis position using the liquid delivery unit; Step S3: Perform the following analysis operations: Boric acid analysis: The sample is placed in a reaction vessel, mannitol is added for complexation, and then titrated with sodium hydroxide standard solution. The titration endpoint is detected by pH electrode, and the boric acid concentration is calculated. Chloride ion analysis: The sample is placed in a reaction vessel and titrated with silver nitrate standard solution. The titration endpoint is detected by a silver electrode, and the chloride ion concentration is calculated. Nickel ion analysis: The diluted sample is passed through a spectrometer to measure the absorbance at a characteristic wavelength and the nickel ion concentration is calculated. Additive analysis: The diluted sample was passed through a spectrometer to measure the absorbance at characteristic wavelengths and the concentration of 110AD3 additive was calculated. Copper ion analysis: The sample is sent to an ICP analyzer to measure the copper signal intensity and calculate the copper ion concentration; Wetting agent analysis: The sample is quantitatively sampled by a syringe pump and dripped into a beaker at a constant rate through a glass dropper. The total number of drops is recorded by a droplet sensor located above the beaker and the total weight is recorded by a weighing sensor located below the beaker. The average weight of a single drop is calculated, and the wetting agent concentration is then analyzed. Step S4: The control and data processing unit collects the detection data, calculates and outputs the concentration results of each component.

[0025] Furthermore, such as Figure 1 As shown, in this embodiment, the specific steps of boric acid analysis in step S3 are as follows: a quantitative sample of nickel plating solution is placed in a reaction cup, and mannitol solution is drawn into the reaction cup by a first peristaltic pump to allow mannitol to undergo a complexation reaction with boric acid in the sample; sodium hydroxide standard solution is added dropwise to the reaction cup by a first injection pump, and the pH value of the reaction solution is monitored in real time by a pH electrode; when the pH value changes abruptly, the titration endpoint is determined to have been reached, the amount of sodium hydroxide standard solution consumed is recorded, and the boric acid concentration in the sample is calculated.

[0026] Furthermore, such as Figure 1 As shown, in this embodiment, the specific steps of chloride ion analysis in step S3 are as follows: a quantitative sample of nickel plating solution is taken into a reaction cup, and silver nitrate standard solution is added dropwise into the reaction cup through a second injection pump to allow silver ions to react with chloride ions in the sample to form silver chloride precipitate; the concentration change of silver ions in the reaction solution is monitored in real time through a silver electrode; when the concentration of silver ions changes abruptly, the titration endpoint is determined to be reached, the amount of silver nitrate standard solution consumed is recorded, and the concentration of chloride ions in the sample is calculated.

[0027] Furthermore, such as Figure 1As shown, in this embodiment, the specific steps of nickel ion analysis and additive analysis in step S3 are as follows: take a nickel plating solution sample, dilute it with deionized water to a predetermined multiple, mix it well, and then pass it into a spectrometer. Measure the absorbance at the characteristic absorption wavelength of nickel ions and at the characteristic absorption wavelength of the 110AD3 additive. Then calculate the concentrations of nickel ions and additives in the sample.

[0028] Furthermore, such as Figure 1 As shown, in this embodiment, the specific steps of the wetting agent analysis in step S3 are as follows: A sample of the nickel plating solution is quantitatively extracted using a third injection pump; the sample is then dripped dropwise into a beaker at a constant speed using a glass dropper; the total number of droplets N is automatically recorded by a droplet sensor located above the beaker; and the total weight W_total of the droplets is recorded by a weighing sensor located below the beaker; the average weight of a single drop is then calculated. The concentration of wetting agent in the sample is calculated based on the pre-established standard curve of average weight of a single drop versus concentration of wetting agent.

[0029] Above, refer to Figure 1 An online analysis system and method for nickel plating solution of integrated circuits according to embodiments of the present invention are described. The system enables fully automated, real-time, and online quantitative analysis of multiple components in the nickel plating solution, such as nickel ions, chloride ions, boric acid, 110AD3 additive, copper ion impurities, and wetting agents, thereby improving analysis efficiency, reducing labor costs, and ensuring process stability.

[0030] It should be noted that, in this specification, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus. Unless otherwise specified, an element defined by the phrase "comprising..." does not exclude the presence of additional identical elements in the process, method, article, or apparatus that includes that element.

[0031] Although the present invention has been described in detail through the preferred embodiments above, it should be understood that the above description should not be considered as a limitation of the present invention. Various modifications and substitutions to the present invention will be apparent to those skilled in the art after reading the above description. Therefore, the scope of protection of the present invention should be defined by the appended claims.

Claims

1. An online analysis system for nickel plating solution of integrated circuits, characterized in that, Include: The sampling unit is used to circulate samples from the nickel plating bath to obtain nickel plating solution samples; The liquid delivery unit includes multiple peristaltic pumps and syringe pumps with measurable volumes for quantitatively delivering the nickel plating solution sample and various chemicals to the corresponding analysis locations; A reaction vessel is used for titration and colorimetric reactions in boric acid and chloride ion analysis. The reaction vessel is equipped with a stir bar driven by a motor. The wetting agent analysis unit includes a beaker, a weighing sensor, and a droplet sensing sensor. The beaker is a container for wetting agent analysis. The weighing sensor is located below the beaker, and the droplet sensing sensor is located above the beaker. The testing instruments include a spectrometer, pH electrode, silver electrode, and ICP analyzer; The control and data processing unit is electrically connected to the sampling unit, liquid delivery unit, detection instrument and wetting agent analysis unit, and is used to control the operation of each unit and collect analysis data; The pH electrode is used to detect the endpoint of boric acid titration, the silver electrode is used to detect the endpoint of chloride ion titration, the spectrometer is used to detect the absorbance of nickel ions and additives, the ICP analyzer is used to detect the signal intensity of copper ions, and the weighing sensor and droplet sensing sensor work together to perform the drop weight method analysis of the wetting agent.

2. The online analysis system for nickel plating solution of integrated circuits as described in claim 1, characterized in that, The liquid delivery unit includes: A first peristaltic pump is used to deliver mannitol into the reaction vessel; A second peristaltic pump is used to deliver pure water into the reaction vessel; A third peristaltic pump is used to deliver ammonia water into the reaction vessel; A first injection pump is used to draw sodium hydroxide solution and titrate it in the reaction vessel; A second syringe pump is used to draw silver nitrate standard solution and titrate it in the reaction vessel; A third injection pump is used for quantitative sampling and droplet injection into the beaker for wetting agent analysis.

3. The online analysis system for nickel plating solution of integrated circuits as described in claim 2, characterized in that, In the aforementioned wetting agent analysis unit, the third injection pump drips the sample into the beaker at a uniform rate through a glass dropper.

4. An online analysis method for nickel plating solution of integrated circuits, comprising the online analysis system for nickel plating solution of integrated circuits as described in any one of claims 1 to 3, characterized in that, Includes the following steps: Step S1: Samples are circulated from the nickel plating tank through the sampling unit, and the nickel plating solution sample is obtained after filtration; Step S2: The sample is quantitatively distributed to each analysis position using the liquid delivery unit; Step S3: Perform the following analysis operations: Boric acid analysis: The sample is placed in a reaction vessel, mannitol is added for complexation, and then titrated with sodium hydroxide standard solution. The titration endpoint is detected by pH electrode, and the boric acid concentration is calculated. Chloride ion analysis: The sample is placed in a reaction vessel and titrated with silver nitrate standard solution. The titration endpoint is detected by a silver electrode, and the chloride ion concentration is calculated. Nickel ion analysis: The diluted sample is passed through a spectrometer to measure the absorbance at a characteristic wavelength and the nickel ion concentration is calculated. Additive analysis: The diluted sample was passed through a spectrometer to measure the absorbance at characteristic wavelengths and the concentration of 110AD3 additive was calculated. Copper ion analysis: The sample is sent to an ICP analyzer to measure the copper signal intensity and calculate the copper ion concentration; Wetting agent analysis: The sample is quantitatively sampled by a syringe pump and dripped into a beaker at a constant rate through a glass dropper. The total number of drops is recorded by a droplet sensor located above the beaker and the total weight is recorded by a weighing sensor located below the beaker. The average weight of a single drop is calculated, and the wetting agent concentration is then analyzed. Step S4: The control and data processing unit collects the detection data, calculates and outputs the concentration results of each component.

5. The online analysis method for nickel plating solution of integrated circuits as described in claim 4, characterized in that, The specific steps of boric acid analysis in step S3 are as follows: a quantitative sample of nickel plating solution is placed in a reaction vessel, and mannitol solution is drawn into the reaction vessel by a first peristaltic pump to allow mannitol to undergo a complexation reaction with boric acid in the sample; sodium hydroxide standard solution is added dropwise to the reaction vessel by a first syringe pump, while the pH value of the reaction solution is monitored in real time by a pH electrode; when the pH value changes abruptly, the titration endpoint is determined to have been reached, the amount of sodium hydroxide standard solution consumed is recorded, and the boric acid concentration in the sample is calculated.

6. The online analysis method for nickel plating solution of integrated circuits as described in claim 4, characterized in that, The specific steps of chloride ion analysis in step S3 are as follows: a quantitative sample of nickel plating solution is placed in a reaction cup, and silver nitrate standard solution is added dropwise to the reaction cup through a second injection pump to allow silver ions to react with chloride ions in the sample to form silver chloride precipitate; the concentration change of silver ions in the reaction solution is monitored in real time through a silver electrode; when the concentration of silver ions changes abruptly, the titration endpoint is determined to have been reached, the amount of silver nitrate standard solution consumed is recorded, and the concentration of chloride ions in the sample is calculated.

7. The online analysis method for nickel plating solution of integrated circuits as described in claim 4, characterized in that, The specific steps for nickel ion analysis and additive analysis in step S3 are as follows: take a nickel plating solution sample, dilute it with deionized water to a predetermined ratio, mix it well, and then pass it into a spectrometer. Measure the absorbance at the characteristic absorption wavelength of nickel ions and the characteristic absorption wavelength of the additives, and then calculate the concentrations of nickel ions and additives in the sample.

8. The online analysis method for nickel plating solution of integrated circuits as described in claim 4, characterized in that, The specific steps of the wetting agent analysis in step S3 are as follows: A sample of the nickel plating solution is quantitatively extracted using a third injection pump; the sample is then dripped dropwise into a beaker at a constant speed using a glass dropper; the total number of droplets N is automatically recorded by a droplet sensor located above the beaker; and the total weight W_total of the droplets is recorded by a weighing sensor located below the beaker; the average weight per drop is then calculated. The concentration of wetting agent in the sample is calculated based on the pre-established standard curve of average weight of a single drop versus concentration of wetting agent.

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