Method for trapping and determining metal ions in high-purity organic silicon material for chip

Abstract

The invention belongs to the technical field of high-purity organic silicon chemical industry, and particularly relates to a method for enriching and determining metal ions in a high-purity organic silicon material for a chip. Comprising the following steps: building a trapping device, cleaning a sample bottle, treating a to-be-detected sample, treating a control group sample, preparing a standard solution, and performing ICP-MS (Inductively Coupled Plasma Mass Spectrometry) on-machine According to the method, the environmental influence in the metal trapping process is avoided, the sample treatment time and the test time are shortened by 339.2%, the parallelism between the samples is good, the RSD is smaller than 10%, the standard addition recovery rate of the samples can be stabilized at 90%-110%, and the standard addition recovery rate of a sample instrument treated by the method can be stabilized at 97%-102%, so that the method is friendly to the instrument and small in Si pollution.

Description

Technical Field

[0001] The present invention belongs to the technical field of high-purity organosilicon chemicals, and specifically relates to a method for capturing and measuring metal ions in high-purity organosilicon materials for chips. Background Art

[0002] In high-end chip manufacturing, silicone materials, thanks to their thermal stability, mechanical flexibility, and dielectric properties, have become key functional materials supporting advanced manufacturing processes. In the packaging and protection phase, they elastically fill interfacial gaps to buffer high-frequency mechanical stresses in miniaturized structures, preventing moisture and contaminants from corroding nanoscale circuits. In high-density interconnects, silicone-based low-k dielectrics effectively reduce interlayer signal delays and crosstalk, alleviating the constraints of RC delay on computing speed. As the manufacturing process evolves to 3nm and below, their molecular designability will further drive nanocomposite modifications (such as porous structure regulation and directional heat conduction network construction), addressing limiting issues such as quantum tunneling and electromagnetic interference, and supporting breakthroughs in computing power density, energy efficiency, and reliability for next-generation chips.

[0003] However, the trace metal ions (such as Na + , K + , Ca 2+ 、Fe 2+ 、Cu 2+ The mobility of metal ions allows them to penetrate into the core areas of the chip under high temperature or electric field conditions. This can trigger gate dielectric interface defects, leading to a surge in leakage current and the risk of oxide breakdown, causing transistor threshold voltage to drift beyond design tolerances. Contamination of photoresist or anti-reflective coatings can cause sub-nanometer pattern distortion (such as EUV lithography critical dimension shifts), while penetration into copper interconnect layers can induce electrochemical corrosion, significantly increasing interconnect resistance and even the risk of short circuits. Therefore, the ability to accurately capture and measure the content of metal impurities is crucial for high-end chip process quality and reliability control, and is crucial for the longevity of the product.

[0004] Currently, hydrofluoric acid digestion is commonly used to test the metal ion content of industrial-grade organosilicon materials. However, high-purity silicon materials (referring to organosilicon products with a SEMI grade of ≥G4 (metal ion impurities ≤ 0.1 ppb)) contain relatively low metal ion content. The violent digestion reaction can easily lead to element loss, making accurate measurement difficult. Furthermore, hydrofluoric acid reacts with element B to form BF4 gas, which evaporates and cannot be accurately captured. Another method involves high-temperature, open-air evaporation of PTFE in a beaker followed by reconstitution in nitric acid. This method requires high heating temperatures, is also prone to element loss, and is susceptible to environmental contamination. Furthermore, some silicon-containing materials are diluted with acid and then directly applied to the instrument. However, most organosilicon-containing materials have low solubility in inorganic solvents, and direct application can easily lead to silicon deposition on the instrument, causing irreversible contamination.

[0005] Therefore, there is currently a lack of efficient and accurate methods for determining metal ions in high-purity organosilicon materials used in chips. Given the rapid development of the semiconductor industry, it is extremely important to develop efficient methods for detecting metal ions in high-purity organosilicon materials used in chips. Summary of the Invention

[0006] The purpose of the present invention is to propose a method for efficiently capturing and determining metal ions from ultra-high purity silicon materials in response to the problems that the existing metal ion capture process of organic silicon materials is easily affected by the environment, the sample processing cycle is long, the test result spike recovery rate is poorly parallel to the sample, and the sample on the machine is prone to contaminating the instrument. The method avoids the environmental impact of the metal capture process, the sample processing time and test time are shortened by more than 330%, the parallelism between samples is good, RSD < 10%, the sample spike recovery rate can be stabilized at 90%-110%, and the sample instrument spike recovery rate after treatment by this method can be stabilized at 97%-102%, indicating that this method is more friendly to the instrument and has less Si pollution. The specific technical solution is as follows: A method for efficiently capturing and determining metal ions from ultra-high purity organic silicon materials for chips, comprising the following steps: (1) Construction of capture device like Figure 1 As shown, place the PFA container with vents on the heating plate, collect all the vents of the PFA container into a main pipe, connect the main pipe to the rear-end condenser, connect the condenser to the adsorption device, connect the adsorption device outlet to the vacuum pump, and evacuate until the pressure in the PFA container reaches -30kPa. Then stop, and the collection device is completed. In some preferred cases, specially customized PFA containers with air vents are arranged in sequence on the heating plate, all the air vents of the PFA containers are connected to a main pipe, the main pipe is connected to the two-stage condensing device at the rear end, the condensing device is connected to the adsorption device, the outlet of the adsorption device is connected to the vacuum pump, and a pressure gauge is installed between the vacuum pump and the adsorption device to detect the system pressure change in real time. After all components are connected, the vacuum pump is started and stopped after the pressure reaches -30kPa. The pressure change on the pressure gauge is observed. If the pressure change is within 1kPa within 5 minutes, it proves that the system is airtight and the capture device is completed.

[0007] (2) Sample bottle cleaning Heat and boil the PFA container in high-purity nitric acid solution several times until the concentration of each metal ion in the high-purity nitric acid solution is less than 10 ppt; In some preferred cases, prepare a PFA container (made of a material suitable for heating at 200°C and vacuum-resistant) rinsed with ultrapure water (resistivity: 18.2 MΩ / cm). First, fill the PFA container with nitric acid (metal impurities within 10 ppt) until the liquid level is approximately 1 cm from the top edge of the container. Heat to 180°C and boil for 30-60 minutes. Discard the boiled nitric acid and replace with clean nitric acid, repeating the above steps. Repeat this process 3-5 times until the metal ion concentration of the nitric acid solution is less than 10 ppt, or meets the required concentration.

[0008] (3) Processing of test samples Place the high-purity organosilicon material sample to be tested into a cleaned PFA container, tighten the screw cap and place it on the heating plate. Open the refrigerant of the condenser tube, start the vacuum pump, adjust the temperature of the heating plate, wait for the sample in the PFA container to completely evaporate, turn off the vacuum, add high-purity nitric acid to the PFA container, turn on the heating plate after adding the acid, set the leaching temperature and time, and leaching the metal ions. After the leaching is completed, wait for the nitric acid solution to cool to room temperature and set aside; In some preferred embodiments, a vacuum-resistant PFA container with a top connection to the outside is prepared. After the solvent is cleaned (see step 2 for specific cleaning steps and criteria), the sample to be processed is placed in the container. The PFA container with the sample is screwed on tightly and placed on a hot plate. The refrigerant in the two-stage condenser is then opened. Once the temperature drops to a specified level, the vacuum pump is turned on. The vacuum pressure is set based on the specific sample properties. The hot plate temperature is adjusted. After the sample in the PFA container is completely evaporated (determined by weighing it on a balance), the vacuum is turned off. High-purity nitric acid is added to the PFA container at a ratio of 1:1.5-2 to the sample volume, ensuring that the nitric acid solution is higher than the sample solution. After the acid is added, the hot plate is turned on, the extraction temperature and time are set, and the metal ions are extracted. After the extraction is complete, the nitric acid solution is cooled to room temperature and set aside.

[0009] To ensure the reliability of the results, multiple groups of parallel control samples need to be processed simultaneously, including samples without standard solution, samples with standard solution, samples with standard solution after testing, and blank control group. The above processing method is shown in step 3. No sample is added to the blank control group, and the remaining steps are the same as step (3). Ensuring the reliability of the results also involves preparing standard solutions and establishing a standard working curve. Specifically, the multi-element mixed standard solution is diluted stepwise to 1 μg / L (the maximum single dilution factor is 100 times), and then a gradient standard solution with concentrations of 0.05, 0.1, 0.15, and 0.2 μg / L is prepared. This is then tested on the ICP-MS to establish a standard working curve. The absorbed sample solution is then measured using the same detection conditions.

[0010] In the present invention, the amount of samples processed in the next step (4) of the method for efficiently capturing and determining metal ions in high-purity organic silicon materials is 16, including 4 samples without adding standard solution, 4 samples with adding standard solution, 4 samples with adding standard solution after detection, and 4 blank control group samples.

[0011] (4) ICP-MS on-machine testing In some preferred cases, after the instrument plasma is preheated (about 30 minutes), the cone port is installed and the gas path (argon, collision gas, etc.) is checked. The blank control sample is first introduced, and then the mixed standard solution is introduced in order from low concentration to high concentration to obtain the standard curve of each metal ion. Finally, the sample to be tested prepared in the test step (4) is introduced.

[0012] The metal ion concentration in the sample to be tested is calculated according to the following formula:

[0013] The high-purity organic silicon material is ≥G4 according to the SEMI grade classification standard, and the metal ion impurities are ≤0.1ppb.

[0014] High-purity silicone materials that are liquid at room temperature include any of the following: (1) The general structural formula is R 4-n SiX n Wherein: n = 0, 1, 2, 3, R is any one of a C1-C6 straight chain alkane or a C3-C6 branched chain alkane, and X is a halogen or -H; (2) The general structural formula is [(CH3)2SiO] n Where: n = 3, 4, 5 (3) The general structural formula is SiH 4-n (NR1R2) nAminosilane, wherein n=1, 2, 3, 4, R1 and R2 are any one of C1-C6 straight-chain alkane and C3-C6 branched alkane, and R1 and R2 are the same or different.

[0015] The invention discloses an efficient capture and determination method for metal ions in high-purity organosilicon materials, characterized in that the high-purity organosilicon materials include any one of monomethyltrichlorosilane, dimethyldichlorosilane, trimethylmonochlorosilane, tetramethylsilane, octamethylcyclotetrasiloxane, bis(tert-butylamino)silane, bis(dihexylamino)silane, bis(dimethylamino)dimethylsilane, tris(dimethylamino)silane, diisopropylaminesilane, hexamethyldisilazane, diethoxymethylsilane, dimethyldimethoxysilane, and tetraethoxysilane.

[0016] In the step (1) shown, the condensation temperature of the two-stage condensation device is 5-10°C, and the filling material in the adsorption device is activated carbon.

[0017] In step (2), the volume of the PFA container is 30-200 ml, the concentration of high-purity nitric acid is 2%-55%, and the single metal concentration is less than 10 ppt.

[0018] In step (3), the amount of sample to be processed is 20 g to 50 g, the temperature of the heating plate is 20 to 55° C., and the vacuum degree is -10 to -100 kPa.

[0019] The concentration of high-purity nitric acid added in step (3) is 2%-10%, and the single metal concentration is less than 10 ppt. The single metal ion includes one or more combinations of Na, Mg, Al, K, Ca, Fe, Cu, Ni, and Zn.

[0020] The extraction temperature is 40-80°C, and the extraction time is 30min-60min.

[0021] The working conditions of the inductively coupled plasma mass spectrometer in step (4) are as follows: high frequency power of 0.5-1.5 kW, sampling depth of 5.0-10 mm, nebulizing gas flow rate of 0.5-0.7 L / min, and compensation gas flow rate of 0.4-0.9 L / min.

[0022] The beneficial effects of the present invention are as follows: the detection method of the present invention uses negative pressure and low temperature to evaporate the sample and acid to extract the metal ions to make the high-purity organosilicon material that cannot be directly diluted on the machine into an inorganic nitric acid solution that can be detected on the machine, and uses an inductively coupled plasma mass spectrometer (ICP-MS) to determine the metal ions in the high-purity organosilicon material. The high-purity organosilicon material to be tested is placed in a PFA container, and by changing the pressure in the container and appropriately increasing the sample temperature, the organic components in the sample to be tested are quickly removed while the non-volatile inorganic metal impurities are enriched. Since the PFA container containing the sample to be tested has only one vent hole that is the same as the outside world, it can effectively avoid metal impurities such as Na in the environment. + , K + , Ca 2+ 、Fe 2+ 、Cu 2+ This method can process multiple samples simultaneously, ensuring consistent conditions across samples. Simultaneous processing of multiple samples can effectively improve detection efficiency. After evaporation, metal ions were extracted with high-purity nitric acid and detected by ICP-MS. This method mitigates environmental impacts during metal capture, shortens sample processing time by 339.2%, and demonstrates excellent parallelism between samples, with RSDs below 10%. Sample spike recoveries are consistently between 90% and 110%, and instrument spike recoveries for samples treated with this method are consistently between 97% and 102%, demonstrating that this method is instrument-friendly and minimizes Si contamination. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 Schematic diagram of the enrichment device.

[0024] Among them: 1. Pressure-resistant perforated PFA container, 2. Graphite heating plate, 3. Primary condenser, 4. Primary condensate collection tank, 5. Secondary condenser, 6. Secondary condensate collection tank, 7. Adsorber, 8. Pressure gauge, 9. Vacuum pump Figure 2 is the standard curve of Na ion concentration-signal intensity.

[0025] Figure 3 is the standard curve of Mg ion concentration-signal intensity.

[0026] Figure 4 is the standard curve of Al ion concentration-signal intensity.

[0027] Figure 5 is the standard curve of K ion concentration-signal intensity.

[0028] Figure 6 is the Ca ion concentration-signal intensity standard curve.

[0029] Figure 7is the standard curve of Fe ion concentration-signal intensity.

[0030] Figure 8 is the standard curve of Cu ion concentration-signal intensity.

[0031] Figure 9 is the Ni ion concentration-signal intensity standard curve.

[0032] Figure 10 is the Zn ion concentration-signal intensity standard curve. DETAILED DESCRIPTION

[0033] (1) Construction of capture device like Figure 1 As shown, specially customized PFA containers with air vents are arranged on the heating plate in sequence, all the air vents of the PFA containers are connected to a main pipe, the main pipe is connected to the two-stage condensing device at the rear end, the adsorption device is connected after the condensing device, the outlet of the adsorption device is connected to the vacuum pump, and a pressure gauge is installed between the vacuum pump and the adsorption device to detect the system pressure change in real time. After all the components are connected, the vacuum pump is started and stopped after the pressure reaches -30kPa. The pressure change on the pressure gauge is observed. If the pressure change is within 1kPa within 5 minutes, it proves that the system is airtight and the capture device is completed.

[0034] (2) Sample bottle cleaning Prepare a clean PFA container (made of a material heatable at 200°C and vacuum-resistant). First, fill the container with nitric acid (single metal concentration <10 ppt) (metal impurities within 10 ppt) until the liquid level is approximately 1 cm from the top edge of the container. Heat to 180°C and boil for 30-60 minutes. Discard the boiled nitric acid and replace with clean nitric acid, then repeat the above steps. Repeat this process five times until the metal ion concentration of the nitric acid solution is less than 10 ppt or meets the required concentration.

[0035] (3) Processing of test samples First, prepare a vacuum-resistant PFA container with a top connection to the outside. After cleaning the solvent (see Step 2 for specific cleaning steps and criteria), place 25g of the sample to be processed (high-purity silicone product, purity G4 grade or higher, single metal concentration <0.1 ppb). Tighten the threaded cap of the PFA container containing the sample and place it on a hot plate. Then, open the refrigerant in the two-stage condenser. After the temperature drops to 10°C, start the vacuum pump and set the vacuum pressure to -50 kPa. Adjust the hot plate temperature to 30°C. After the sample in the PFA container is completely evaporated (determined by weighing the sample before and after on a balance), turn off the vacuum and add 5% high-purity nitric acid to the PFA container at a ratio of 1:2 to the sample mass, ensuring that the nitric acid solution is higher than the sample solution. After adding the acid, turn on the hot plate and extract the metal ions at 60°C for 30 minutes. After the extraction is complete, allow the nitric acid solution to cool to room temperature and set aside.

[0036] (4) Treatment of control group samples Standard solution preparation The multi-element mixed standard solution was diluted step by step to 1 μg / L (the maximum single dilution factor was no more than 100 times), and then prepared into gradient standard solutions with concentrations of 0.05, 0.1, 0.15, and 0.2 μg / L, respectively. The standard working curve was established by ICP-MS testing (e.g. Figure 2-10 ). The absorbed sample solution was then measured using the same detection conditions.

[0037] The multi-element mixed standard solution is a ready-made product.

[0038] (5) To ensure the reliability of the results, 16 parallel samples need to be processed simultaneously, including 4 samples without adding standard solution obtained by the treatment method in step (3), 4 samples with standard solution added to the samples after treatment in step (3), 4 samples with standard solution added after detection, and 4 blank control groups. The above treatment method is as shown in step 3. No sample is added to the blank control group. The remaining steps are the same as step (3).

[0039] The sample without adding standard solution refers to the sample in step (3).

[0040] The spiked standard solution sample refers to a separately prepared spiked standard solution sample with a concentration of 50-100ppt.

[0041] Adding standard solution to the sample after testing means: 1. To monitor the stability of the instrument, it is necessary to test the sample and then add the standard solution for testing. For example, the iron content in sample A is 100ppt. After the test is completed, add 100ppt of iron standard solution for testing. If the test result is about 200ppt, it indicates that the instrument is stable and there is no signal attenuation. At the same time, it indicates that the sample obtained by the pretreatment method has no effect on the instrument. It also prepares for the next sample test to ensure the accuracy of the subsequent test data. This step is often performed halfway and at the end of the test. For example, if a total of 20 samples are tested on the same day, before the 11th sample is randomly tested, the previous sample is spiked and tested on the machine. After the 20th sample is tested, the previous sample is spiked and tested on the machine again.

[0042] 2.Concentration of standard solution: 50-100ppt.

[0043] The blank control group refers to the same steps as step (3) except that no sample is added.

[0044] (6) ICP-MS on-machine testing After the instrument plasma is preheated (about 30 minutes), install the cone and check the gas path (argon, collision gas, etc.). First, introduce the blank control sample, and then introduce the mixed standard solution in order from low concentration to high concentration to obtain the standard curve of each metal ion (the concentration of each element in the mixed standard solution is known. After dilution, the signal intensity corresponding to different concentrations of each element can be obtained, and then the standard curve is established). Finally, introduce the sample to be tested prepared in the test step (4).

[0045] (7) Results analysis

[0046] The present invention is described in more detail below with reference to the following examples and comparative examples, but the present invention is not limited thereto.

[0047] Example 1 According to the above specific implementation steps, the specific sample is electronic-grade hexamethyldisilazane (HMDS), a photoresist adhesive used in the photolithography process of chip manufacturing. According to the calculation formula (1), the measured data and the measured sample mass are substituted into the formula to directly calculate the metal ion concentration. The metal ions to be measured in this test are: sodium ion, magnesium ion, aluminum ion, potassium ion, calcium ion, iron ion, copper ion, nickel ion, and zinc ion.

[0048] The ion contents detected by the method described in Example 1 are shown in Table 1 below.

[0049] Table 1

[0050] From the above data, it can be seen that the RSDs are all within 10%, and the four groups of parallel samples have good parallelism. In addition, in order to verify the feasibility and reliability of the sample processing method, four groups of samples were selected in step (4) for spike addition, and the concentration of the standard solution was 50ppt. Then, the sample concentration was taken as the average value of the four groups of parallel samples in Table (1). The spike recovery rate was calculated before and after spike addition. The specific results are shown in Table 2 below.

[0051] Table 2

[0052] The above data are the average recoveries of the four groups of samples spiked. The recovery rates of each element can be maintained between 90% and 110%, indicating that the pretreatment method has high reliability. In addition, to verify the detection stability of the instrument, four groups of samples were selected for testing in step (4). After the test, a standard solution with a concentration of 50 ppt was added to the samples. The instrument was tested again and the recovery rates were calculated before and after the spike addition. The specific test results are shown in Table 3 below.

[0053] Table 3

[0054] The above data is the average value of the four groups of samples after instrument detection. After further addition of spikes, the samples were tested on the instrument. The results showed that the recovery rate of each element was stable between 97% and 102%, proving that this method has no attenuation on the signal intensity of each element during the instrument detection process.

[0055] Example 2 The difference from Example 1 is that the system pressure in step (3) of this embodiment is -40 kPa, and the rest is the same as Example 1. Example 3 The difference from Example 1 is that the system pressure in step (3) of this embodiment is -60 kPa, and the rest is the same as Example 1.

[0056] Example 4 The difference from Example 1 is that the sample heating temperature of this example is 35° C., and the rest is the same as Example 1. Example 5 The difference from Example 1 is that the sample heating temperature of this example is 40° C., and the rest is the same as Example 1. Example 6 The difference from Example 1 is that the sample amount of this example is 30 g, and the rest is the same as Example 1. Example 7 The difference from Example 1 is that the sample amount of this example is 40 g, and the rest is the same as Example 1.

[0057] The metal ions to be tested in this test are: sodium ion, magnesium ion, aluminum ion, potassium ion, calcium ion, iron ion, copper ion, nickel ion, and zinc ion. The ion contents detected by the methods described in the examples are shown in Table 4.

[0058] Table 4

[0059] Comparative Example 1 In order to verify that the evaporation temperature and pressure have different effects on the metal elements in high-purity silicone materials, this comparative example uses high-temperature open evaporation to remove the organic components in the sample. The specific operation steps are as follows: (1) Construction of capture device Same as Example 1 (2) Sample bottle cleaning Same as Example 1 (3) Processing of test samples First, prepare a PFA container and place 25g of the sample to be processed on a hot plate. Adjust the hot plate temperature to 150°C. Wait until the sample in the PFA container is completely evaporated (determined by weighing it on a scale). Then, add nitric acid solution in a 1:2 ratio to the sample volume, ensuring that the height of the added nitric acid solution is higher than the sample solution. After adding the acid, turn on the hot plate and extract the metal ions at 60°C for 30 minutes. After extraction, allow the nitric acid solution to cool to room temperature and set aside.

[0060] (4) Treatment of control group samples Same as Example 1 (5) Preparation of standard solution Same as Example 1 (6) ICP-MS / MS on-machine testing Same as Example 1 (7) Results analysis Same as Example 1 Comparative Example 2 In order to verify that the digestion method has different effects on the metal elements in high-purity organosilicon materials, this comparative example uses high-temperature and high-pressure digestion to remove the organic components in the sample. The other steps are the same as those in Example 1. The specific operation steps are as follows: (1) Sample bottle cleaning Same as Example 1 (2) Processing of test samples First, prepare a vacuum-resistant PFA container. After cleaning the solvent (see Step 2 for specific cleaning steps and criteria), place 5g of the sample to be processed in the container. Add 15g of high-purity (<10 ppt for single metals) 70% concentrated nitric acid. Tighten the threaded cap of the PFA container containing the sample and place it on a hot plate. Adjust the hot plate temperature to 100°C. After 2 hours of digestion, turn off the hot plate and allow it to cool naturally. Dilute the concentrated nitric acid to less than 10% and set aside.

[0061] (4) Treatment of control group samples Same as Example 1 (5) Preparation of standard solution Same as Example 1 (6) ICP-MS / MS on-machine testing Same as Example 1 (7) Results analysis Same as Example 1 According to the above specific implementation steps, the specific sample is electronic-grade hexamethyldisilazane (HMDS), a photoresist adhesive used in the photolithography process of chip manufacturing. According to the calculation formula (1), the measured data and the measured sample mass are substituted into the formula to directly calculate the metal ion concentration. The metal ions to be measured in this test are: sodium ion, magnesium ion, aluminum ion, potassium ion, calcium ion, iron ion, copper ion, nickel ion, and zinc ion.

[0062] The results obtained by the above comparative example are shown in Table 5 below.

[0063] Table 5

[0064] As can be seen from the results in Table 5, the method described in the present invention is of great significance for the detection of metal elements in high-purity silicone materials. The spiked recovery rates of the detected elements are between 90% and 110%, and the detection efficiency is increased by 339.2% compared with traditional treatment methods such as room temperature and no pressure.

Claims

1. A method for efficiently capturing and measuring metal ions from high-purity organosilicon materials for chips, characterized in that: The following steps are involved: (1) Construction of capture device Place the PFA container with vents on the heating plate. Collect all the vents of the PFA container into a main pipe. Connect the main pipe to the rear condenser. Connect the condenser to the adsorption device. Connect the adsorption device outlet to the vacuum pump. Vacuum until the pressure in the PFA container reaches -30kPa. Stop. The collection device is now complete. (2) Sample bottle cleaning Heat and boil the PFA container in high-purity nitric acid solution several times until the concentration of each metal ion in the high-purity nitric acid solution is less than 10 ppt; (3) Processing of test samples Place the high-purity organosilicon material sample to be tested into a cleaned PFA container, tighten the screw cap and place it on the heating plate. Open the refrigerant of the condenser tube, start the vacuum pump, adjust the temperature of the heating plate, wait for the sample in the PFA container to completely evaporate, turn off the vacuum, add high-purity nitric acid to the PFA container, turn on the heating plate after adding the acid, set the leaching temperature and time, and leaching the metal ions. After the leaching is completed, wait for the nitric acid solution to cool to room temperature and set aside; (4) ICP-MS on-machine testing After the inductively coupled plasma mass spectrometer is preheated, the sample to be tested prepared in step (3) is injected into the test chamber; The metal ion concentration in the sample to be tested is calculated according to the following formula: 。 2. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, characterized in that: High-purity silicone materials are ≥G4 according to the SEMI grade classification standard, with metal ion impurities ≤0.1ppb.

3. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, characterized in that: High-purity silicone materials that are liquid at room temperature include any of the following: (1) The general structural formula is R 4-n SiX n Wherein: n = 0, 1, 2, 3, R is any one of a C1-C6 straight chain alkane or a C3-C6 branched chain alkane, and X is a halogen or -H; (2) The general structural formula is [(CH3)2SiO] n Where: n = 3, 4, 5; (3) The general structural formula is SiH 4-n (NR1R2) n Aminosilane, wherein n=1, 2, 3, 4, R1 and R2 are any one of C1-C6 straight-chain alkane and C3-C6 branched alkane, and R1 and R2 are the same or different.

4. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 2 or 3, characterized in that: The high-purity silicone material includes any one of monomethyltrichlorosilane, dimethyldichlorosilane, trimethylmonochlorosilane, tetramethylsilane, octamethylcyclotetrasiloxane, bis(tert-butylamino)silane, bis(dihexylamino)silane, bis(dimethylamino)dimethylsilane, tris(dimethylamino)silane, diisopropylaminesilane, hexamethyldisilazane, diethoxymethylsilane, dimethyldimethoxysilane, and tetraethoxysilane.

5. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, wherein: In the step (1) shown, the condensation temperature of the two-stage condensation device is 5-10°C, and the filling material in the adsorption device is activated carbon.

6. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, characterized in that: In step (2), the volume of the PFA container is 30-200 ml, the concentration of high-purity nitric acid is 2%-55%, and the single metal concentration is less than 10 ppt.

7. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, characterized in that: In step (3), the amount of sample to be processed is 20 g to 50 g, the temperature of the heating plate is 20 to 85° C., and the vacuum degree is -90 to -100 kPa.

8. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, characterized in that: The concentration of high-purity nitric acid added in step (3) is 2%-10%, and the single metal concentration is less than 10 ppt.

9. The method for efficiently capturing and determining metal ions in organosilicon materials according to claim 1, wherein: The extraction temperature is 40-80°C, and the extraction time is 30min-60min.

10. The method for efficiently capturing and determining metal ions in high-purity organosilicon materials according to claim 1, characterized in that: The working conditions of the inductively coupled plasma mass spectrometer in step (4) are as follows: high frequency power of 0.5-1.5 kW, sampling depth of 5.0-10 mm, nebulizing gas flow rate of 0.5-0.7 L / min, and compensation gas flow rate of 0.4-0.9 L / min.

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