Preparation method of titanium etching solution

Abstract

The invention discloses a preparation method of a titanium etching solution, which comprises the following steps: S1, dividing 88.75-96.25 parts of water into three parts of A, B and C according to a volume ratio of 10: 1: 1, and the two parts of B and C are equal in quantity; s2, mixing 2.5-7.5 parts of ferric salt with B parts of water to obtain ferric salt premixed liquid; s3, mixing 1.25-3.75 parts of ammonium bifluoride with C parts of water to obtain an ammonium bifluoride premixed solution; s4, mixing the iron salt premixed solution obtained in the step S2 with the ammonium bifluoride premixed solution obtained in the step S3 to obtain an intermediate mixed solution; and S5, slowly adding the part A of water into the intermediate mixed solution obtained in the step S4, and detecting for multiple times to obtain the final titanium etching solution. According to the invention, on one hand, the etching effect on peptide products is ensured, and on the other hand, environmental pollution and harm to human bodies are reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of titanium etching liquid, and more specifically, particularly relates to a preparation method of titanium etching liquid. Background Art

[0002] Examples of techniques for processing such metal films to form patterns such as wiring microstructures include wet etching techniques and dry etching techniques. Among them, wet etching uses chemical reagents, and the photoresist pattern formed on the surface of the metal film by photolithography is used as a shield for chemical etching to form a pattern on the metal film. Wet etching technology is economical and does not require expensive equipment, but uses relatively cheap chemical reagents. Using this wet etching technology, a large area of ​​the substrate can be uniformly etched, and the production efficiency per unit time is high.

[0003] In the past, etching compositions containing acids and oxidants were often used to etch aluminum, chromium or silver metals and their alloys. However, due to the different etching degrees and the different types of metals to be etched, the best etching effect is achieved by properly selecting the types of acids and oxidants and then adjusting the concentrations appropriately. Although there are currently a variety of etching liquid compositions for silver alloys, their etching effects on titanium products are not ideal. Therefore, we propose a method for preparing a titanium etching liquid. Summary of the invention

[0004] The purpose of the present invention is to solve the shortcomings of the prior art and to propose a method for preparing a titanium etching solution, which, on the one hand, ensures the etching effect on peptide products and, on the other hand, reduces environmental pollution and harm to the human body.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A method for preparing a titanium etching solution, wherein the raw materials for preparing the titanium etching solution are 88.75-96.25 parts of water, 2.5-7.5 parts of iron salt, and 1.25-3.75 parts of ammonium bifluoride;

[0007] The preparation method comprises the following steps:

[0008] S1. Divide 88.75-96.25 parts of water into three parts: A, B, and C, with a volume ratio of 10:1:1, of which B and C are equal in volume;

[0009] S2, mix 2.5-7.5 parts of iron salt with B parts of water to obtain an iron salt premix;

[0010] S3, mixing 1.25-3.75 parts of ammonium bifluoride with C parts of water to obtain an ammonium bifluoride premix solution;

[0011] S4, mixing the iron salt premix solution obtained in step S2 and the ammonium bifluoride premix solution obtained in step S3 to obtain an intermediate mixed solution;

[0012] S5. Slowly add A portion of water to the intermediate mixed solution obtained in step S4, and perform multiple tests to obtain a final titanium etching solution.

[0013] Preferably, the iron salt is one or more of ferric sulfate or ferric chloride.

[0014] Preferably, the multiple tests in step S5 include measuring the pH value of the mixed solution and the concentrations of iron salt and ammonium bifluoride to ensure the stability and etching effect of the titanium etching solution.

[0015] Preferably, the specific process of step S5 is:

[0016] S51. Ensure that A portion of water has been prepared in a container that is easy to control, and slowly add A portion of water to the intermediate mixture to promote the smooth progress of the reaction in the mixture and avoid any possible violent reaction or formation of precipitates;

[0017] S52. During the water adding process, the intermediate mixed liquid is continuously stirred to ensure that the A portion of water is fully mixed with the mixed liquid to avoid local uneven mixing;

[0018] S53. After the addition of A portion of water is completed, a preliminary test is performed, including measuring the pH value, the concentration of iron salt and ammonium bifluoride to ensure that they are within the expected range;

[0019] S54. Based on the initial test results, further adjust the composition of the solution and continue to perform multiple tests until the desired chemical and physical parameters are achieved.

[0020] Preferably, if the test result in step S54 shows that some parameters do not meet the requirements, more water, iron salt or ammonium bifluoride needs to be added to adjust the ratio, and the performance of the titanium etching solution is optimized by fine-tuning the formula to ensure the best etching effect on the titanium material.

[0021] Preferably, step S5 further includes detecting the viscosity of the titanium etching solution by using a spectrophotometer to measure the chemical properties of the liquid and further infer its viscosity.

[0022] Preferably, in step S5, multiple tests and adjustments are determined by feedback control algorithm and chemical analysis algorithm to ensure the etching effect on the titanium material, specifically:

[0023] Feedback control algorithm, which monitors the pH value, temperature and concentration of the etching solution in real time through sensors; the sensors send the collected data to the detection system and compare them with the preset target values;

[0024] If the detected parameter deviates from the target value, the control system will automatically calculate the deviation and issue an adjustment instruction;

[0025] Correct the deviation by adjusting the amount of water, iron salt or ammonium bifluoride added to ensure that the composition of the etching solution always meets the requirements;

[0026] The control system will continuously optimize and adjust strategies based on historical data and real-time data to improve the accuracy of detection and adjustment; the dynamic optimization process can effectively respond to the impact of raw material quality fluctuations and environmental changes.

[0027] Preferably, the chemical analysis algorithm is specifically:

[0028] The absorbance of the liquid was measured using a spectrophotometer, and the concentrations of iron salt and ammonium bifluoride were calculated using the standard curve method;

[0029] The stability of the etching solution is evaluated through chemical analysis algorithms, including the determination of hydrofluoric acid content, which can determine the stability of the etching solution and its potential rheological properties. According to the stability evaluation results, the formula is adjusted in time to ensure that the etching solution maintains constant performance during long-term use;

[0030] By monitoring the decomposition rate of hydrogen peroxide, the activity change of the etching solution can be predicted, so as to arrange the production plan reasonably.

[0031] Preferably, the adjustment of pH value is usually based on the principle of acid-base titration, and the expression is:

[0032]

[0033] Among them, the slope of the titration curve depends on the nature and concentration of the added acid or base;

[0034] The viscosity is modeled using empirical formulas or experimental data, and the expression is:

[0035] η=k×C+b;

[0036] Among them, η is the viscosity, C is the concentration of a key component, and k and b are coefficients obtained from experimental data.

[0037] The present invention provides a method for preparing a titanium etching solution. Compared with the conventional technology, the titanium etching solution prepared by the present invention has the following effects:

[0038] Improve etching accuracy: By precisely controlling the chemical composition and concentration, more accurate etching of titanium materials can be achieved, meeting the high precision requirements of industries such as microelectronics manufacturing.

[0039] Enhanced stability: Chemical analysis algorithms are used to evaluate the stability of the etching solution, and the formula is adjusted in a timely manner to ensure that the etching solution maintains constant performance during long-term use, reducing product defects caused by fluctuations in etching solution performance.

[0040] Improve production efficiency: Real-time monitoring and adjustment of key parameters of etching solution through feedback control algorithm reduces the need for manual intervention and improves the automation and efficiency of the production process.

[0041] Reduce production costs: Optimizing the use ratio of raw materials and reducing the generation of waste liquid can help reduce production costs while reducing the impact on the environment.

[0042] Ensure environmental safety: Strict control of the use and handling of chemicals reduces the emission of harmful substances and helps protect the environment and the health of operators.

[0043] Strong adaptability: The flexibility of the preparation method allows the formulation of the etching solution to be adjusted according to different titanium materials and application requirements, enhancing the adaptability to different process conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 The present invention is a flow chart of the preparation method of the titanium etching solution;

[0045] Figure 2 The present invention is a flow chart of a method for preparing titanium etching solution from an intermediate mixed solution. DETAILED DESCRIPTION

[0046] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0047] The invention provides a method for preparing a titanium etching solution. The raw materials for preparing the titanium etching solution are 88.75-96.25 parts of water, 2.5-7.5 parts of iron salt and 1.25-3.75 parts of ammonium hydrogen fluoride; wherein the iron salt is one or more of iron sulfate or iron chloride.

[0048] like Figure 1 As shown, the preparation method comprises the following steps:

[0049] S1. Divide 88.75-96.25 parts of water into three parts: A, B, and C, with a volume ratio of 10:1:1, of which B and C are equal in volume;

[0050] S2, mix 2.5-7.5 parts of iron salt with B parts of water to obtain an iron salt premix;

[0051] S3, mixing 1.25-3.75 parts of ammonium bifluoride with C parts of water to obtain an ammonium bifluoride premix solution;

[0052] S4, mixing the iron salt premix solution obtained in step S2 and the ammonium bifluoride premix solution obtained in step S3 to obtain an intermediate mixed solution;

[0053] S5, slowly adding A part of water to the intermediate mixed solution obtained in step S4, and performing multiple tests to obtain a final titanium etching solution. The multiple tests in step S5 include measuring the pH value of the mixed solution and the concentrations of iron salt and ammonium bifluoride to ensure the stability and etching effect of the titanium etching solution.

[0054] It should be noted that if Figure 2 As shown, the specific process of step S5 is:

[0055] S51. Ensure that A portion of water has been prepared in a container that is easy to control, and slowly add A portion of water to the intermediate mixture to promote the smooth progress of the reaction in the mixture and avoid any possible violent reaction or formation of precipitates;

[0056] S52. During the water adding process, the intermediate mixed liquid is continuously stirred to ensure that the A portion of water is fully mixed with the mixed liquid to avoid local uneven mixing;

[0057] S53. After the addition of A portion of water is completed, a preliminary test is performed, including measuring the pH value, the concentration of iron salt and ammonium bifluoride to ensure that they are within the expected range;

[0058] S54. According to the initial test results, the composition of the solution is further adjusted, and multiple tests are continued until the required chemical and physical parameters are reached. If the test results in step S54 show that some parameters do not meet the requirements, more water, iron salt or ammonium bifluoride needs to be added to adjust the proportion. By fine-tuning the formula, the performance of the titanium etching solution is optimized to ensure the best etching effect on the titanium material.

[0059] In addition, step S5 also includes detecting the viscosity of the titanium etching solution by using a spectrophotometer to measure the chemical properties of the liquid and then infer its viscosity.

[0060] It should be noted that in step S5, multiple tests and adjustments are determined by feedback control algorithm and chemical analysis algorithm to ensure the etching effect on titanium material, specifically:

[0061] Feedback control algorithm, which monitors the pH value, temperature and concentration of the etching solution in real time through sensors; the sensors send the collected data to the detection system and compare them with the preset target values;

[0062] If the detected parameter deviates from the target value, the control system will automatically calculate the deviation and issue an adjustment instruction;

[0063] Correct the deviation by adjusting the amount of water, iron salt or ammonium bifluoride added to ensure that the composition of the etching solution always meets the requirements;

[0064] The control system will continuously optimize and adjust strategies based on historical data and real-time data to improve the accuracy of detection and adjustment; the dynamic optimization process can effectively cope with the impact of raw material quality fluctuations and environmental changes. The chemical analysis algorithm is as follows:

[0065] The absorbance of the liquid was measured using a spectrophotometer, and the concentrations of iron salt and ammonium bifluoride were calculated using the standard curve method;

[0066] The stability of the etching solution is evaluated through chemical analysis algorithms, including the determination of hydrofluoric acid content, which can determine the stability of the etching solution and its potential rheological properties. According to the stability evaluation results, the formula is adjusted in time to ensure that the etching solution maintains constant performance during long-term use;

[0067] By monitoring the decomposition rate of hydrogen peroxide, the activity change of the etching solution can be predicted, so as to arrange the production plan reasonably.

[0068] In addition, the adjustment of pH value is usually based on the principle of acid-base titration, expressed as:

[0069]

[0070] Among them, the slope of the titration curve depends on the nature and concentration of the added acid or base;

[0071] The viscosity is modeled using empirical formulas or experimental data, and the expression is:

[0072] η=k×C+b;

[0073] Among them, η is the viscosity, C is the concentration of a key component, and k and b are coefficients obtained from experimental data.

[0074] As an option in this embodiment, the viscosity is measured using a viscometer as follows:

[0075] Rotational Viscometer

[0076] A rotational viscometer is one of the most commonly used instruments for measuring viscosity. It evaluates viscosity by measuring the resistance of a liquid to a rotating body. This type of viscometer can measure at different shear rates, providing detailed information about the flow behavior of the liquid. This method is suitable for most liquids, including etching fluids.

[0077] 2. Capillary viscometer

[0078] Capillary viscometers measure viscosity based on the time it takes a liquid to flow through a capillary tube. They are typically used for relatively thin liquids. Although not as widely used as rotational viscometers, they are still valuable in certain applications.

[0079] 3. Vibration Viscometer

[0080] Vibration viscometers measure viscosity by using the damping effect of a liquid on a vibration sensor. The sensor's vibration attenuation is related to the viscosity of the liquid, which can be used to calculate the viscosity value. This method is easy to operate, has a quick response, and is suitable for real-time monitoring and process control.

[0081] 4. UV / Visible Spectrophotometer

[0082] In the detection of the composition of etching liquid, UV / visible spectrophotometer can be used to indirectly measure some chemical properties of the liquid and then infer its viscosity. For example, by measuring the hydrofluoric acid content, the stability of the etching liquid and its potential rheological properties can be understood.

[0083] The viscosity test of etching fluid is an important quality control link to ensure the efficiency and consistency of the etching process. Choosing the right viscosity test method can not only improve production efficiency, but also effectively reduce production costs and improve the quality of the final product. By continuously optimizing the test methods and equipment, the strict requirements of etching fluid accuracy and reliability in industries such as microelectronics manufacturing can be better met.

[0084] In summary, improving etching accuracy: by precisely controlling the chemical composition and concentration, more accurate etching of titanium materials can be achieved, meeting the high precision requirements of industries such as microelectronics manufacturing.

[0085] Enhanced stability: Chemical analysis algorithms are used to evaluate the stability of the etching solution, and the formula is adjusted in a timely manner to ensure that the etching solution maintains constant performance during long-term use, reducing product defects caused by fluctuations in etching solution performance.

[0086] Improve production efficiency: Real-time monitoring and adjustment of key parameters of etching solution through feedback control algorithm reduces the need for manual intervention and improves the automation and efficiency of the production process.

[0087] Reduce production costs: Optimizing the use ratio of raw materials and reducing the generation of waste liquid can help reduce production costs while reducing the impact on the environment.

[0088] Ensure environmental safety: Strict control of the use and handling of chemicals reduces the emission of harmful substances and helps protect the environment and the health of operators.

[0089] Strong adaptability: The flexibility of the preparation method allows the formulation of the etching solution to be adjusted according to different titanium materials and application requirements, enhancing the adaptability to different process conditions.

[0090] Finally, it should be noted that the above are only preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a titanium etching solution, characterized in that: The raw materials for preparing the titanium etching solution are 88.75-96.25 parts of water, 2.5-7.5 parts of iron salt, and 1.25-3.75 parts of ammonium bifluoride; The preparation method comprises the following steps: S1. Divide 88.75-96.25 parts of water into three parts: A, B, and C, with a volume ratio of 10:1:1, of which B and C are equal in volume; S2, mix 2.5-7.5 parts of iron salt with B parts of water to obtain an iron salt premix; S3, mixing 1.25-3.75 parts of ammonium bifluoride with C parts of water to obtain an ammonium bifluoride premix solution; S4, mixing the iron salt premix solution obtained in step S2 and the ammonium bifluoride premix solution obtained in step S3 to obtain an intermediate mixed solution; S5. Slowly add A portion of water to the intermediate mixed solution obtained in step S4, and perform multiple tests to obtain a final titanium etching solution.

2. The method for preparing a titanium etching solution according to claim 1, wherein: The iron salt is one or more of ferric sulfate or ferric chloride.

3. The method for preparing a titanium etching solution according to claim 1, wherein: The multiple tests in step S5 include measuring the pH value of the mixed solution and the concentrations of iron salt and ammonium bifluoride to ensure the stability and etching effect of the titanium etching solution.

4. The method for preparing a titanium etching solution according to claim 3, characterized in that: The specific process of step S5 is as follows: S51. Ensure that A portion of water has been prepared in a container that is easy to control, and slowly add A portion of water to the intermediate mixture to promote the smooth progress of the reaction in the mixture and avoid any possible violent reaction or formation of precipitates; S52. During the water adding process, the intermediate mixed liquid is continuously stirred to ensure that the A portion of water is fully mixed with the mixed liquid to avoid local uneven mixing; S53. After the addition of A portion of water is completed, a preliminary test is performed, including measuring the pH value, the concentration of iron salt and ammonium bifluoride to ensure that they are within the expected range; S54. Based on the initial test results, further adjust the composition of the solution and continue to perform multiple tests until the desired chemical and physical parameters are achieved.

5. The method for preparing a titanium etching solution according to claim 4, characterized in that: If the test result in step S54 shows that some parameters do not meet the requirements, more water, iron salt or ammonium bifluoride needs to be added to adjust the ratio. By fine-tuning the formula, the performance of the titanium etching solution is optimized to ensure the best etching effect on the titanium material.

6. The method for preparing a titanium etching solution according to claim 1, characterized in that: Step S5 also includes detecting the viscosity of the titanium etching solution, using a spectrophotometer to indirectly measure the chemical properties of the liquid, and then inferring its viscosity.

7. The method for preparing a titanium etching solution according to claim 1, characterized in that: In step S5, multiple tests and adjustments are determined by feedback control algorithm and chemical analysis algorithm to ensure the etching effect on titanium material, specifically: Feedback control algorithm, which monitors the pH value, temperature and concentration of the etching solution in real time through sensors; the sensors send the collected data to the detection system and compare them with the preset target values; If the detected parameter deviates from the target value, the control system will automatically calculate the deviation and issue an adjustment instruction; Correct the deviation by adjusting the amount of water, iron salt or ammonium bifluoride added to ensure that the composition of the etching solution always meets the requirements; The control system will continuously optimize and adjust strategies based on historical data and real-time data to improve the accuracy of detection and adjustment; the dynamic optimization process can effectively respond to the impact of raw material quality fluctuations and environmental changes.

8. The method for preparing a titanium etching solution according to claim 7, characterized in that: The chemical analysis algorithm is specifically: The absorbance of the liquid was measured using a spectrophotometer, and the concentrations of iron salt and ammonium bifluoride were calculated using the standard curve method; The stability of the etching solution is evaluated through chemical analysis algorithms, including the determination of hydrofluoric acid content, which can determine the stability of the etching solution and its potential rheological properties. According to the stability evaluation results, the formula is adjusted in time to ensure that the etching solution maintains constant performance during long-term use; By monitoring the decomposition rate of hydrogen peroxide, the activity change of the etching solution can be predicted, so as to arrange the production plan reasonably.

Images