A purity detection method for preparing high-purity ammonia water

Abstract

The present invention discloses a purity detection method for the preparation of high-purity ammonia water, and relates to the technical field of high-purity ammonia water testing. The purity detection method for the preparation of high-purity ammonia water comprises the following steps: real-time monitoring of semi-finished high-purity ammonia water in circulating filtration; performing a semi-finished high-purity ammonia water circulation execution degree analysis according to the original parameters of the semi-finished high-purity ammonia water; performing purity detection and analysis on the semi-finished high-purity ammonia water according to the results of the semi-finished high-purity ammonia water circulation execution degree analysis, and regulating the semi-finished high-purity ammonia water circulation filtration process through a liquid filter according to the results of the semi-finished high-purity ammonia water purity detection and analysis. The present invention achieves the effect of improving the accuracy of the purity detection method for the preparation of pure ammonia water by analyzing the purity detection, evaluation and analysis of the circulation filtration of the preparation of high-purity ammonia water, and regulating the circulation filtration process of the semi-finished high-purity ammonia water according to the analysis results, thereby solving the problem of insufficient accuracy of the purity detection method for the preparation of high-purity ammonia water in the prior art.

Description

Technical Field

[0001] The invention relates to the technical field of high-purity ammonia water testing, and in particular to a purity detection method for preparing high-purity ammonia water. Background Art

[0002] With the wide application of high-purity ammonia in the manufacture of semiconductor and compound semiconductor devices, the purity requirements for ultra-clean high-purity ammonia are increasing with the development of semiconductor industry technology. Impurities such as metal ions and solid particles in ammonia have a significant impact on the manufacturing and yield of products, especially in the manufacture of integrated circuits with small line widths, where a small amount of impurities may cause the circuit to be scrapped.

[0003] The purity detection method of the existing high-purity ammonia water preparation is achieved through the following technologies, including: gas chromatography can be used to analyze the volatile components in the ammonia water; ion chromatography can be used to detect anionic impurities in the ammonia water; plasma mass spectrometry can be used to detect metal elements in the ammonia water; microporous membrane filtration technology can be used to evaluate the impurity content by analyzing the residue on the filter membrane after filtration.

[0004] For example, the patent application with publication number: CN118130823A discloses a device and method for online monitoring of ammonia content, including: a reaction unit, a detection unit and a control unit. The reaction unit includes a reaction tank, an injection pump, and a multi-channel switching valve; a water outlet is provided at the top center of the reaction tank; the injection pump is connected to the main channel of the multi-channel switching valve; the three sub-channels of the multi-channel switching valve are respectively connected to the ammonia sample to be tested, the titration standard solution and the indicator solution through pipelines, and the other three sub-channels are respectively connected to the reaction tank through pipelines; the detection unit includes a light source and a light sensor; the light source and the light sensor are respectively arranged in the middle of the side wall of the reaction tank. The control unit is an embedded controller; the embedded controller is electrically connected to the injection pump, the light source of the multi-channel switching valve, and the light sensor.

[0005] For example, the invention patent announcement with announcement number: CN103033438B discloses a method for detecting the total non-volatile matter content in high-purity and ultra-pure ammonia, comprising: directly passing ammonia into a volumetric flask to dissolve it in water, calculating the mass of ammonia by weighing the mass difference before and after the volumetric flask, and slowly heating the ammonia solution at the same time, first evaporating at a low temperature to release ammonia, and then setting the heating temperature to 100±1°C, after the ammonia solution evaporates to the 100mL scale line, pouring the ammonia solution into an evaporating dish, and after all the ammonia in the evaporating dish is evaporated, heating it in an oven at 100±5°C for 30 minutes, and then cooling it in a dryer for 15 minutes, and then weighing it on an analytical balance and recording the reading, and finally the total non-volatile matter content in the ammonia is obtained by comparing the difference before and after the ammonia solution is evaporated from the evaporating dish and the mass of ammonia dissolved in water.

[0006] However, in the process of implementing the technical solution of the invention in the embodiments of the present application, the present application found that the above technology has at least the following technical problems:

[0007] In the existing technology, the preparation of high-purity ammonia water is relatively complicated, the production environment is relatively strict, the production process is long, and there are many influencing factors. Currently, a single factor is often used to evaluate the completion of a certain production stage, which results in large errors. There is a problem of insufficient accuracy in the purity detection method for the preparation of high-purity ammonia water. Summary of the invention

[0008] The embodiment of the present application solves the problem of insufficient accuracy of the purity detection method for preparing high-purity ammonia water in the prior art by providing a purity detection method for preparing high-purity ammonia water, thereby achieving the effect of improving the accuracy of the purity detection method for preparing pure ammonia water.

[0009] An embodiment of the present application provides a purity detection method for preparing high-purity ammonia water, comprising the following steps: circulating and filtering semi-finished high-purity ammonia water through a liquid filter, monitoring the semi-finished high-purity ammonia water in the circulating filtration in real time, and obtaining original parameters of the semi-finished high-purity ammonia water; performing a circulation execution degree analysis of the semi-finished high-purity ammonia water according to the original parameters of the semi-finished high-purity ammonia water, and obtaining a circulation execution degree analysis result of the semi-finished high-purity ammonia water; performing purity detection and analysis on the semi-finished high-purity ammonia water according to the circulation execution degree analysis result of the semi-finished high-purity ammonia water, and obtaining a purity detection and analysis result of the semi-finished high-purity ammonia water; and regulating the circulation filtration process of the semi-finished high-purity ammonia water through the liquid filter according to the purity detection and analysis result of the semi-finished high-purity ammonia water.

[0010] Furthermore, the specific process of obtaining the original parameters of the semi-finished high-purity ammonia water is as follows: performing liquid particle number analysis on the semi-finished high-purity ammonia water by a liquid particle counter to obtain the number of particles per unit volume of the semi-finished high-purity ammonia water; performing liquid phase ion chromatography analysis on the semi-finished high-purity ammonia water by an ion chromatograph to obtain the anion type parameter and ion concentration parameter of the semi-finished high-purity ammonia water; performing metal ion analysis on the semi-finished high-purity ammonia water by a plasma mass spectrometer to obtain the cation type parameter and ion concentration parameter of the semi-finished high-purity ammonia water; and performing metal ion analysis on the semi-finished high-purity ammonia water by a plasma mass spectrometer to obtain the cation type parameter and ion concentration parameter of the semi-finished high-purity ammonia water. The sub-category parameters are used to classify the unit ion relative concentration parameters of the semi-finished high-purity ammonia water, and the unit ion relative concentration parameters of different types of semi-finished high-purity ammonia water with different circulation filtration times are obtained; the number of circulation filtration times of the semi-finished high-purity ammonia water through the liquid filter and the ion type parameters of the semi-finished high-purity ammonia water are used to classify the number of particles of the semi-finished high-purity ammonia water, and the relative number parameters of different types of semi-finished high-purity ammonia water particles with different circulation filtration times are obtained; the flow rate parameters of the semi-finished high-purity ammonia water circulating through the liquid filter are collected by the liquid flowmeter; the liquid filter usage time parameters are obtained through the production log.

[0011] Furthermore, the semi-finished high-purity ammonia water circulation execution degree analysis results specifically include: obtaining the liquid circulation metal ion execution degree index, liquid circulation anion execution degree index and liquid circulation impurity particle execution degree index according to the relative number parameters of unit ions of different types of semi-finished high-purity ammonia water with different circulation filtration times and the relative number parameters of particles of different types of semi-finished high-purity ammonia water with different circulation filtration times; extracting the semi-finished high-purity ammonia water standard parameters from the high-purity ammonia water preparation database; thereby analyzing and obtaining the liquid circulation execution degree index of the semi-finished high-purity ammonia water with different circulation filtration times.

[0012] Furthermore, the analysis result of the circulation execution degree of the semi-finished high-purity ammonia water also includes: subtracting the liquid circulation execution degree index of the semi-finished high-purity ammonia water with adjacent circulation filtration times to obtain the difference of the liquid circulation execution degree index of the semi-finished high-purity ammonia water with adjacent circulation filtration times; extracting the liquid filter scrapping time and the liquid filter filtration standard rate from the high-purity ammonia water preparation database; obtaining the flow rate parameters of the semi-finished high-purity ammonia water circulating through the liquid filter and the liquid filter usage time parameters; thereby analyzing and obtaining the liquid circulation execution indication values ​​of the semi-finished high-purity ammonia water with different circulation filtration times.

[0013] Furthermore, the step of obtaining the analysis result of the execution degree of the semi-finished high-purity ammonia water cycle also includes: sequentially numbering the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter. The number indicating the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter. , It indicates the total number of times the semi-finished high-purity ammonia water is filtered through the liquid filter; the comprehensive coefficient of liquid circulation execution degree is obtained through the comprehensive analysis formula through the liquid circulation execution degree index of the semi-finished high-purity ammonia water and the liquid circulation execution indication value of the semi-finished high-purity ammonia water. The specific comprehensive analysis formula is as follows; ; ; Indicates The comprehensive coefficient of liquid circulation execution degree of semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. Indicates The liquid circulation execution index of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. Indicates The liquid circulation execution indicator value of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. is the preset liquid cycle execution index influencing weight factor obtained from the high-purity ammonia preparation database. The indicator value influence weighting factor is implemented for the preset liquid cycle obtained from the high purity ammonia preparation database.

[0014] Furthermore, the purity detection and analysis results of the semi-finished high-purity ammonia water specifically include: if the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is greater than or equal to the comprehensive threshold of liquid circulation execution, then the first purity detection and analysis is performed on the semi-finished high-purity ammonia water; if the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is less than the comprehensive threshold of liquid circulation execution, then the purity detection of the semi-finished high-purity ammonia water is judged to be unqualified, the semi-finished high-purity ammonia water continues to be circulated and filtered through the liquid filter, and the second purity detection and analysis is performed on the semi-finished high-purity ammonia water.

[0015] Furthermore, the first purity detection and analysis of the semi-finished high-purity ammonia water is performed, specifically including: if the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is less than or equal to the historical average number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, then it is judged that the purity production process of the semi-finished high-purity ammonia water is qualified, and sampling is performed to verify the purity result. If it is qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated to obtain UP-III grade high-purity ammonia water; if it is unqualified, the liquid circulation execution index is reset according to the test result. If the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is greater than the historical average number of times the filter is filtered when the cycle is completed and less than the historical maximum number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, then it is judged that the production process of the semi-finished high-purity ammonia water meets the standards and samples are taken for testing whether it is qualified. If it is qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated to obtain UP-Ⅱ grade high-purity ammonia water, otherwise, the liquid circulation execution indication threshold is reset according to the test results and the filtration is performed again.

[0016] Furthermore, the second purity detection and analysis of the semi-finished high-purity ammonia water is specifically performed, which specifically includes: continuing to circulate and filter the semi-finished high-purity ammonia water through the liquid filter until the number of filtration times of the semi-finished high-purity ammonia water through the liquid filter is equal to the maximum number of filtration times when the cycle is completed in history, then stopping the circulation filtration to obtain a first semi-finished high-purity ammonia water to be detected; performing purity detection and analysis on the first semi-finished high-purity ammonia water to be detected to obtain a liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected and a liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be detected; if the liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected is If the number is greater than or equal to the preset liquid circulation execution threshold and the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be detected is less than or equal to the preset liquid circulation execution indication threshold, then the purity test of the first semi-finished high-purity ammonia water to be detected is judged to be qualified, and UP-Ⅱ grade high-purity ammonia water is obtained; if the liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected is less than the preset liquid circulation execution threshold or the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be detected is greater than the preset liquid circulation execution indication threshold, then the purity test of the first semi-finished high-purity ammonia water to be detected is judged to be unqualified, and the first semi-finished high-purity ammonia water to be detected is scrapped.

[0017] Furthermore, the first purity detection and analysis of the semi-finished high-purity ammonia water also includes: if the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is greater than the historical average number of times the filter is filtered when the cycle is completed and less than the historical maximum number of times the filter is filtered when the cycle is completed, and the liquid cycle execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid cycle execution threshold and the liquid cycle execution indication value is greater than the preset liquid cycle execution indication threshold, it is determined to continue the circulation filtration until the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is equal to the historical maximum number of times the filter is filtered when the cycle is completed, and the second semi-finished high-purity ammonia water to be detected is obtained; the second semi-finished high-purity ammonia water to be detected The semi-finished high-purity ammonia water is tested for purity detection and analysis to obtain the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested; if the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested is less than or equal to the preset liquid circulation execution indication threshold value, the purity test of the semi-finished high-purity ammonia water is judged to be qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated, and the high-purity ammonia water is recorded as UP-Ⅱ grade high-purity ammonia water; if the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested is greater than the preset liquid circulation execution indication threshold value, the purity test of the second semi-finished high-purity ammonia water to be tested is judged to be unqualified, and a new circulation filtration control is performed on the second semi-finished high-purity ammonia water to be tested.

[0018] Furthermore, the new circulation filtration control of the second semi-finished high-purity ammonia water to be detected specifically includes: increasing the output power of the liquid filter to improve the circulation filtration efficiency of the liquid filter; circulating the second semi-finished high-purity ammonia water to be detected through the adjusted liquid filter, and recounting the number of circulation filtration times; when the number of circulation filtration times of the second semi-finished high-purity ammonia water to be detected through the adjusted liquid filter is equal to the maximum number of filtration times when the cycle is completed in history, the circulation filtration is stopped to obtain the third semi-finished high-purity ammonia water to be detected; purity detection and analysis are performed on the third semi-finished high-purity ammonia water to be detected to obtain the liquid circulation execution degree of the third semi-finished high-purity ammonia water to be detected. Comprehensive coefficient; if the comprehensive coefficient of liquid circulation execution of the third semi-finished high-purity ammonia water to be tested is greater than or equal to the comprehensive threshold of liquid circulation execution, the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be qualified, the third semi-finished high-purity ammonia water to be tested is recorded as UP-I grade high-purity ammonia water, and the relevant personnel are notified to clean or replace the liquid filter components in the liquid filter; if the comprehensive coefficient of liquid circulation execution of the third semi-finished high-purity ammonia water to be tested is less than the comprehensive threshold of liquid circulation execution, the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be unqualified, the third semi-finished high-purity ammonia water to be tested is scrapped, and the relevant personnel are notified to replace the liquid filter.

[0019] One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:

[0020] 1. The present invention conducts purity detection, evaluation and analysis on the circulating filtration of high-purity ammonia water preparation, thereby regulating the circulating filtration process of semi-finished high-purity ammonia water according to the analysis results, thereby achieving the effect of improving the accuracy of the purity detection method for preparing pure ammonia water, and solving the problem of insufficient accuracy of the purity detection method for preparing high-purity ammonia water in the prior art.

[0021] 2. Perform a circulation execution analysis on the semi-finished high-purity ammonia water according to its original parameters to obtain the analysis result of the circulation execution analysis on the semi-finished high-purity ammonia water. Thus, by analyzing the semi-finished high-purity ammonia water with different circulation filtration times, the parameters in the production process can be monitored and adjusted in real time. By analyzing the difference in liquid circulation execution index, combined with the filter's scrapping time and standard filtration rate, the use status of the filtration equipment can be predicted, potential problems can be discovered in advance, and equipment failures can be prevented, thereby achieving the safety of the purity detection method for the preparation of high-purity ammonia water.

[0022] 3. According to the purity test and analysis results of the semi-finished high-purity ammonia water, the circulating filtration process of the semi-finished high-purity ammonia water through the liquid filter is regulated. Through different purity test and analysis steps, the semi-finished high-purity ammonia water can be accurately classified into UP-I, UP-II or UP-III high-purity ammonia water to meet the needs of different quality standards. At the same time, multi-stage step-by-step judgment and analysis can be performed to quickly decide whether to continue the circulating filtration, thereby realizing the high efficiency of the purity test method for the preparation of high-purity ammonia water. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 A flow chart of a purity detection method for preparing high-purity ammonia water provided in an embodiment of the present application;

[0024] Figure 2 A schematic diagram of a function image of an analytical formula for a liquid circulation execution indication value provided in an embodiment of the present application. DETAILED DESCRIPTION

[0025] The embodiment of the present application solves the problem of insufficient accuracy of the purity detection method for preparing high-purity ammonia water in the prior art by providing a purity detection method for preparing high-purity ammonia water. By evaluating and analyzing the purity detection of circulating filtration in the preparation of high-purity ammonia water, the circulating filtration process of the semi-finished high-purity ammonia water is regulated according to the analysis results, thereby achieving the effect of improving the accuracy of the purity detection method for preparing pure ammonia water.

[0026] In order to better understand the above technical solution, the above technical solution will be described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0027] like Figure 1 As shown, it is a flow chart of the purity detection method for preparing high-purity ammonia water provided in an embodiment of the present application, and the method comprises the following steps: circulating and filtering the semi-finished high-purity ammonia water through a liquid filter, monitoring the semi-finished high-purity ammonia water in circulating filtration in real time, and obtaining original parameters of the semi-finished high-purity ammonia water; performing circulation execution degree analysis on the semi-finished high-purity ammonia water according to the original parameters of the semi-finished high-purity ammonia water, and obtaining circulation execution degree analysis results of the semi-finished high-purity ammonia water; performing purity detection and analysis on the semi-finished high-purity ammonia water according to the circulation execution degree analysis results of the semi-finished high-purity ammonia water, and obtaining purity detection and analysis results of the semi-finished high-purity ammonia water; and regulating the circulation filtration process of the semi-finished high-purity ammonia water through the liquid filter according to the purity detection and analysis results of the semi-finished high-purity ammonia water.

[0028] In this embodiment, obtaining semi-finished high-purity ammonia water is a production process step in the preparation of high-purity ammonia water, and the pre-production process steps for obtaining the semi-finished high-purity ammonia water specifically include:

[0029] 1. Pressure reduction evaporation: industrial-grade liquid ammonia is evaporated by pressure reduction evaporator to obtain ammonia gas;

[0030] 2. Oil-water separation: Pass ammonia through an oil-water separator to remove oil and water from the ammonia;

[0031] 3. Circulation filtration: The ammonia after oil-water separation is filtered through a gas filter to obtain high-purity ammonia;

[0032] 4. Absorption and mixing: Use ultrapure water to circulate and absorb ammonia gas to obtain semi-finished high-purity ammonia water.

[0033] Furthermore, the specific process of obtaining the original parameters of the semi-finished high-purity ammonia water is as follows: the liquid particle number analysis of the semi-finished high-purity ammonia water is performed by a liquid particle counter to obtain the particle number parameters per unit volume of the semi-finished high-purity ammonia water; the liquid phase ion chromatography analysis of the semi-finished high-purity ammonia water is performed by an ion chromatograph to obtain the anion type parameters and ion concentration parameters of the semi-finished high-purity ammonia water; the metal ion analysis of the semi-finished high-purity ammonia water is performed by a plasma mass spectrometer to obtain the cation type parameters and ion concentration parameters of the semi-finished high-purity ammonia water; the semi-finished high-purity ammonia water is analyzed by the number of cycles of filtration of the semi-finished high-purity ammonia water through the liquid filter and the ion concentration parameters of the semi-finished high-purity ammonia water. The type parameters are used to classify the unit ion relative concentration parameters of the semi-finished high-purity ammonia water, and the unit ion relative concentration parameters of the different types of semi-finished high-purity ammonia water with different circulation filtration times are obtained; the number of circulation filtration times of the semi-finished high-purity ammonia water through the liquid filter and the ion type parameters of the semi-finished high-purity ammonia water are used to classify the particle number parameters of the semi-finished high-purity ammonia water, and the relative number parameters of the particles of the different types of semi-finished high-purity ammonia water with different circulation filtration times are obtained; the flow rate parameters of the semi-finished high-purity ammonia water circulating through the liquid filter are collected by the liquid flowmeter; the liquid filter usage time parameters are obtained through the production log.

[0034] In this embodiment, in the actual production process, if the original volume of the semi-finished high-purity ammonia water is 100 liters, and the semi-finished high-purity ammonia water passes through the liquid filter for each cycle of filtering a volume of 100 liters, the number of cycle filtration is increased by 1. The ion concentrations in the above and below can be directly obtained through the chromatogram.

[0035] Furthermore, the results of the semi-finished high-purity ammonia water circulation execution analysis are obtained, specifically including: obtaining the liquid circulation metal ion execution index, liquid circulation anion execution index and liquid circulation impurity particle execution index according to the relative number parameters of unit ions of different types of semi-finished high-purity ammonia water with different circulation filtration times and the relative number parameters of particles of different types of semi-finished high-purity ammonia water with different circulation filtration times; extracting the standard parameters of semi-finished high-purity ammonia water from the high-purity ammonia water preparation database; thereby analyzing and obtaining the liquid circulation execution index of the semi-finished high-purity ammonia water with different circulation filtration times.

[0036] In this embodiment, the specific analysis formula of the liquid circulation execution index is as follows: ;like ,but ;like ,but ;like ,but ;like ,but ;like ,but ;like ,but ; The semi-finished high-purity ammonia water is filtered through the liquid filter in cycles and numbered in sequence. The number indicating the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter. , It indicates the total number of times the semi-finished high-purity ammonia water is filtered through the liquid filter.

[0037] Indicates The liquid circulation execution index of the semi-finished high-purity ammonia water that is circulated and filtered through the liquid filter.

[0038] Indicates The liquid circulation metal ion execution index of the semi-finished high-purity ammonia water that is circulated and filtered through a liquid filter.

[0039] Indicates The liquid circulation anion execution index of the semi-finished high-purity ammonia water that is circulated and filtered through the liquid filter.

[0040] Indicates The liquid circulation impurity particle execution index of the semi-finished high-purity ammonia water that is circulated and filtered by the liquid filter.

[0041] The types of metal ions detected in the semi-finished high-purity ammonia water are numbered in sequence. The number indicating the type of metal ion in the semi-finished high-purity ammonia water. , Represents the total number of metal ion types in semi-finished high-purity ammonia water.

[0042] The types of anions detected in the semi-finished high-purity ammonia water are numbered in sequence. The number indicating the type of anion in the semi-finished high-purity ammonia water. , Represents the total number of anion types in semi-finished high-purity ammonia water.

[0043] Indicates The maximum particle concentration of the semi-finished high-purity ammonia water after circulating filtration through the liquid filter is expressed in pieces / ml, that is, the number of particles per milliliter.

[0044] in, Indicates the particle size standard corresponding to the semi-finished high-purity ammonia particles. For example, the particle size standard corresponding to the semi-finished high-purity ammonia particles is 0.5 microns. , which means that all particles in the semi-finished high-purity ammonia water with a size greater than or equal to 0.5 microns are counted.

[0045] like , it means that the maximum concentration of particles larger than or equal to 0.5 microns in the semi-finished high-purity ammonia water is 25 particles / ml. The above particles refer to the impurity particles in the semi-finished high-purity ammonia water.

[0046] It represents the maximum allowable concentration of semi-finished high-purity ammonia particles, which is extracted from the high-purity ammonia preparation database.

[0047] Indicates The semi-finished high-purity ammonia water is filtered through the liquid filter. The maximum value of the metal ion content of a semi-finished high-purity ammonia water is expressed in ppt, which is one trillionth. For example, if the copper ion content of a semi-finished high-purity ammonia water sample is less than 50 ppt, then among one trillion semi-finished high-purity ammonia water molecules, there are less than 50 molecules containing copper ions.

[0048] Indicates The maximum allowable value of the metal ion content of the semi-finished high-purity ammonia water is extracted from the high-purity ammonia water preparation database. For example, the maximum allowable value of calcium ion content is 50ppt, which means that among one trillion semi-finished high-purity ammonia water molecules, no more than 50 molecules containing calcium ions are allowed.

[0049] Indicates The semi-finished high-purity ammonia water is filtered through the liquid filter. The maximum anion content of a semi-finished high-purity ammonia water sample, in ppb, which means "parts per billion". It is used to describe the trace concentration of a certain component in a solution. 1 ppb is equivalent to 1 unit of a substance dissolved in 1 billion units of a solvent. For example, if the phosphate content in a semi-finished high-purity ammonia water sample is less than 50 ppb, then among the billion semi-finished high-purity ammonia water molecules, there are less than 50 molecules containing phosphate.

[0050] Indicates The maximum permissible value of anion content of semi-finished high-purity ammonia water anions is extracted from the high-purity ammonia water preparation database. For example, the maximum permissible value of sulfate content is 40ppb, which means that among one trillion semi-finished high-purity ammonia water molecules, no more than 40 molecules containing sulfate are allowed.

[0051] Furthermore, the results of the semi-finished high-purity ammonia water circulation execution degree analysis are obtained, which also includes: subtracting the liquid circulation execution degree index of the semi-finished high-purity ammonia water with adjacent circulation filtration times to obtain the difference in the liquid circulation execution degree index of the semi-finished high-purity ammonia water with adjacent circulation filtration times; extracting the liquid filter scrapping time and the liquid filter filtration standard rate from the high-purity ammonia water preparation database; obtaining the flow rate parameters of the semi-finished high-purity ammonia water circulating through the liquid filter and the liquid filter usage time parameters; thereby analyzing and obtaining the liquid circulation execution indicator values ​​of the semi-finished high-purity ammonia water with different circulation filtration times.

[0052] In this embodiment, the specific analysis formula of the liquid circulation execution indicator value is as follows: ; ; Indicates The liquid circulation execution indicator value of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. The larger the liquid circulation execution indicator value, the higher the relative level of ionic impurities removed by the liquid filter. However, as the number of cyclic filtration increases, the ionic impurities themselves continue to decrease, which reduces the relative level of ionic impurities removed by the liquid filter. Therefore, in actual production, the liquid circulation execution indicator value is the largest after the first liquid circulation, and decreases as the number of liquid circulation increases.

[0053] It means that the semi-finished high-purity ammonia water is not circulated before the first circulation filtration through the liquid filter. It represents the liquid circulation execution index of the semi-finished high-purity ammonia water before it is circulated through the liquid filter, that is, the liquid circulation execution index calculated under the above parameters when the semi-finished high-purity ammonia water has not been circulated through the liquid filter.

[0054] Indicates The use time of the liquid filter of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter, in days;

[0055] Indicates The length of time it takes for the liquid filter of the semi-finished high-purity ammonia water to be scrapped after the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter, in days;

[0056] Indicates The average filtration rate of the semi-finished high-purity ammonia water through the liquid filter is liters / hour, that is, how many liters per hour;

[0057] Indicates The standard filtration rate of the liquid filter for circulating filtration of semi-finished high-purity ammonia water through the liquid filter; the standard filtration rate of the liquid filter is the standard rate of the liquid filter under rated power operation during factory inspection, in liters / hour, and is extracted from the high-purity ammonia water preparation database.

[0058] like Figure 2 As shown, it is a schematic diagram of the function image of the analysis formula of the liquid circulation execution indication value provided in the embodiment of the present application; Set to 2, take the average filtration rate of semi-finished high-purity ammonia water in the liquid filter as the independent variable, and take the liquid circulation execution indicator value as the dependent variable;

[0059] Function curve in the figure , ,express and and , function curve Indicates when and and The analytical formula function graph of the liquid circulation execution indication value is shown in FIG.

[0060] Function curve in the figure , ,express and and , function curve Indicates when and and The analytical formula function graph of the liquid circulation execution indication value is shown in FIG.

[0061] Function curve in the figure , ,express and and , function curve Indicates when and and The analytical formula function graph of the liquid circulation execution indication value is shown in FIG.

[0062] It can be seen from the figure that when the average filtration rate of the semi-finished high-purity ammonia water in the liquid filter increases, it means that when the average filtration rate of the semi-finished high-purity ammonia water in the liquid filter becomes faster and faster, the filtration efficiency is improved and the liquid circulation execution indication value also increases.

[0063] From the function curve in the figure And the function curve in the figure It is known that when and The value of is the same as When the values ​​are different, The larger the value, the longer the liquid filter of the semi-finished high-purity ammonia water has been used. At this time, the liquid filter of the semi-finished high-purity ammonia water is relatively older. The function curve Relative to the function curve The liquid circulation execution indication value is smaller and the relative rising trend is slower.

[0064] From the function curve in the figure And the function curve in the figure It is known that when and The value of is the same as When the values ​​are different, The larger the value, the greater the standard filtration rate of the liquid filter. Relative to the function curve The liquid circulation execution indication value is smaller and the relative rising trend is slower.

[0065] As can be seen from the figure, When the value is fixed, the liquid circulation execution indication value increases dramatically with the change of other influencing factors. In actual situations, in the continuous production and preparation of high-purity ammonia water in a short period of time, the number of circulation filtration times of the semi-finished high-purity ammonia water increases, which makes the liquid circulation execution indication value decrease continuously, that is, the filtering effect of the circulation filtration on the impurity ions continues to decrease, which conforms to the objective situation of the circulation filtration of the semi-finished high-purity ammonia water in the liquid filter.

[0066] Further, obtaining the analysis result of the execution degree of the semi-finished high-purity ammonia water cycle also includes: sequentially numbering the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter. The number indicating the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter. , It indicates the total number of times the semi-finished high-purity ammonia water is filtered through the liquid filter; the comprehensive coefficient of liquid circulation execution degree is obtained through the comprehensive analysis formula through the liquid circulation execution degree index of the semi-finished high-purity ammonia water and the liquid circulation execution indication value of the semi-finished high-purity ammonia water. The specific comprehensive analysis formula is as follows; ; ; Indicates The comprehensive coefficient of liquid circulation execution degree of semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. Indicates The liquid circulation execution index of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. Indicates The liquid circulation execution indicator value of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. is the preset liquid cycle execution index influencing weight factor obtained from the high-purity ammonia preparation database. The indicator value influence weighting factor is implemented for the preset liquid cycle obtained from the high purity ammonia preparation database.

[0067] In this embodiment, It is a preset liquid circulation execution index influencing weight factor obtained from the high-purity ammonia preparation database, and is used to represent the numerical value of the influence degree of the liquid circulation execution index on the liquid circulation execution comprehensive coefficient due to the change in the number of circulation filtration times. The preset liquid circulation execution indicator value influencing weight factor obtained from the high-purity ammonia water preparation database is used to represent the numerical value of the degree of influence of the liquid circulation execution indicator value on the comprehensive coefficient of liquid circulation execution due to the change in the number of circulation filtrations. When used, the liquid circulation execution index influencing weight factor and the liquid circulation execution indicator value influencing weight factor corresponding to the number of circulation filtrations can be directly obtained from the high-purity ammonia water preparation database, and the corresponding relationship can be a pre-set mapping relationship. For example, the number of circulation filtrations and the liquid circulation execution index influencing weight factor and the liquid circulation execution indicator value influencing weight factor in the medical treatment database form a mapping set, and the real-time circulation filtration number is input into the mapping set to obtain the liquid circulation execution index influencing weight factor and the liquid circulation execution indicator value influencing weight factor. The liquid circulation execution index influencing weight factor and the liquid circulation execution indicator value influencing weight factor in this example have a value range of (0,1), and the sum of the two is 1.

[0068] When the number of cycle filtration is small, the liquid filter has a better effect of removing ionized impurities. When the number of cycle filtration increases, the filtering effect of the liquid filter decreases. When the number of cycle filtration is large, the semi-finished high-purity ammonia water has been filtered many times, and various ion impurities are already low. After more cycle filtration times, the deionization impurity effect is not obvious, and the liquid filter filtering effect is low. The liquid circulation execution indicator value is used to describe the relative level of deionized impurities filtered by the liquid filter. Therefore, as the real-time cycle filtration number increases, the liquid circulation execution indicator value affects the weight factor decreases. Conversely, the liquid circulation execution index affects the weight factor increases.

[0069] Table 1 is an example table of comprehensive coefficients of liquid circulation execution. The example parameters in Table 1 are only taken as an example of the parameters of semi-finished high-purity ammonia water being filtered through a liquid filter once. Table 1 is shown below.

[0070] Table 1 Example of comprehensive coefficient of liquid circulation execution

[0071]

[0072] According to Table 1, if and When nothing changes, or When it increases, the comprehensive coefficient of liquid circulation execution becomes larger. The liquid circulation execution index is used to describe the purity level of the semi-finished high-purity ammonia water after it is circulated and filtered through the liquid filter. The liquid circulation execution indicator value is used to describe the efficiency level of the circulation filtration and impurity ion removal of the semi-finished high-purity ammonia water after it is circulated and filtered through the liquid filter. Comprehensive evaluation of the above factors makes it easier to quantitatively evaluate the comprehensive coefficient of liquid circulation execution.

[0073] Furthermore, the purity detection and analysis results of the semi-finished high-purity ammonia water are obtained, specifically including: if the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is greater than or equal to the comprehensive threshold of liquid circulation execution, the first purity detection and analysis is performed on the semi-finished high-purity ammonia water; if the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is less than the comprehensive threshold of liquid circulation execution, the purity detection of the semi-finished high-purity ammonia water is judged to be unqualified, the semi-finished high-purity ammonia water continues to be circulated and filtered through the liquid filter, and the second purity detection and analysis is performed on the semi-finished high-purity ammonia water.

[0074] In this embodiment, if the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is greater than or equal to the comprehensive threshold of liquid circulation execution, it means that the circulation filtration of the semi-finished high-purity ammonia water can be preliminarily judged to be in compliance with the purity test, but further judgment is still needed; if the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is less than the comprehensive threshold of liquid circulation execution, it means that the circulation filtration of the semi-finished high-purity ammonia water can be preliminarily judged to be not in compliance with the purity test, but further judgment is still needed.

[0075] Furthermore, a first purity detection and analysis is performed on the semi-finished high-purity ammonia water, specifically including: if the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is less than or equal to the historical average number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, then it is judged that the purity production process of the semi-finished high-purity ammonia water is qualified, and sampling is performed to verify the purity result. If it is qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated to obtain UP-III grade high-purity ammonia water. If it is unqualified, the preset liquid circulation execution is reset according to the test result. If the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is greater than the historical average number of times the filter is filtered when the cycle is completed and less than the historical maximum number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, then it is judged that the production process of the semi-finished high-purity ammonia water meets the standards and samples are taken for testing whether it is qualified. If it is qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated to obtain UP-Ⅱ grade high-purity ammonia water, otherwise, the liquid circulation execution indication threshold is reset according to the test results and the filtration is performed again.

[0076] In this embodiment, according to the above analysis, it can be preliminarily determined that the purity test is met, but further judgment is still needed, so the first purity test analysis is performed.

[0077] If the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is less than or equal to the historical average number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, it means that the semi-finished high-purity ammonia water has reached the purity requirement when the number of cycles is less than or equal to the average number of cycles and the relative level of ionic impurities removed by the liquid filter circulation filtration is low, which means that the circulation removal execution degree of the semi-finished high-purity ammonia water is already very high, so UP-III grade high-purity ammonia water is obtained.

[0078] Conversely, if the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is greater than the historical average number of times the cycle is completed and less than the historical maximum number of times the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, it means that the circulation decontamination execution degree of the semi-finished high-purity ammonia water is also very high at this time, but the number of cycles used is relatively large, so only UP-Ⅱ grade high-purity ammonia water can be obtained.

[0079] UP-Ⅰ grade high-purity ammonia water, UP-Ⅱ grade high-purity ammonia water and UP-Ⅲ grade high-purity ammonia water can correspond to the electronic-grade ammonia water group standard document T / CSTM 01148-2024 of the actual electronic-grade ammonia water standard document, or can be set according to the business standards in the actual production industry.

[0080] Electronic-grade ammonia is divided into three grades: UP-III, UP-II and UP-I, among which UP is the abbreviation of Ultra Purity in English.

[0081] UP-III is mainly used in the semiconductor advanced process industry;

[0082] UP-Ⅱ and UP-I are mainly used in conventional semiconductor processes and high-process panel industries.

[0083] UP-III grade high-purity ammonia water has the highest purity requirement, UP-II grade high-purity ammonia water has the second highest purity requirement, and UP-I grade high-purity ammonia water has the lowest purity requirement.

[0084] Furthermore, a second purity detection and analysis is performed on the semi-finished high-purity ammonia water, specifically including: continuing to circulate and filter the semi-finished high-purity ammonia water through the liquid filter until the number of filtration times of the semi-finished high-purity ammonia water through the liquid filter is equal to the maximum number of filtration times when the cycle is completed in history, then stopping the circulation filtration to obtain the first semi-finished high-purity ammonia water to be detected; performing purity detection and analysis on the first semi-finished high-purity ammonia water to be detected to obtain the liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected and the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be detected; if the liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected is If the liquid circulation execution index of the first semi-finished high-purity ammonia water to be tested is greater than or equal to the preset liquid circulation execution threshold and the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be tested is less than or equal to the preset liquid circulation execution indication threshold, then the purity test of the first semi-finished high-purity ammonia water to be tested is judged to be qualified, and UP-Ⅱ grade high-purity ammonia water is obtained; if the liquid circulation execution index of the first semi-finished high-purity ammonia water to be tested is less than the preset liquid circulation execution threshold or the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be tested is greater than the preset liquid circulation execution indication threshold, then the purity test of the first semi-finished high-purity ammonia water to be tested is judged to be unqualified, and the first semi-finished high-purity ammonia water to be tested is scrapped.

[0085] In this embodiment, the circulating filtration of the semi-finished high-purity ammonia water can be preliminarily judged to be not in compliance with the purity test and further judgment is required.

[0086] First, the semi-finished high-purity ammonia water is filtered through the liquid filter as many times as necessary and then tested again. If the liquid circulation execution index of the first semi-finished high-purity ammonia water to be tested is greater than or equal to the preset liquid circulation execution threshold and the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be tested is less than or equal to the preset liquid circulation execution indication threshold, then the purity test of the first semi-finished high-purity ammonia water to be tested is judged to be qualified, indicating that the circulation de-impurity execution degree of the semi-finished high-purity ammonia water is also very high at this time, but the number of cycles used is relatively large, so only UP-Ⅱ grade high-purity ammonia water can be obtained.

[0087] Conversely, if the number of cycles used reaches the limit and the product is still unqualified, the first semi-finished high-purity ammonia water to be tested will be scrapped.

[0088] Furthermore, a first purity detection and analysis is performed on the semi-finished high-purity ammonia water, which also includes: if the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is greater than the historical average number of times the filter is filtered when the cycle is completed and less than the historical maximum number of times the filter is filtered when the cycle is completed, and the liquid cycle execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid cycle execution threshold and the liquid cycle execution indication value is greater than the preset liquid cycle execution indication threshold, it is determined to continue the cycle filtration until the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is equal to the historical maximum number of times the filter is filtered when the cycle is completed, and the second semi-finished high-purity ammonia water to be detected is obtained; the second semi-finished high-purity ammonia water to be detected is analyzed. The semi-finished high-purity ammonia water is tested for purity and analyzed to obtain the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested; if the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested is less than or equal to the preset liquid circulation execution indication threshold value, the purity test of the semi-finished high-purity ammonia water is judged to be qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated, and the high-purity ammonia water is recorded as UP-Ⅱ grade high-purity ammonia water; if the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested is greater than the preset liquid circulation execution indication threshold value, the purity test of the second semi-finished high-purity ammonia water to be tested is judged to be unqualified, and a new circulation filtration control is performed on the second semi-finished high-purity ammonia water to be tested.

[0089] In this embodiment, it has been judged above that during the circulation filtration, if the number of times the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter is greater than the historical average number of times the circulation is completed and less than the historical maximum number of times the circulation is completed, the liquid circulation execution index and the liquid circulation execution indication value both meet the threshold requirements, and there are other situations that need to be judged.

[0090] The liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold and the liquid circulation execution indication value is greater than the preset liquid circulation execution indication threshold. This means that although the purity of the semi-finished high-purity ammonia water has met the standards, the impurity removal effect of the circulation filtration is still obvious, indicating that although the purity of the semi-finished high-purity ammonia water meets the standards, it can still be circulated and filtered to achieve a higher purity level. It is necessary to circulate until the maximum number of times and then evaluate. If the result of the re-evaluation meets the purity requirements, UP-Ⅱ grade high-purity ammonia water is obtained. If high-purity ammonia water that meets the purity requirements still cannot be obtained, it means that there may be problems in the circulation filtration process of the semi-finished high-purity ammonia water, and the problem needs to be further analyzed.

[0091] Further, a new circulation filtration control is performed on the second semi-finished high-purity ammonia water to be detected, specifically including: increasing the output power of the liquid filter to improve the circulation filtration efficiency of the liquid filter; circulating the second semi-finished high-purity ammonia water to be detected through the adjusted liquid filter, and recounting the number of circulation filtration times; when the number of circulation filtration times of the second semi-finished high-purity ammonia water to be detected through the adjusted liquid filter is equal to the maximum number of filtration times when the cycle is completed in history, the circulation filtration is stopped to obtain the third semi-finished high-purity ammonia water to be detected; purity detection and analysis is performed on the third semi-finished high-purity ammonia water to be detected, and the liquid circulation execution degree of the third semi-finished high-purity ammonia water to be detected is obtained. Comprehensive coefficient; if the comprehensive coefficient of liquid circulation execution degree of the third semi-finished high-purity ammonia water to be tested is greater than or equal to the comprehensive threshold value of liquid circulation execution degree, the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be qualified, the third semi-finished high-purity ammonia water to be tested is recorded as UP-I grade high-purity ammonia water, and the relevant personnel are notified to clean or replace the liquid filter components in the liquid filter; if the comprehensive coefficient of liquid circulation execution degree of the third semi-finished high-purity ammonia water to be tested is less than the comprehensive threshold value of liquid circulation execution degree, the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be unqualified, the third semi-finished high-purity ammonia water to be tested is scrapped, and the relevant personnel are notified to replace the liquid filter.

[0092] In this embodiment, during the process of circulating and filtering the semi-finished high-purity ammonia water through the liquid filter, the problem of the filtration efficiency of the liquid filter decreasing as the usage time increases may occur. This situation usually occurs in the following types of liquid filters:

[0093] 1. Deep filter: This type of filter captures particles through multiple layers of media. As the filtration time increases, the pores in the media layer may be blocked by particles, resulting in a decrease in filtration efficiency.

[0094] 2. Surface filter: This type of filter relies on the pore size on the surface of the filter medium to retain particles. As the filtration proceeds, more and more particles may accumulate on the surface, forming a layer of filter cake, which can improve filtration efficiency under certain conditions, but once the filter cake is saturated, additional particles will pass through, resulting in a decrease in filtration efficiency.

[0095] 3. Membrane filters: including microfiltration, ultrafiltration, nanofiltration and reverse osmosis, these filters rely on membrane pore size to retain particles and solutes. Over time, the membrane may become contaminated, clogged or the membrane pores may deform, all of which may lead to a decrease in filtration efficiency.

[0096] Here are some factors that may cause a decrease in the efficiency of your liquid filter:

[0097] 1. Particle accumulation: As the filtration proceeds, the amount of particles accumulated on the filter medium increases, which may cause the filter pore size to decrease and increase the filtration resistance.

[0098] 2. Media wear: Long-term use may cause the filter media to wear and the pore size to become larger, allowing particles that were originally intercepted to pass through.

[0099] 3. Biological contamination: When filtering water or other liquids, microorganisms may grow on the filter and form a biofilm, which will block the filter pores and reduce the filtration efficiency.

[0100] 4. Chemical changes: Certain chemicals may react with the filter media, changing its structure and properties, affecting filtration efficiency.

[0101] Generally, in order to maintain the filtration efficiency, the filter usually needs to be cleaned, regenerated or the filter medium replaced regularly.

[0102] Therefore, in the above text, the second semi-finished high-purity ammonia water to be tested is subjected to new circulation filtration and regulation to obtain the third semi-finished high-purity ammonia water to be tested and the purity is tested again in order to analyze whether there is any hardware problem with the liquid filter.

[0103] If the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be qualified at this time, it means that the liquid filter can still perform the filtering function normally, but the filtering efficiency has been greatly reduced, and the corresponding parts need to be replaced, such as the filter medium and the filter membrane.

[0104] If the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be unqualified at this time, it means that the liquid filter can no longer perform its filtering function normally. The third semi-finished high-purity ammonia water to be tested needs to be scrapped and relevant personnel should be notified to replace the liquid filter.

[0105] It will be appreciated by those skilled in the art that embodiments of the present invention may be provided as methods, systems, or computer program products. Therefore, the present invention may take the form of a complete hardware embodiment, a complete software embodiment, or an embodiment combining software and hardware. Furthermore, the present invention may take the form of a computer program product implemented on one or more computer-usable storage media (including but not limited to disk storage, CD-ROM, optical storage, etc.) containing computer-usable program code.

[0106] The present invention is described with reference to flowcharts and / or block diagrams of methods, devices (systems), and computer program products according to embodiments of the present invention. It should be understood that each process and / or block in the flowchart and / or block diagram, as well as the combination of processes and / or blocks in the flowchart and / or block diagram, can be implemented by computer program instructions. These computer program instructions can be provided to a processor of a general-purpose computer, a special-purpose computer, an embedded processor, or other programmable data processing device to produce a machine, so that the instructions executed by the processor of the computer or other programmable data processing device generate instructions for implementing the processes in the flowchart and / or block diagram. Figure 1 A process or multiple processes and / or boxes Figure 1 A device that provides the functions specified in a block or multiple blocks.

[0107] These computer program instructions may also be stored in a computer-readable memory capable of directing a computer or other programmable data processing device to operate in a specific manner, so that the instructions stored in the computer-readable memory produce an article of manufacture comprising an instruction device, which implements the process Figure 1 A process or multiple processes and / or boxes Figure 1 A function specified in one or more boxes.

[0108] These computer program instructions can also be loaded onto a computer or other programmable data processing device so that a series of operating steps are executed on the computer or other programmable device to produce a computer-implemented process, thereby providing instructions for implementing the process. Figure 1 A process or multiple processes and / or boxes Figure 1 A step that specifies a function in one or more boxes.

[0109] Although the preferred embodiments of the present invention have been described, those skilled in the art may make other changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention.

[0110] Obviously, those skilled in the art may make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.

Claims

1. A purity detection method for preparing high-purity ammonia water, characterized in that: The following steps are involved: The semi-finished high-purity ammonia water is circulated and filtered through a liquid filter, and the semi-finished high-purity ammonia water in the circulated filtration is monitored in real time to obtain the original parameters of the semi-finished high-purity ammonia water; Performing a semi-finished product high-purity ammonia water circulation execution degree analysis based on the original parameters of the semi-finished product high-purity ammonia water, and obtaining a semi-finished product high-purity ammonia water circulation execution degree analysis result; According to the semi-finished product high-purity ammonia water circulation execution degree analysis result, the semi-finished product high-purity ammonia water is subjected to purity detection and analysis to obtain the semi-finished product high-purity ammonia water purity detection and analysis result, and according to the semi-finished product high-purity ammonia water purity detection and analysis result, the semi-finished product high-purity ammonia water circulation filtration process through the liquid filter is regulated and controlled; The step of obtaining the semi-finished high-purity ammonia water cycle execution degree analysis result also includes: The semi-finished high-purity ammonia water is numbered in sequence for the number of times it is filtered through the liquid filter. The number indicating the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter. , It indicates the total number of times the semi-finished high-purity ammonia water is filtered through the liquid filter; The comprehensive coefficient of liquid circulation execution degree is obtained by using the liquid circulation execution degree index of the semi-finished high-purity ammonia water and the liquid circulation execution indication value of the semi-finished high-purity ammonia water through a comprehensive analysis formula. The specific comprehensive analysis formula is as follows; ; ; Indicates The comprehensive coefficient of liquid circulation execution degree of semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. Indicates The liquid circulation execution index of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. Indicates The liquid circulation execution indicator value of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered by the liquid filter. is the preset liquid cycle execution index influencing weight factor obtained from the high-purity ammonia preparation database. A weighting factor affecting the indicated value for a preset liquid cycle execution obtained from a high purity ammonia preparation database; The analysis result of the semi-finished high-purity ammonia water cycle execution degree obtained specifically includes: According to the relative number parameters of unit ions of different types of semi-finished high-purity ammonia water with different circulation filtration times and the relative number parameters of particles of different types of semi-finished high-purity ammonia water with different circulation filtration times, the liquid circulation metal ion execution index, the liquid circulation anion execution index and the liquid circulation impurity particle execution index are obtained; Extract the standard parameters of semi-finished high-purity ammonia water from the high-purity ammonia water preparation database; The liquid circulation execution index of semi-finished high-purity ammonia water with different circulation filtration times is thus obtained; The specific analysis formula of the liquid circulation execution index is as follows: ; like ,but ; like ,but ; like ,but ; like ,but ; like ,but ; like ,but ; Indicates Liquid circulation execution index of semi-finished high-purity ammonia water after circulating filtration of semi-finished high-purity ammonia water through a liquid filter; Indicates Liquid circulation metal ion execution index of semi-finished high-purity ammonia water after circulating filtration of semi-finished high-purity ammonia water through a liquid filter; Indicates Liquid circulation anion execution index of semi-finished high-purity ammonia water after circulating filtration of semi-finished high-purity ammonia water through a liquid filter; Indicates Liquid circulation impurity particle execution index of semi-finished high-purity ammonia water after circulating filtration of semi-finished high-purity ammonia water through a liquid filter; The types of metal ions detected in the semi-finished high-purity ammonia water are numbered in sequence. The number indicating the type of metal ion in the semi-finished high-purity ammonia water. , It indicates the total number of metal ion types in semi-finished high-purity ammonia water; The types of anions detected in the semi-finished high-purity ammonia water are numbered in sequence. The number indicating the type of anion in the semi-finished high-purity ammonia water. , It indicates the total number of anion species in semi-finished high-purity ammonia water; Indicates The maximum particle concentration of semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter; It represents the maximum allowable concentration of semi-finished high-purity ammonia water particles, which is extracted from the high-purity ammonia water preparation database; Indicates The semi-finished high-purity ammonia water is filtered through the liquid filter. The maximum value of the metal ion content of the semi-finished high-purity ammonia water; Indicates The maximum allowable value of the metal ion content of the semi-finished high-purity ammonia water is extracted from the high-purity ammonia water preparation database; Indicates The semi-finished high-purity ammonia water is filtered through the liquid filter. The maximum anion content of the semi-finished high-purity ammonia water anion; Indicates The maximum permissible value of anion content of the semi-finished high-purity ammonia water anion is extracted from the high-purity ammonia water preparation database; The step of obtaining the semi-finished high-purity ammonia water cycle execution degree analysis result also includes: By subtracting the liquid circulation execution index of the semi-finished high-purity ammonia water with adjacent circulation filtration times, the difference of the liquid circulation execution index of the semi-finished high-purity ammonia water with adjacent circulation filtration times is obtained; The liquid filter scrapping time and the liquid filter filtration standard rate are extracted from the high-purity ammonia preparation database; Obtaining the flow rate parameters of the semi-finished high-purity ammonia water circulating through the liquid filter and the use time parameters of the liquid filter; The liquid circulation execution indicator value of the semi-finished high-purity ammonia water with different circulation filtration times is thus obtained; The specific analysis formula of the liquid circulation execution indication value is as follows: ; ； Indicates Liquid circulation execution indicator value of semi-finished high-purity ammonia water after being circulated and filtered by the liquid filter; It means that the semi-finished high-purity ammonia water is not circulated before the first circulation filtration through the liquid filter. It indicates the liquid circulation execution index of the semi-finished high-purity ammonia water before circulation filtration through the liquid filter; Indicates The use time of the liquid filter of the semi-finished high-purity ammonia water after the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter; Indicates The length of time it takes for the liquid filter of the semi-finished high-purity ammonia water to be scrapped after the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter; Indicates The average filtration rate of semi-finished high-purity ammonia water through the liquid filter where the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter; Indicates The standard filtration rate of the liquid filter for circulating filtration of the semi-finished high-purity ammonia water through the liquid filter; the standard filtration rate of the liquid filter is the standard rate of the liquid filter under rated power operation during factory inspection, in liters / hour, extracted from the high-purity ammonia water preparation database; The purity test and analysis results of the semi-finished high-purity ammonia water obtained specifically include: If the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is greater than or equal to the comprehensive threshold of liquid circulation execution, a first purity detection and analysis is performed on the semi-finished high-purity ammonia water; If the comprehensive coefficient of liquid circulation execution of the semi-finished high-purity ammonia water is less than the comprehensive threshold of liquid circulation execution, the purity test of the semi-finished high-purity ammonia water is judged to be unqualified, the semi-finished high-purity ammonia water is further circulated and filtered through the liquid filter, and a second purity test analysis is performed on the semi-finished high-purity ammonia water; The first purity detection and analysis of the semi-finished high-purity ammonia water specifically includes: If the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter is less than or equal to the historical average number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, then the purity production process of the semi-finished high-purity ammonia water is judged to be qualified, and sampling is carried out to verify the purity result. If it is qualified, the semi-finished high-purity ammonia water circulation filtration is terminated to obtain UP-III grade high-purity ammonia water. If it is unqualified, the liquid circulation execution indication threshold is reset according to the test result and the filtration is repeated; If the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter through a circulation filter is greater than the historical average number of times the filter is filtered when the circulation is completed and less than the historical maximum number of times the filter is filtered when the circulation is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold, and the liquid circulation execution indication value is less than or equal to the preset liquid circulation execution indication threshold, then it is judged that the production process of the semi-finished high-purity ammonia water meets the standards and samples are taken for testing to see if they are qualified. If they are qualified, the circulation filtration of the semi-finished high-purity ammonia water is terminated to obtain UP-II grade high-purity ammonia water. Otherwise, the preset liquid circulation execution indication threshold is reset according to the test results and filtering is performed again; The second purity detection and analysis of the semi-finished high-purity ammonia water specifically includes: The semi-finished high-purity ammonia water is continuously filtered through the liquid filter in a circulation manner until the number of times the semi-finished high-purity ammonia water passes through the liquid filter in a circulation manner equals to the maximum number of times the semi-finished high-purity ammonia water has been filtered in a history, and then the circulation filtering is stopped to obtain the first semi-finished high-purity ammonia water to be tested; Performing purity detection and analysis on the first semi-finished high-purity ammonia water to be detected, and obtaining a liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected and a liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be detected; If the liquid circulation execution index of the first semi-finished high-purity ammonia water to be detected is greater than or equal to the preset liquid circulation execution threshold and the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be detected is less than or equal to the preset liquid circulation execution indication threshold, it is judged that the purity test of the first semi-finished high-purity ammonia water to be detected is qualified, and UP-II grade high-purity ammonia water is obtained; If the liquid circulation execution index of the first semi-finished high-purity ammonia water to be tested is less than the preset liquid circulation execution threshold or the liquid circulation execution indication value of the first semi-finished high-purity ammonia water to be tested is greater than the preset liquid circulation execution indication threshold, it is judged that the purity test of the first semi-finished high-purity ammonia water to be tested is unqualified, and the first semi-finished high-purity ammonia water to be tested is scrapped.

2. The method for detecting the purity of high-purity ammonia water as claimed in claim 1, characterized in that: The specific process of obtaining the original parameters of the semi-finished high-purity ammonia water is as follows: The liquid particle number analysis of the semi-finished high-purity ammonia water is performed by a liquid particle counter to obtain the particle number parameter per unit volume of the semi-finished high-purity ammonia water; Performing liquid phase ion chromatography analysis on the semi-finished high-purity ammonia water by an ion chromatograph to obtain anion type parameters and ion concentration parameters of the semi-finished high-purity ammonia water; Metal ion analysis is performed on the semi-finished high-purity ammonia water by using a plasma mass spectrometer to obtain cation type parameters and ion concentration parameters of the semi-finished high-purity ammonia water; Data classification is performed on the unit ion relative concentration parameter of the semi-finished high-purity ammonia water according to the number of times the semi-finished high-purity ammonia water is circulated and filtered through the liquid filter and the ion type parameters of the semi-finished high-purity ammonia water, so as to obtain unit ion relative concentration parameters of different types of semi-finished high-purity ammonia water with different circulatory filtration times; Data classification is performed on the number of particles of semi-finished high-purity ammonia water according to the number of times the semi-finished high-purity ammonia water passes through the liquid filter and the ion type parameters of the semi-finished high-purity ammonia water, so as to obtain relative number parameters of particles of different types of semi-finished high-purity ammonia water with different number of cycle filtrations; The flow rate parameters of semi-finished high-purity ammonia water circulating through the liquid filter are collected by a liquid flow meter; The liquid filter usage time parameters are obtained through the production log.

3. The purity detection method for preparing high-purity ammonia water as claimed in claim 2, characterized in that: The first purity detection and analysis of the semi-finished high-purity ammonia water also includes: If the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter through circulation is greater than the historical average number of times the filter is filtered when the cycle is completed and less than the historical maximum number of times the filter is filtered when the cycle is completed, and the liquid circulation execution index of the semi-finished high-purity ammonia water is greater than or equal to the preset liquid circulation execution threshold and the liquid circulation execution indication value is greater than the preset liquid circulation execution indication threshold, it is determined to continue the circulation filtration until the number of times the semi-finished high-purity ammonia water is filtered through the liquid filter through circulation is equal to the historical maximum number of times the filter is filtered when the cycle is completed, and the second semi-finished high-purity ammonia water to be tested is obtained; Performing purity detection and analysis on the second semi-finished high-purity ammonia water to be detected, and obtaining a liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be detected; If the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be detected is less than or equal to the preset liquid circulation execution indication threshold, the purity test of the second semi-finished high-purity ammonia water to be detected is judged to be qualified, and the second semi-finished high-purity ammonia water to be detected is recorded as UP-II grade high-purity ammonia water; If the liquid circulation execution indication value of the second semi-finished high-purity ammonia water to be tested is greater than the preset liquid circulation execution indication threshold, it is judged that the purity test of the second semi-finished high-purity ammonia water to be tested is unqualified, and a new circulation filtration and regulation is performed on the second semi-finished high-purity ammonia water to be tested.

4. The purity detection method for preparing high-purity ammonia water as claimed in claim 3, characterized in that: The new circulation filtration and regulation of the second semi-finished high-purity ammonia water to be detected specifically includes: Increase the output power of the liquid filter and improve the circulation filtration efficiency of the liquid filter; The second semi-finished high-purity ammonia water to be tested is circulated and filtered through the adjusted liquid filter, and the number of cyclic filtrations is recounted; When the number of times the second semi-finished high-purity ammonia water to be tested is filtered through the adjusted liquid filter is equal to the maximum number of times the filter has completed the cycle in history, the circulating filtration is stopped to obtain the third semi-finished high-purity ammonia water to be tested; Performing purity detection and analysis on the third semi-finished high-purity ammonia water to be detected, and obtaining a comprehensive coefficient of liquid circulation execution degree of the third semi-finished high-purity ammonia water to be detected; If the comprehensive coefficient of liquid circulation execution degree of the third semi-finished high-purity ammonia water to be tested is greater than or equal to the comprehensive threshold value of liquid circulation execution degree, the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be qualified, the third semi-finished high-purity ammonia water to be tested is recorded as UP-I grade high-purity ammonia water, and relevant personnel are notified to clean or replace the liquid filter component in the liquid filter; If the comprehensive coefficient of liquid circulation execution of the third semi-finished high-purity ammonia water to be tested is less than the comprehensive threshold of liquid circulation execution, the purity test of the third semi-finished high-purity ammonia water to be tested is judged to be unqualified, the third semi-finished high-purity ammonia water to be tested is scrapped, and relevant personnel are notified to replace the liquid filter.

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