Flow regulation and control method and system for etching liquid preparation, terminal and medium

By real-time monitoring and dynamic adjustment of organic acid flow rate and stirring speed, the problem of low efficiency caused by the reduction of ammonia concentration in the etching solution preparation process was solved, achieving more efficient etching solution preparation and equipment utilization.

CN122018576AInactive Publication Date: 2026-05-12SICHUAN JIANGHUA MICROELECTRONIC MATERIALS CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SICHUAN JIANGHUA MICROELECTRONIC MATERIALS CO LTD
Filing Date
2026-04-14
Publication Date
2026-05-12
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

In the existing process of preparing oxalic acid-based ITO etching solutions, the reaction between organic acids and ammonia water leads to a decrease in the concentration of ammonia water in the mixed solution, which slows down the reaction rate and affects the efficiency of etching solution preparation.

Method used

By monitoring the temperature and ammonia concentration in the additive mixing tank in real time, the target flow rate and stirring speed of the organic acid are dynamically adjusted to generate an updated target flow rate of the organic acid, and the etching solution is prepared according to the updated flow rate and speed.

Benefits of technology

It improved the efficiency of etching solution preparation, shortened the preparation time per batch, and increased the equipment capacity utilization rate.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a flow regulation and control method and system for etching liquid preparation, a terminal and a medium, and relates to the technical field of etching liquid preparation. According to the main technical scheme, the initial ammonia water concentration in an additive stirring tank is obtained; organic acid is discharged into the ammonia water diluent according to the initial organic acid target flow; collecting target parameters in the additive stirring tank in real time; the target parameters comprise real-time temperature and real-time ammonia water concentration; generating updated organic acid target flow according to the initial organic acid target flow, the temperature early warning value, the real-time temperature, the real-time ammonia water concentration and the initial ammonia water concentration; and replacing the initial organic acid target flow with the updated organic acid target flow. The invention aims to achieve the purposes of dynamically increasing the flow, fully utilizing the temperature control safety margin released due to the reduction of the reactant concentration, further effectively reducing the risk of maintaining low-efficiency conservative flow for a long time in the later period of the reaction, greatly shortening the preparation time of a single batch of etching liquid and improving the productivity utilization rate of equipment by dynamically increasing the flow and further effectively reducing the risk of maintaining low-efficiency conservative flow for a long time.
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Description

Technical Field

[0001] This invention relates to the field of etching solution preparation technology, and specifically to a method, system, terminal, and medium for flow control in etching solution preparation. Background Technology

[0002] Etching solutions can be classified into compatible etching solutions, acetic acid etching solutions, and oxalic acid etching solutions. Among them, oxalic acid etching solutions are mainly obtained by mixing oxalic acid, etching solution additives, and ultrapure water. When preparing etching solution additives, organic acids, such as hexanoic acid, are often simply mixed with ammonia and ultrapure water.

[0003] The prior art discloses an automated flow control method and system for preparing oxalic acid-based ITO etching solution, comprising: calculating the required amount of solution to be prepared based on the required amount of ITO etching solution; discharging ammonia water into additive ultrapure water and mixing it evenly with the additive ultrapure water to obtain an ammonia water dilution; calculating the target flow rate of organic acid based on the temperature warning value and the required amount of organic acid; discharging organic acid into the ammonia water dilution using a discharge regulating valve, the target flow rate of organic acid, and the required amount of organic acid, and stirring it evenly to obtain an etching solution additive; discharging ultrapure water into an etching solution stirring tank to obtain etching solution ultrapure water; discharging oxalic acid into the etching solution ultrapure water and discharging the etching solution additive into the etching solution stirring tank and stirring it evenly to obtain an oxalic acid-based ITO etching solution.

[0004] However, in actual use, when organic acids are gradually added to the ammonia dilution solution at the target flow rate, the organic acids react with the ammonia, causing the concentration of ammonia in the mixture to gradually decrease. This leads to a reduction in the reaction rate between the organic acids and ammonia, resulting in a decrease in the exothermic reaction rate and consequently a slower rate of temperature rise in the additive mixing tank. Therefore, continuing to add organic acids at the original target flow rate will significantly reduce the efficiency of etching solution preparation. Summary of the Invention

[0005] The purpose of this invention is to provide a flow rate control method, system, terminal and medium for etching solution preparation, which solves the problem that the existing automated flow rate control method and system for oxalic acid-based ITO etching solution preparation greatly reduces the efficiency of etching solution preparation in actual use.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0007] In a first aspect, a method for controlling the flow rate of an etching solution is provided, comprising the following operations:

[0008] S1, Obtain the initial ammonia concentration in the ammonia dilution solution in the additive mixing tank;

[0009] S2, control the discharge regulating valve in the organic acid storage tank to discharge organic acid into the ammonia dilution solution according to the initial target flow rate of organic acid, and stir evenly;

[0010] S3, Real-time acquisition of target parameters in the additive mixing tank; the target parameters include real-time temperature and real-time ammonia concentration;

[0011] S4. Based on the initial target flow rate of organic acid, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration, generate the updated target flow rate of organic acid.

[0012] S5, replace the initial organic acid target flow rate with the updated organic acid target flow rate;

[0013] S6. Repeat steps S2 to S5 until the total amount of organic acids discharged into the ammonia dilution reaches the required amount of organic acids.

[0014] A further step is to include, prior to S5, the following: dynamically adjust the stirring speed in the additive mixing tank based on the updated target flow rate of the organic acid and the initial target flow rate of the organic acid.

[0015] A further solution is: the method for dynamically adjusting the stirring speed in the additive mixing tank includes: determining whether the updated target flow rate of the organic acid is greater than the initial target flow rate of the organic acid; if the updated target flow rate of the organic acid is greater than the initial target flow rate of the organic acid, increasing the stirring speed in the additive mixing tank; if the updated target flow rate of the organic acid is equal to the initial target flow rate of the organic acid, maintaining the stirring speed in the additive mixing tank; if the updated target flow rate of the organic acid is less than the initial target flow rate of the organic acid, decreasing the stirring speed in the additive mixing tank.

[0016] A further proposed approach is to generate an initial target flow rate of organic acid based on the temperature warning value, the demand for organic acid, the heat dissipation rate, the initial temperature inside the additive mixing tank, the surface area inside the additive mixing tank, the temperature outside the additive mixing tank, the specific heat capacity of the mixture, and the demand for ammonia.

[0017] In a second aspect, a flow control system for preparing an etching solution is provided, the flow control system being applicable to the flow control method described in the first aspect, the flow control system comprising:

[0018] The acquisition module is used to execute S1 to obtain the initial ammonia concentration in the ammonia dilution solution in the additive stirring tank.

[0019] The control module is used to execute S2 to control the discharge regulating valve in the organic acid storage tank to discharge organic acid into the ammonia dilution solution according to the initial target flow rate of organic acid, and to stir it evenly;

[0020] The acquisition module is used to execute S3 to acquire target parameters in the additive mixing tank in real time; the target parameters include real-time temperature and real-time ammonia concentration.

[0021] A generation module is used to execute S4 to generate an updated organic acid target flow rate based on the initial organic acid target flow rate, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration.

[0022] The setting module is used to execute S5 to replace the initial organic acid target flow rate with the updated organic acid target flow rate;

[0023] An execution module is used to execute S6 to repeat steps S2 to S5 until the total amount of organic acids discharged into the ammonia dilution reaches the required amount of organic acids.

[0024] Thirdly, a terminal is provided, including a processor and a memory, the memory being used to store processor-executable instructions; wherein the processor is configured to invoke the instructions stored in the memory to execute the flow control method as described in the first aspect.

[0025] Fourthly, a computer-readable storage medium is provided, having stored thereon computer program instructions that, when executed by a processor, implement the flow control method as described in the first aspect.

[0026] Compared with the prior art, the beneficial effects of the present invention are:

[0027] The etching solution preparation flow control method in this embodiment generates an updated organic acid target flow rate based on the initial target flow rate of organic acid, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration. Organic acid is then discharged into the ammonia dilution solution according to the updated target flow rate. The aim is to dynamically increase the flow rate to fully utilize the temperature control safety margin "released" due to the decrease in reactant concentration, thereby effectively reducing the risk of maintaining an inefficient and conservative flow rate for an extended period in the later stages of the reaction. This significantly shortens the preparation time of a single batch of etching solution and improves equipment capacity utilization. Attached Figure Description

[0028] Figure 1 This is a schematic flowchart of a flow control method for preparing an etching solution in this embodiment. Detailed Implementation

[0029] The invention will now be further described with reference to the accompanying drawings.

[0030] Example 1: This example provides a method for controlling the flow rate of an etching solution, such as... Figure 1 As shown, the following operations are included:

[0031] S100. Obtain the initial ammonia concentration in the ammonia dilution solution in the additive mixing tank;

[0032] For example, during implementation, before discharging the organic acid from the organic acid storage tank into the ammonia dilution in the additive mixing tank, the initial ammonia concentration in the ammonia dilution in the additive mixing tank is measured by an online concentration sensor (such as a conductivity meter, pH meter, or near-infrared spectrometer).

[0033] S200. Control the discharge regulating valve in the organic acid storage tank to discharge organic acid into the ammonia dilution solution according to the initial target flow rate of organic acid, and stir evenly;

[0034] In this embodiment, the initial target flow rate of organic acid is generated based on the temperature warning value, the demand for organic acid, the heat dissipation rate, the initial temperature in the additive mixing tank, the surface area in the additive mixing tank, the temperature outside the additive mixing tank, the specific heat capacity of the mixture, and the demand for ammonia.

[0035] For example, during implementation, based on the temperature warning value, organic acid demand, heat dissipation rate, initial temperature in the additive mixing tank, surface area in the additive mixing tank, temperature outside the additive mixing tank, mixing specific heat capacity, and ammonia demand, the target organic acid flow rate is calculated using the organic acid flow rate adjustment formula, and this target organic acid flow rate is recorded as the initial target organic acid flow rate. The organic acid flow rate adjustment formula is shown in equation (1):

[0036] (1)

[0037] in, Indicates the temperature warning value; Indicates the heating coefficient; This indicates the demand for organic acids; This indicates the target flow rate of organic acids (i.e., the initial target flow rate of organic acids). Indicates the heat dissipation rate; This indicates the initial temperature inside the additive mixing tank; Indicates the heat dissipation coefficient; This indicates the surface area inside the additive mixing tank; This indicates the temperature outside the additive mixing tank; Indicates the specific heat capacity of the mixture; This indicates the amount of ammonia required.

[0038] The opening of the discharge regulating valve in the organic acid storage tank is controlled according to the initial target flow rate of organic acid, so that the organic acid in the organic acid storage tank is discharged into the ammonia dilution solution in the additive stirring tank according to the initial target flow rate of organic acid, and is stirred evenly at a certain stirring speed.

[0039] S300. Real-time acquisition of target parameters within the additive mixing tank; the target parameters include real-time temperature and real-time ammonia concentration;

[0040] For example, during the implementation process, while the organic acid in the organic acid storage tank is discharged into the ammonia dilution solution in the additive mixing tank according to the initial target flow rate of organic acid, and is stirred uniformly at a certain stirring speed, the target parameters such as the real-time temperature and real-time ammonia concentration in the additive mixing tank are collected in real time.

[0041] S400. Generate an updated target flow rate for organic acids based on the initial target flow rate of organic acids, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration.

[0042] For example, during implementation, the updated target flow rate of organic acid is calculated and generated based on the initial target flow rate of organic acid, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration. The calculation formula for the updated target flow rate of organic acid is shown in (2):

[0043] (2)

[0044] in, This indicates the updated target flow rate of organic acids; This indicates the target flow rate of organic acids (i.e., the initial target flow rate of organic acids). This represents the temperature feedback adjustment coefficient; This indicates the time when the real-time temperature and ammonia concentration in the additive mixing tank are collected. express Real-time temperature of the additive mixing tank, collected continuously. express The concentration of ammonia in the additive mixing tank was collected at all times; This indicates the initial ammonia concentration in the ammonia dilution solution within the additive mixing tank.

[0045] S500. Replace the initial organic acid target flow rate with the updated organic acid target flow rate;

[0046] For example, during implementation, the updated target flow rate of organic acids is utilized. Replace the initial target flow rate of organic acids .

[0047] S600. Repeat steps S200 to S500 until the total amount of organic acids discharged into the ammonia dilution reaches the required amount of organic acids.

[0048] For example, during implementation, based on the updated target flow rate of organic acids Control the opening of the discharge regulating valve in the organic acid storage tank to meet the updated target flow rate of the organic acid. The organic acid in the organic acid storage tank is discharged into the ammonia dilution solution in the additive mixing tank, and stirred evenly at a certain stirring speed. Steps S200 to S500 are repeated. While discharging the organic acid from the organic acid storage tank into the ammonia dilution solution in the additive mixing tank, the cumulative total amount of organic acid discharged into the additive mixing tank is simultaneously collected until the cumulative total amount of organic acid reaches the required amount. At this point, the discharge regulating valve in the organic acid storage tank is immediately closed.

[0049] The etching solution preparation flow control method in this embodiment generates an updated organic acid target flow rate based on the initial target flow rate of organic acid, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration. Organic acid is then discharged into the ammonia dilution solution according to the updated target flow rate. The aim is to dynamically increase the flow rate to fully utilize the temperature control safety margin "released" due to the decrease in reactant concentration, thereby effectively reducing the risk of maintaining an inefficient and conservative flow rate for an extended period in the later stages of the reaction. This significantly shortens the preparation time of a single batch of etching solution and improves equipment capacity utilization.

[0050] In this embodiment, before S500, the method further includes: dynamically adjusting the stirring speed in the additive mixing tank based on the updated target flow rate of the organic acid and the initial target flow rate of the organic acid.

[0051] In this embodiment, the method for dynamically adjusting the stirring speed in the additive mixing tank includes: determining whether the updated target flow rate of the organic acid is greater than the initial target flow rate of the organic acid; if the updated target flow rate of the organic acid is greater than the initial target flow rate of the organic acid, increasing the stirring speed in the additive mixing tank; if the updated target flow rate of the organic acid is equal to the initial target flow rate of the organic acid, maintaining the stirring speed in the additive mixing tank; and if the updated target flow rate of the organic acid is less than the initial target flow rate of the organic acid, decreasing the stirring speed in the additive mixing tank.

[0052] For example, during implementation, the updated target flow rate of organic acids is utilized. Replace the initial target flow rate of organic acids Before that, determine the updated target flow rate of organic acids. Is it greater than the initial target flow rate of organic acids? .

[0053] If the updated target flow rate of organic acids Greater than the initial target flow rate of organic acids To increase the mixing speed in the additive mixing tank, the aim is twofold: firstly, to enhance mixing intensity, thereby reducing the risk of localized overheating or side reactions caused by the increased instantaneous injection of organic acid, which could lead to excessively high local concentrations and concentrated, violent exothermic reactions. Secondly, as the organic acid flow rate increases, the mixing speed is simultaneously increased to rapidly disperse the newly added organic acid, further reducing the risk of excessively high local acid concentrations and ensuring sufficient and uniform contact between the organic acid and ammonia, thus maximizing the neutralization reaction rate.

[0054] If the updated target flow rate of organic acids Equal to the initial target flow rate of organic acids This maintains the stirring speed within the additive mixing tank, aiming to ensure a stable reaction.

[0055] If the updated target flow rate of organic acids Less than the initial target flow rate of organic acids This reduces the stirring speed in the additive mixing tank. The aim is to reduce unnecessary mechanical energy consumption while ensuring thorough mixing, thereby reducing the risk of shear forces disturbing the system (especially at the later stages of the reaction) and extending the service life of the equipment.

[0056] Example 2: This example provides a flow control system for preparing etching solution. The flow control system is applicable to the flow control method described in Example 1. The flow control system includes an acquisition module, a control module, a collection module, a generation module, a setting module, and an execution module.

[0057] The acquisition module performs step S100 to obtain the initial ammonia concentration in the ammonia dilution solution within the additive mixing tank. The control module performs step S200 to control the discharge regulating valve in the organic acid storage tank to discharge organic acid into the ammonia dilution solution according to the initial target flow rate and to stir it evenly. The acquisition module performs step S300 to collect the target parameters within the additive mixing tank in real time, including the real-time temperature and real-time ammonia concentration. The generation module performs step S400 to generate an updated target flow rate for organic acid based on the initial target flow rate, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration. The setting module performs step S500 to replace the initial target flow rate with the updated target flow rate. The execution module performs step S600 to repeat steps S200 to S500 until the total cumulative amount of organic acid discharged into the ammonia dilution solution reaches the required amount of organic acid.

[0058] The etching solution preparation flow control system in this embodiment utilizes a generation module to generate an updated organic acid target flow rate based on the initial target flow rate of the organic acid, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration. The control module then discharges the organic acid into the ammonia dilution solution according to the updated target flow rate. The aim is to dynamically increase the flow rate to fully utilize the temperature control safety margin "released" due to the decrease in reactant concentration, thereby effectively reducing the risk of maintaining an inefficient and conservative flow rate for an extended period in the later stages of the reaction. This significantly shortens the preparation time for a single batch of etching solution and improves equipment capacity utilization.

[0059] In this embodiment, a terminal is also provided, including a processor and a memory, the memory being used to store processor-executable instructions; wherein the processor is configured to invoke the instructions stored in the memory to execute the flow control method as described in Embodiment 1.

[0060] In this embodiment, a computer-readable storage medium is also provided, on which computer program instructions are stored, which, when executed by a processor, implement the flow control method as described in Embodiment 1.

[0061] Although the invention has been described herein with reference to several illustrative embodiments, it should be understood that many other modifications and implementations can be devised by those skilled in the art, which will fall within the scope and spirit of the principles disclosed herein. More specifically, various variations and modifications can be made to the components and / or layout of the subject matter arrangement within the scope of the disclosure, drawings, and claims. Besides variations and modifications to the components and / or layout, other uses will be apparent to those skilled in the art.

Claims

1. A method for controlling the flow rate of an etching solution, characterized in that, Includes the following operations: S1, Obtain the initial ammonia concentration in the ammonia dilution solution in the additive mixing tank; S2, control the discharge regulating valve in the organic acid storage tank to discharge organic acid into the ammonia dilution solution according to the initial target flow rate of organic acid, and stir evenly; S3, Real-time acquisition of target parameters in the additive mixing tank; the target parameters include real-time temperature and real-time ammonia concentration; S4. Based on the initial target flow rate of organic acid, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration, generate the updated target flow rate of organic acid. S5, replace the initial organic acid target flow rate with the updated organic acid target flow rate; S6. Repeat steps S2 to S5 until the total amount of organic acids discharged into the ammonia dilution reaches the required amount of organic acids.

2. The flow control method according to claim 1, characterized in that, The S5 also includes: dynamically adjusting the stirring speed in the additive mixing tank based on the updated target flow rate of organic acids and the initial target flow rate of organic acids.

3. The flow control method according to claim 2, characterized in that, The method for dynamically adjusting the stirring speed in the additive mixing tank includes: determining whether the updated target flow rate of the organic acid is greater than the initial target flow rate of the organic acid; if the updated target flow rate of the organic acid is greater than the initial target flow rate of the organic acid, increasing the stirring speed in the additive mixing tank; if the updated target flow rate of the organic acid is equal to the initial target flow rate of the organic acid, maintaining the stirring speed in the additive mixing tank; and if the updated target flow rate of the organic acid is less than the initial target flow rate of the organic acid, decreasing the stirring speed in the additive mixing tank.

4. The flow control method according to claim 1, characterized in that: The initial target flow rate of organic acid is generated based on the temperature warning value, the demand for organic acid, the heat dissipation rate, the initial temperature inside the additive mixing tank, the surface area inside the additive mixing tank, the temperature outside the additive mixing tank, the specific heat capacity of the mixture, and the demand for ammonia.

5. A flow control system for preparing an etching solution, characterized in that, The flow control system is applicable to the flow control method as described in any one of claims 1-4, and the flow control system comprises: The acquisition module is used to execute S1 to obtain the initial ammonia concentration in the ammonia dilution solution in the additive stirring tank. The control module is used to execute S2 to control the discharge regulating valve in the organic acid storage tank to discharge organic acid into the ammonia dilution solution according to the initial target flow rate of organic acid, and to stir it evenly; The acquisition module is used to execute S3 to acquire target parameters in the additive mixing tank in real time; the target parameters include real-time temperature and real-time ammonia concentration. A generation module is used to execute S4 to generate an updated organic acid target flow rate based on the initial organic acid target flow rate, temperature warning value, real-time temperature, real-time ammonia concentration, and initial ammonia concentration. The setting module is used to execute S5 to replace the initial organic acid target flow rate with the updated organic acid target flow rate; An execution module is used to execute S6 to repeat steps S2 to S5 until the total amount of organic acids discharged into the ammonia dilution reaches the required amount of organic acids.

6. A terminal, characterized in that, include: A processor and a memory, wherein the memory is used to store processor-executable instructions; The processor is configured to invoke instructions stored in the memory to execute the flow control method as described in any one of claims 1-4.

7. A computer-readable storage medium having computer program instructions stored thereon, characterized in that, When the computer program instructions are executed by the processor, they implement the flow control method as described in any one of claims 1-4.