Polysilicon surface metal impurity detection system and method for realizing automatic weighing and acid addition

Abstract

The present invention relates to the field of semiconductor material detection technology, and in particular, to a polysilicon surface metal impurity detection system and method for realizing automatic weighing and acid addition. It comprises: an identification module obtains a sample information two-dimensional code image; a weighing module measures the mass of an empty sample bottle, the mass of a sample, and the mass of real-time liquid addition; a liquid addition module automatically adds acid to a polysilicon sample; a background system receives and stores data, considers the influence of temperature and humidity environmental factors, constructs a temperature compensation calculation model and a humidity compensation calculation model, optimizes and calculates the final empty sample bottle mass and the final sample mass, and uses the background system liquid addition control algorithm to calculate the liquid addition mass; a control module is used to control the weighing module and the liquid addition module; and an impurity detection module is used to analyze the metal impurity content. The design of the present invention is based on the background system liquid addition control algorithm and the coordinated operation of multiple modules to realize automatic impurity detection of acid addition.

Description

Technical Field

[0001] The invention relates to the technical field of semiconductor material detection, in particular to a polysilicon surface metal impurity detection system and method for realizing automatic weighing and acid addition. Background Art

[0002] The polysilicon surface metal impurity detection system and method based on automatic weighing and acid addition is aimed at improving the detection accuracy and automation level and reducing human errors. Through the high-precision semiconductor electronic-grade pump valve system and the background system liquid addition control algorithm, the acid addition amount and the dynamic adjustment of the sample processing process are controlled to achieve efficient and accurate detection of metal impurities on the polysilicon surface.

[0003] Existing systems and methods for detecting metal impurities on the surface of polycrystalline silicon are usually difficult to achieve real-time dynamic adjustment and precise control of the acid addition process. In addition, due to manual intervention and inaccurate equipment calibration during the detection process, it will lead to problems such as unstable acid addition amount, insufficient detection accuracy and inconsistent detection results of metal impurities dissolved after acid addition. Therefore, a system and method for detecting metal impurities on the surface of polycrystalline silicon that can automatically weigh and add acid is provided. Summary of the invention

[0004] The purpose of the present invention is to provide a system and method for detecting metal impurities on the surface of polysilicon by automatic weighing and acid addition, so as to solve the problems raised in the above background technology that manual intervention and inaccurate equipment calibration during the detection process will lead to unstable acid addition amount, insufficient detection accuracy and inconsistent detection results of metal impurities dissolved after acid addition.

[0005] To achieve the above object, the present invention aims to provide a polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition, comprising:

[0006] The identification module obtains the polysilicon sample information QR code image through the built-in CMOS photosensitive device and the dedicated lens module, and converts it into a polysilicon digital signal using the QR code recognition algorithm and transmits it to the background system; the specific steps are as follows:

[0007] S1.1. The built-in CMOS photosensitive device is used to collect images, and the dedicated lens module recognizes the QR code image of the polysilicon sample;

[0008] S1.2, using a two-dimensional code recognition algorithm to analyze the two-dimensional code image and convert the two-dimensional code image information into a digital signal;

[0009] S1.3, transmitting the digital signal to the background system for storage and processing;

[0010] It also includes a weighing module, which sets the weighing process through a PLC program, measures the mass of the empty sample bottle, the mass of the sample, and the real-time mass of the added liquid, and outputs the results to the background system;

[0011] It also includes a liquid adding module, which automatically adds acid to the polysilicon sample using a high-precision semiconductor electronic grade pump valve system according to the theoretical liquid adding mass calculated by the background system;

[0012] It also includes a background system, which receives and stores data information from the identification module, the weighing module and the liquid adding module, considers the influence of temperature and humidity environmental factors during the calculation process, builds a temperature compensation calculation model and a humidity compensation calculation model, optimizes the calculation of the final empty sample bottle mass and the final sample mass, and uses the background system liquid adding control algorithm to calculate the theoretical liquid adding mass and feed it back to the control module;

[0013] It also includes a control module, which is used to receive feedback signals from the background system to control the weighing module and the liquid adding module;

[0014] It also includes an impurity detection module, which is used to analyze the content of metal impurities dissolved in the polysilicon sample after being leached with acid solution.

[0015] As a further improvement of the present technical solution, the two-dimensional code recognition algorithm is used to identify sample information in real time, convert it into a digital signal and upload it.

[0016] As a further improvement of the technical solution, the weighing module includes a start weighing unit, a liquid adding weighing unit and a completion weighing unit;

[0017] The initial weighing unit is used to weigh the mass of the empty sample bottle initially placed. , and then the PLC controls the peeling operation to weigh the sample quality , and transmit it to the backend system;

[0018] The liquid adding weighing unit is controlled by PLC to weigh the total mass of the added liquid and the sample every ten seconds during the liquid adding process, and then subtract the sample mass. Get real-time dosing quality , and transmit it to the backend system;

[0019] The acid-added sample bottle weighing unit is used to measure the total mass of the liquid-added sample bottle after the liquid addition is completed, and transmit it to the background system.

[0020] As a further improvement of the technical solution, the liquid adding module is used to automatically add the acid solution of theoretical liquid adding mass to the sample, and includes an acid solution storage pumping unit, a liquid adding control execution unit and an acid solution cleaning unit;

[0021] Wherein, the acid storage pumping unit controls the acid flow rate through a high-precision semiconductor electronic-grade pump valve system;

[0022] The liquid addition control execution unit is based on the theoretical acid addition quality provided by the background system. , add to the sample bottle The weight of the acid solution is calculated and the actual weight is weighed after the addition is completed. Feedback to the backend system;

[0023] The acid cleaning unit is used to automatically clean the pipeline and pump valve after each liquid addition operation.

[0024] As a further improvement of the technical solution, the liquid addition control execution unit is based on the theoretical acid addition quality provided by the background system. , add to the sample bottle The quality of the acid solution is fed back to the background system after the addition is completed. The specific steps are as follows:

[0025] S3.1. The background system calculates the theoretical liquid addition mass After that, the liquid adding control execution unit starts the high-precision semiconductor electronic grade pump valve system and starts to add liquid according to the theoretical liquid adding quality. Add acid;

[0026] S3.2, the liquid adding control execution unit is based on the real-time liquid adding mass measured by the liquid adding weighing unit. , dynamically adjust the acid flow rate;

[0027] S3.3. After receiving the instruction to stop adding liquid from the background system, stop adding liquid and feed back the completion information of adding liquid to the background system.

[0028] As a further improvement of the technical solution, the background system includes a storage unit, a temperature and humidity model building unit and a calculation and analysis unit;

[0029] The storage unit receives and stores the sample digital signal from the identification module and the empty sample bottle mass from the weighing module in real time. , Sample quality and real-time dosing quality , and the actual weight of the liquid adding module (3) ;

[0030] The temperature and humidity model construction unit is used to construct a temperature compensation calculation model and a humidity compensation calculation model according to the influence of temperature and humidity environmental factors on the sample quality and the quality of the empty sample bottle during the calculation process, as follows:

[0031] S4.2.1. Collect the temperature of the current working environment in real time through sensors and relative humidity ;

[0032] S4.2.2. Obtaining the thermal expansion coefficient of the sample , Thermal expansion coefficient of sample bottle , sample humidity adsorption coefficient , Sample bottle humidity adsorption coefficient And the ambient reference temperature and base humidity ;

[0033] S4.2.3. Calculate the current ambient temperature With reference temperature The difference , and based on the principle of thermal expansion, a temperature compensation model is constructed:

[0034] ;

[0035] ;

[0036] in, is the coefficient of thermal expansion; is the initial object mass;

[0037] S4.2.4. Calculate the current relative humidity With reference humidity The difference , build a temperature compensation model:

[0038] ;

[0039] ;

[0040] in, is the humidity adsorption coefficient; is the initial object mass;

[0041] The calculation and analysis unit uses the background system liquid addition control algorithm to determine whether the sample information has been entered, whether a container is placed on the weighing module, and combines the temperature compensation calculation model and the humidity compensation calculation model to calculate the final sample mass and the final empty sample bottle mass, and calculate the theoretical liquid addition mass. , Calculate the liquid addition quality judgment value , determine whether the amount of acid added has reached the target value and stop adding acid and calculate whether the actual total mass is correct.

[0042] As a further improvement of the technical solution, the calculation and analysis unit uses the background system liquid addition control algorithm to determine whether the sample information has been entered, whether a container is placed on the weighing module, and combines the temperature compensation calculation model and the humidity compensation calculation model to calculate the final sample mass and the final empty sample bottle mass, and calculate the theoretical liquid addition mass. , Calculate the liquid addition quality judgment value , determine whether the amount of acid added has reached the target value and stop adding acid and calculate whether the actual total mass is correct;

[0043] The specific operation steps of the background system liquid addition control algorithm are as follows:

[0044] S4.3.1. Based on the sample digital signal, determine whether the current sample information has been entered into the background system, and feed back the existing sample information to the control module;

[0045] S4.3.2. Analyze the quality of empty sample bottles and sample quality , determine whether there are containers and samples on the weighing module;

[0046] S4.3.3. Calculate the final mass of the empty sample bottle by combining the temperature compensation calculation model and the humidity compensation calculation model and final sample quality , as follows:

[0047] Temperature and relative humidity compensated sample mass changes :

[0048] ;

[0049] Temperature and relative humidity compensated empty vial mass variation :

[0050] ;

[0051] Final sample quality :

[0052] ;

[0053] Final empty vial mass :

[0054] ;

[0055] S4.4. Calculate the theoretical liquid addition mass , and feed back the information of starting to add liquid to the control module;

[0056] ;

[0057] in, is the acid addition ratio coefficient;

[0058] S4.3.5. Calculate the liquid addition quality judgment value :

[0059] ;

[0060] in, The mass of liquid added for calibration;

[0061] S4.3.6. Determine whether the acid addition amount has reached the target value and stop adding acid:

[0062] If the real-time liquid addition quality Greater than or equal to the liquid addition quality judgment value and feed back the information of stopping liquid addition to the control module;

[0063] S4.3.7. Calculate actual weight Is it equal to the theoretical liquid addition mass? , Calibration of liquid filling quality , Final sample quality and final empty vial mass If the sum is equal, a liquid filling completion instruction is sent to the control module.

[0064] As a further improvement of the technical solution, the control module is used to receive feedback signals from the background system to control the weighing module and the liquid adding module, as follows:

[0065] S5.1, receiving sample information from the background system, and controlling the weighing module to start weighing;

[0066] S5.2, receiving the information of starting to add liquid from the background system, and controlling the adding module to start adding liquid;

[0067] S5.3, receiving the information of stopping adding liquid from the background system, controlling the adding liquid module to stop adding liquid and ending.

[0068] As a further improvement of the technical solution, the impurity detection module is used to analyze the content of metal impurities dissolved in the polysilicon sample after acid leaching, and the specific steps are as follows:

[0069] S6.1, the impurity detection module receives the solution that has been treated with acid;

[0070] S6.2. Use inductively coupled plasma mass spectrometry to analyze and detect metal impurities;

[0071] S6.3. Process and analyze the test data, generate a test report and transmit it to the backend system for storage.

[0072] On the other hand, the present invention provides a method for detecting metal impurities on the surface of polycrystalline silicon by automatic weighing and acid addition. Based on the above-mentioned system for detecting metal impurities on the surface of polycrystalline silicon by automatic weighing and acid addition, the method comprises the following steps:

[0073] S10.1. Use the built-in CMOS photosensitive device and the dedicated lens module to obtain the QR code information of the polysilicon sample, and use the QR code recognition algorithm to convert it into a digital signal, which is then transmitted to the backend system for storage and processing;

[0074] S10.2. Set the weighing process through the PLC program, measure the mass of the empty sample bottle, weigh the net weight of the sample after tare, and transmit the weighing data to the background system for calculation;

[0075] S10.3, according to the theoretical liquid addition mass, the acid solution is automatically added to the sample in proportion, the liquid addition mass is monitored in real time, and the acid addition process is adjusted according to the feedback data;

[0076] S10.4. Determine whether the predetermined amount of liquid added is reached according to the real-time weighing data, and stop adding acid after reaching the target;

[0077] S10.5. After the acid addition is completed, the actual total mass after the liquid addition is completed is measured again, and the actual total mass is transmitted to the background system for storage;

[0078] S10.6. Perform metal impurity analysis on the polysilicon sample solution after acid treatment, and use an inductively coupled plasma mass spectrometer to detect the metal content.

[0079] Compared with the prior art, the present invention has the following beneficial effects:

[0080] 1. The polysilicon surface metal impurity detection system and method that realizes automatic weighing and acid addition can accurately control the amount of acid added and adjust the acid flow in real time to avoid insufficient or excessive acid addition based on a high-precision semiconductor electronic-grade pump valve system and real-time dynamic weighing feedback.

[0081] 2. In the polysilicon surface metal impurity detection system and method that realizes automatic weighing and acid addition, the background system liquid addition control algorithm and multi-module collaborative working mechanism are used to automatically judge the sample status, accurately calculate the acid addition amount, monitor the acid addition process in real time, and finally generate a test report to ensure efficient acid addition automation during the detection process. BRIEF DESCRIPTION OF THE DRAWINGS

[0082] Figure 1 It is the overall flow chart of the present invention;

[0083] The meaning of each number in the figure is:

[0084] 1. Identification module; 2. Weighing module; 3. Liquid adding module; 4. Background system; 5. Control module; 6. Impurity detection module. DETAILED DESCRIPTION

[0085] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0086] See also Figure 1 As shown, the present invention provides a polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition, comprising:

[0087] Identification module 1, which obtains the polysilicon sample information two-dimensional code image through a built-in CMOS photosensitive device and a dedicated lens module, and converts it into a polysilicon digital signal using a two-dimensional code recognition algorithm and transmits it to the background system 4;

[0088] In this embodiment, the recognition module 1 obtains the polysilicon sample information two-dimensional code image through the built-in CMOS photosensitive device and the dedicated lens module, and converts it into a polysilicon sample digital signal using a two-dimensional code recognition algorithm and transmits it to the background system 4. The specific steps are as follows:

[0089] S1.1. The built-in CMOS photosensitive device is used to collect images, and the dedicated lens module recognizes the QR code image of the polysilicon sample;

[0090] The QR code information contains key information of the chemical sample, such as sample number, source, historical processing records, etc.

[0091] S1.2, using a two-dimensional code recognition algorithm to analyze the two-dimensional code image and convert the two-dimensional code image information into a digital signal;

[0092] S1.3, transmitting the digital signal to the background system 4 for storage and processing;

[0093] Among them, the two-dimensional code recognition algorithm is used to identify sample information in real time, convert it into a digital signal and upload it.

[0094] In this embodiment, each polysilicon sample is uniquely identified by a QR code to ensure information monitoring during acid addition and pretreatment to avoid confusion or loss; the identification module 1 works in conjunction with the background system 4 to achieve automatic storage and dynamic updating of sample information.

[0095] It also includes a weighing module 2, which sets a weighing process through a PLC program, measures the mass of an empty sample bottle, the mass of a sample, and the mass of liquid added in real time, and outputs the results to a background system 4;

[0096] In this embodiment, the weighing module 2 includes a start weighing unit, a liquid adding weighing unit and a completion weighing unit;

[0097] The initial weighing unit is used to weigh the mass of the empty sample bottle initially placed. , and then the PLC controls the peeling operation to weigh the sample quality , and transmit to the background system 4;

[0098] In this embodiment, the liquid adding weighing unit is controlled by PLC to weigh the total mass of the added liquid and the sample every ten seconds during the liquid adding process, and then subtract the sample mass. Get real-time dosing quality , and transmit to the background system 4;

[0099] In this embodiment, the acid-added sample bottle weighing unit is used to measure the total mass of the liquid-added sample bottle after the liquid addition is completed, and transmit it to the background system 4 .

[0100] In this embodiment, the PLC program is a control unit for controlling industrial equipment and processes. The start weighing unit, the liquid adding weighing unit and the completion weighing unit set the weighing process through the PLC program to achieve automatic control and accurate weighing. The specific process is as follows:

[0101] The PLC program of the start weighing unit first executes the weighing instruction of the empty sample bottle to collect the weight data of the empty sample bottle. The PLC control system performs the tare operation to deduct the weight of the sample bottle from the system. The sample is placed in the sample bottle. The system measures the total weight of the sample and the sample bottle by starting the weighing unit to obtain the net weight of the sample.

[0102] The real-time weighing data of the liquid adding weighing unit is automatically recorded by the PLC system and transmitted to the background system 4 every ten seconds. The system automatically determines the current acid addition amount and compares it with the preset theoretical acid addition amount;

[0103] The weighing unit is used to perform weighing again after the addition of liquid is completed, and measure the total weight of the sample bottle after the addition of liquid is completed.

[0104] It also includes a liquid adding module 3, which automatically adds acid to the polysilicon sample using a high-precision semiconductor electronic grade pump valve system according to the theoretical liquid adding mass calculated by the background system 4;

[0105] In this embodiment, the liquid adding module 3 is used to automatically add the acid solution of theoretical liquid adding mass to the sample, and includes an acid solution storage pumping unit, a liquid adding control execution unit and an acid solution cleaning unit;

[0106] Wherein, the acid storage pumping unit controls the acid flow rate through a high-precision semiconductor electronic-grade pump valve system;

[0107] In this embodiment, the acid solution is stored in a high-purity liquid storage container, and the acid solution storage pumping unit ensures that the acid solution is accurately pumped into the sample bottle under a suitable pressure to ensure that the acid solution is not contaminated during storage. The electronic-grade pump valve is used to accurately control the amount of acid solution pumped each time, and the pumping accuracy can reach the microliter level to ensure the accuracy of each acid addition;

[0108] In this embodiment, the liquid addition control execution unit calculates the acid addition quality according to the theoretical acid addition quality provided by the background system 4. , add to the sample bottle The weight of the acid solution is calculated and the actual weight is weighed after the addition is completed. Feedback to the backend system 4;

[0109] In this embodiment, the acid cleaning unit is used to automatically clean the pipeline and the pump valve after each liquid addition operation.

[0110] In this embodiment, the liquid addition control execution unit calculates the acid addition quality according to the theoretical acid addition quality provided by the background system 4. , add to the sample bottle The quality of the acid solution is fed back to the background system 4 after the addition is completed. The specific steps are as follows:

[0111] S3.1, backend system 4 calculates the theoretical liquid addition mass After that, the liquid adding control execution unit starts the high-precision semiconductor electronic grade pump valve system and starts to add liquid according to the theoretical liquid adding quality. Add acid;

[0112] S3.2, the liquid adding control execution unit is based on the real-time liquid adding mass measured by the liquid adding weighing unit. , dynamically adjust the acid flow rate;

[0113] S3.3, after receiving the instruction to stop adding liquid from the background system 4, stop adding liquid and feed back the information of completion of adding liquid to the background system 4.

[0114] It also includes a background system 4, which receives and stores data information from the identification module 1, the weighing module 2 and the liquid adding module 3, considers the influence of temperature and humidity environmental factors during the calculation process, builds a temperature compensation calculation model and a humidity compensation calculation model, optimizes the calculation of the final empty sample bottle mass and the final sample mass, and uses the background system liquid adding control algorithm to calculate the theoretical liquid adding mass and feed it back to the control module 5;

[0115] In this embodiment, the background system 4 includes a storage unit, a temperature and humidity model building unit, and a calculation and analysis unit;

[0116] The storage unit receives and stores the sample digital signal from the identification module 1 and the empty sample bottle mass from the weighing module 2 in real time. , Sample quality and real-time dosing quality , and the actual weight of the liquid adding module 3 ;

[0117] The temperature and humidity model construction unit is used to construct a temperature compensation calculation model and a humidity compensation calculation model according to the influence of temperature and humidity environmental factors on the sample quality and the quality of the empty sample bottle during the calculation process, as follows:

[0118] S4.2.1. Collect the temperature of the current working environment in real time through sensors and relative humidity ;

[0119] S4.2.2. Obtaining the thermal expansion coefficient of the sample , Thermal expansion coefficient of sample bottle , sample humidity adsorption coefficient , Sample bottle humidity adsorption coefficient And the ambient reference temperature and base humidity ;

[0120] S4.2.3. Calculate the current ambient temperature With reference temperature The difference , and based on the principle of thermal expansion, a temperature compensation model is constructed:

[0121] ;

[0122] ;

[0123] in, is the coefficient of thermal expansion; is the initial object mass;

[0124] In this embodiment, is the thermal expansion coefficient of the sample or thermal expansion coefficient of the sample bottle ; The empty sample bottle mass or sample quality ;

[0125] S4.2.4. Calculate the current relative humidity With reference humidity The difference , build a temperature compensation model:

[0126] ;

[0127] ;

[0128] in, is the humidity adsorption coefficient; is the initial object mass;

[0129] In this embodiment, the calculation and analysis unit uses the background system liquid addition control algorithm to determine whether the sample information has been entered, whether a container is placed on the weighing module, and combines the temperature compensation calculation model and the humidity compensation calculation model to calculate the final sample mass and the final empty sample bottle mass, and calculate the theoretical liquid addition mass. , Calculate the liquid addition quality judgment value , determine whether the amount of acid added has reached the target value and stop adding acid and calculate whether the actual total mass is correct.

[0130] In this embodiment, the calculation and analysis unit uses the background system liquid addition control algorithm to determine whether the sample information has been entered, whether a container is placed on the weighing module, and combines the temperature compensation calculation model and the humidity compensation calculation model to calculate the final sample mass and the final empty sample bottle mass, and calculate the theoretical liquid addition mass. , Calculate the liquid addition quality judgment value , determine whether the amount of acid added has reached the target value and stop adding acid and calculate whether the actual total mass is correct;

[0131] In this embodiment, the specific operation method and steps of the background system liquid addition control algorithm are as follows:

[0132] S4.3.1. Based on the sample digital signal, determine whether the current sample information has been entered into the background system, and feed back the existing sample information to the control module 5;

[0133] If the sample information has been entered, proceed to the next step; if not, the system will prompt the operator to enter the sample information or enter it automatically;

[0134] S4.3.2. Analyze the quality of empty sample bottles and sample quality , determine whether there are containers and samples on the weighing module;

[0135] If the correct container and sample are detected, the system continues operation; if the container or sample is not placed, the system will issue a warning and suspend operation;

[0136] S4.3.3. Calculate the final mass of the empty sample bottle by combining the temperature compensation calculation model and the humidity compensation calculation model and final sample quality , as follows:

[0137] Temperature and relative humidity compensated sample mass changes :

[0138] ;

[0139] In this embodiment, Select the thermal expansion coefficient of the sample ; Select as sample quality ;

[0140] Temperature and relative humidity compensated empty vial mass variation :

[0141] ;

[0142] In this embodiment, Select the thermal expansion coefficient for the vial ; Select Empty Vial Mass ;

[0143] Final sample quality :

[0144] ;

[0145] Final empty vial mass :

[0146] ;

[0147] S4.3.4. Calculate the theoretical liquid addition mass , and feed back the information of starting to add liquid to the control module 5;

[0148] ;

[0149] in, is the acid addition ratio coefficient;

[0150] S4.3.5. Calculate the liquid addition quality judgment value :

[0151] ;

[0152] in, The mass of liquid added for calibration;

[0153] S4.3.6. Determine whether the acid addition amount has reached the target value and stop adding acid:

[0154] If the real-time liquid addition quality Greater than or equal to the liquid addition quality judgment value , and feed back the information of stopping adding liquid to the control module 5;

[0155] S4.3.7. Calculate actual weight Is it equal to the theoretical liquid addition mass? , Calibration of liquid filling quality , Final sample quality and final empty vial mass If the sum is equal, a liquid addition completion instruction is issued to the control module 5. The system makes a final confirmation of the acid addition process and stores all data in the background system. After confirming the amount of acid added, all data, including sample weight, amount of acid added, acid addition time, etc., are automatically stored in the storage unit for subsequent analysis and recording.

[0156] It also includes a control module 5, which is used to receive feedback signals from the background system 4 to control the weighing module 2 and the liquid adding module 3;

[0157] In this embodiment, the control module 5 is used to receive the feedback signal from the background system 4 to control the weighing module 2 and the liquid adding module 3, as follows:

[0158] S5.1, receiving sample existence information from the background system 4, and controlling the weighing module 2 to start weighing;

[0159] S5.2, receiving the liquid adding start information from the background system 4, and controlling the liquid adding module 3 to start liquid adding;

[0160] S5.3, receiving the liquid adding stop information from the background system 4, controlling the liquid adding module 3 to stop the liquid adding and ending.

[0161] It also includes an impurity detection module 6, which is used to analyze the content of metal impurities dissolved in the polysilicon sample after acid leaching;

[0162] In this embodiment, the impurity detection module 6 is used to analyze the content of metal impurities dissolved in the polysilicon sample after acid leaching. The specific steps are as follows:

[0163] S6.1, the impurity detection module receives the solution that has been treated with acid;

[0164] S6.2. Use inductively coupled plasma mass spectrometry to analyze and detect metal impurities;

[0165] S6.3, process and analyze the test data, generate a test report and transmit it to the backend system 4 for storage.

[0166] In addition, the present invention introduces a static mechanical property collection and analysis method used in a polysilicon surface metal impurity detection system that realizes automatic weighing and acid addition.

[0167] A method for detecting metal impurities on the surface of polycrystalline silicon by automatic weighing and acid addition is provided. Based on the above-mentioned system for detecting metal impurities on the surface of polycrystalline silicon by automatic weighing and acid addition, the method comprises the following steps:

[0168] S10.1. Use the built-in CMOS photosensitive device and the dedicated lens module to obtain the QR code information of the polysilicon sample, and use the QR code recognition algorithm to convert it into a digital signal, which is then transmitted to the backend system for storage and processing;

[0169] S10.2. Set the weighing process through the PLC program, measure the mass of the empty sample bottle, weigh the net weight of the sample after tare, and transmit the weighing data to the background system for calculation;

[0170] S10.3, according to the theoretical liquid addition mass, the acid solution is automatically added to the sample in proportion, the liquid addition mass is monitored in real time, and the acid addition process is adjusted according to the feedback data;

[0171] S10.4. Determine whether the predetermined amount of liquid added is reached according to the real-time weighing data, and stop adding acid after reaching the target;

[0172] S10.5. After the acid addition is completed, the actual total mass after the liquid addition is completed is measured again, and the actual total mass is transmitted to the background system for storage;

[0173] S10.6. Perform metal impurity analysis on the polysilicon sample solution after acid treatment, and use an inductively coupled plasma mass spectrometer to detect the metal content.

[0174] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments, and the above embodiments and descriptions are only preferred examples of the present invention, and are not intended to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.

Claims

1. A polysilicon surface metal impurity detection system with automatic weighing and acid addition is realized, characterized in that: include: An identification module (1), wherein the identification module (1) obtains a two-dimensional code image of polysilicon sample information through a built-in CMOS photosensitive device and a dedicated lens module, and converts the image into a polysilicon digital signal using a two-dimensional code recognition algorithm and transmits the signal to a background system (4); The specific steps are as follows: S1.

1. The built-in CMOS photosensitive device is used to collect images, and the dedicated lens module recognizes the QR code image of the polysilicon sample; S1.2, using a two-dimensional code recognition algorithm to analyze the two-dimensional code image and convert the two-dimensional code image information into a digital signal; S1.3, transmitting the digital signal to the background system (4) for storage and processing; A weighing module (2), wherein the weighing module (2) sets a weighing process through a PLC program, measures the mass of an empty sample bottle, the mass of a sample, and the mass of liquid added in real time, and outputs the mass to a background system (4); A liquid adding module (3), wherein the liquid adding module (3) automatically adds acid liquid to the polysilicon sample using a high-precision semiconductor electronic grade pump valve system according to the theoretical liquid adding mass calculated by the background system (4); A backend system (4), wherein the backend system (4) receives and stores data information from the identification module (1), the weighing module (2) and the liquid adding module (3), considers the influence of temperature and humidity environmental factors during the calculation process, constructs a temperature compensation calculation model and a humidity compensation calculation model, optimizes the calculation of the final empty sample bottle mass and the final sample mass, and uses the backend system liquid adding control algorithm to calculate the theoretical liquid adding mass and feed it back to the control module (5); A control module (5), the control module (5) being used to receive a feedback signal from a background system (4) to control the weighing module (2) and the liquid adding module (3); An impurity detection module (6), wherein the impurity detection module (6) is used to analyze the content of metal impurities dissolved in the polysilicon sample after being leached with acid solution.

2. The polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition according to claim 1 is characterized in that: The two-dimensional code recognition algorithm is used to identify sample information in real time, convert it into a digital signal and upload it.

3. The polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition according to claim 1 is characterized in that: The weighing module (2) comprises a start weighing unit, a liquid adding weighing unit and a completion weighing unit; The initial weighing unit is used to weigh the mass of the empty sample bottle initially placed. , and then the PLC controls the peeling operation to weigh the sample quality , and transmit it to the backend system (4); The liquid adding weighing unit is controlled by PLC to weigh the total mass of the added liquid and the sample every ten seconds during the liquid adding process, and then subtract the sample mass. Get real-time dosing quality , and transmit it to the backend system (4); The completion weighing unit is used to measure the total mass of the liquid-filled sample bottle after the liquid-filling is completed, and transmits it to the background system (4).

4. The polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition according to claim 1, characterized in that: The liquid adding module (3) is used to automatically add the acid solution of theoretical liquid adding mass into the sample, and comprises an acid solution storage pumping unit, a liquid adding control execution unit and an acid solution cleaning unit; Wherein, the acid storage pumping unit controls the acid flow rate through a high-precision semiconductor electronic-grade pump valve system; The liquid addition control execution unit is based on the theoretical acid addition quality provided by the background system (4). , add to the sample bottle The weight of the acid solution is calculated and the actual weight is weighed after the addition is completed. Feedback to the backend system (4); The acid cleaning unit is used to automatically clean the pipeline and pump valve after each liquid addition operation.

5. The polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition according to claim 4 is characterized in that: The liquid addition control execution unit is based on the theoretical acid addition quality provided by the background system (4). , add to the sample bottle The quality of the acid solution is then fed back to the background system (4) after the addition is completed. The specific steps are as follows: S3.1, the backend system (4) calculates the theoretical liquid addition mass After that, the liquid adding control execution unit starts the high-precision semiconductor electronic grade pump valve system and starts to add liquid according to the theoretical liquid adding quality. Add acid; S3.2, the liquid adding control execution unit is based on the real-time liquid adding mass measured by the liquid adding weighing unit. , dynamically adjust the acid flow rate; S3.

3. After receiving the instruction to stop adding liquid from the background system (4), the liquid addition is stopped, and the completion information of the liquid addition is fed back to the background system (4).

6. The polysilicon surface metal impurity detection system realizing automatic weighing and acid addition according to claim 1 is characterized in that: The background system (4) includes a storage unit, a temperature and humidity model building unit and a calculation and analysis unit; The storage unit receives and stores in real time the sample digital signal from the identification module (1) and the mass of the empty sample bottle from the weighing module (2). , Sample quality and real-time dosing quality , and the actual weight of the liquid adding module (3) ; The temperature and humidity model construction unit is used to construct a temperature compensation calculation model and a humidity compensation calculation model according to the influence of temperature and humidity environmental factors on the sample quality and the quality of the empty sample bottle during the calculation process, as follows: S4.2.

1. Collect the temperature of the current working environment in real time through sensors and relative humidity ; S4.2.

2. Obtaining the thermal expansion coefficient of the sample , Thermal expansion coefficient of sample bottle , sample humidity adsorption coefficient , Sample bottle humidity adsorption coefficient And the ambient reference temperature and base humidity ; S4.2.

3. Calculate the current ambient temperature With reference temperature The difference , and based on the principle of thermal expansion, a temperature compensation model is constructed: ; ; in, is the coefficient of thermal expansion; is the initial object mass; S4.2.

4. Calculate the current relative humidity With reference humidity The difference , build a temperature compensation model: ; ; in, is the humidity adsorption coefficient; is the initial object mass; The calculation and analysis unit uses the background system liquid addition control algorithm to determine whether the sample information has been entered, whether a container is placed on the weighing module, and combines the temperature compensation calculation model and the humidity compensation calculation model to calculate the final sample mass and the final empty sample bottle mass, and calculate the theoretical liquid addition mass. , Calculate the liquid addition quality judgment value , determine whether the amount of acid added has reached the target value and stop adding acid and calculate whether the actual total mass is correct.

7. The polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition according to claim 6, characterized in that: The calculation and analysis unit uses the background system liquid addition control algorithm to determine whether the sample information has been entered, whether a container is placed on the weighing module, and combines the temperature compensation calculation model and the humidity compensation calculation model to calculate the final sample mass and the final empty sample bottle mass, and calculate the theoretical liquid addition mass. , Calculate the liquid addition quality judgment value , determine whether the amount of acid added has reached the target value and stop adding acid and calculate whether the actual total mass is correct; The specific operation steps of the background system liquid addition control algorithm are as follows: S4.3.

1. Based on the sample digital signal, determine whether the current sample information has been entered into the background system, and feed back the existing sample information to the control module (5); S4.3.

2. Analyze the quality of empty sample bottles and sample quality , determine whether there are containers and samples on the weighing module; S4.3.

3. Calculate the final mass of the empty sample bottle by combining the temperature compensation calculation model and the humidity compensation calculation model and final sample quality , as follows: Temperature and relative humidity compensated sample mass changes : ; Temperature and relative humidity compensated empty vial mass variation : ; Final sample quality : ; Final empty vial mass : ； S4.3.

4. Calculate the theoretical liquid addition mass and feeds back the information of starting to add liquid to the control module (5); ; in, is the acid addition ratio coefficient; S4.3.

5. Calculate the liquid addition quality judgment value : ; in, The mass of liquid added for calibration; S4.3.

6. Determine whether the acid addition amount has reached the target value and stop adding acid: If the real-time liquid addition quality Greater than or equal to the liquid addition quality judgment value and feeds back the information of stopping the liquid addition to the control module (5); S4.3.

7. Calculate actual weight Is it equal to the theoretical liquid addition mass? , Calibration of liquid filling quality , Final sample quality and final empty vial mass If the sum is equal, a liquid addition completion instruction is sent to the control module (5).

8. The polysilicon surface metal impurity detection system realizing automatic weighing and acid addition according to claim 1 is characterized in that: The control module (5) is used to receive feedback signals from the background system (4) to control the weighing module (2) and the liquid adding module (3), as follows: S5.1, receiving sample existence information from the background system (4), and controlling the weighing module (2) to start weighing; S5.2, receiving the liquid adding start information from the background system (4), and controlling the liquid adding module (3) to start liquid adding; S5.3, receiving the liquid adding stop information from the background system (4), controlling the liquid adding module (3) to stop liquid adding and ending.

9. The polysilicon surface metal impurity detection system for realizing automatic weighing and acid addition according to claim 1, characterized in that: The impurity detection module (6) is used to analyze the content of metal impurities dissolved in the polysilicon sample after acid leaching. The specific steps are as follows: S6.1, the impurity detection module receives the solution that has been treated with acid; S6.

2. Use inductively coupled plasma mass spectrometry to analyze and detect metal impurities; S6.

3. Process and analyze the test data, generate a test report and transmit it to the backend system (4) for storage.

10. A method for detecting metal impurities on the surface of polycrystalline silicon by automatic weighing and acid addition, based on a system for detecting metal impurities on the surface of polycrystalline silicon by automatic weighing and acid addition as claimed in any one of claims 1 to 9, characterized in that: The steps include: S10.

1. Use the built-in CMOS photosensitive device and the dedicated lens module to obtain the QR code information of the polysilicon sample, and use the QR code recognition algorithm to convert it into a digital signal, and transmit it to the background system for storage and processing; S10.

2. Set the weighing process through the PLC program, measure the mass of the empty sample bottle, weigh the net weight of the sample after tare, and transmit the weighing data to the background system for calculation; S10.3, according to the theoretical liquid addition mass, the acid solution is automatically added to the sample in proportion, the liquid addition mass is monitored in real time, and the acid addition process is adjusted according to the feedback data; S10.

4. Determine whether the predetermined amount of liquid added is reached according to the real-time weighing data, and stop adding acid after reaching the target; S10.

5. After the acid addition is completed, the actual total mass after the liquid addition is completed is measured again, and the actual total mass is transmitted to the background system for storage; S10.

6. Perform metal impurity analysis on the polysilicon sample solution after acid treatment, and use an inductively coupled plasma mass spectrometer to detect the metal content.

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