Gas chromatography content determination method for tetra (dimethylamino) titanium

Abstract

The invention relates to a gas chromatography content determination method of tetra (dimethylamino) titanium, which adopts a gas chromatography method for detection, the method has simple steps and is convenient to operate, the content of tetra (dimethylamino) titanium in a sample to be detected can be rapidly and accurately determined by adopting the gas chromatography method, and the content of tetra (dimethylamino) titanium in the sample to be detected can be accurately determined by selecting a specific chromatographic column type according to the specific method. According to the present invention, the rapid and efficient detection of the tetrakis (dimethylamino) titanium is achieved through the detection of the tetrakis (dimethylamino) titanium and the limitation of the chromatographic instrument condition parameters, and compared with the nuclear magnetic hydrogen spectrum method in the prior art, the analysis speed is rapid, the operation is simple, the result is accurate, the detection cost is low, the refrigerant and the high pollution solvent are not required, and the production and the purification work of the tetrakis (dimethylamino) titanium can be rapidly guided.

Description

Technical Field

[0001] The invention belongs to the technical field of compound content analysis and determination, in particular to a gas chromatography content analysis and determination method for tetrakis(dimethylamino)titanium. Background Art

[0002] With the continuous development of the semiconductor manufacturing industry, ALD (atomic layer deposition) technology has become one of the most ideal deposition methods in the semiconductor manufacturing process due to its simple operation, highly controllable deposition parameters, and excellent deposition uniformity. Tetrakis(dimethylamino)titanium is a precursor material for high-k and metal gate materials suitable for ALD. It can form thin films such as TiN, TiSiN, TiALN, TiO2, etc. through deposition, and has good conductivity, chemical stability and diffusion barrier properties. When tetrakis(dimethylamino)titanium is used as a precursor material, its own purity is crucial because: other impurity components contained in the composition of tetrakis(dimethylamino)titanium products will directly affect the uniformity and conductivity of the deposited film.

[0003] At present, the accurate detection of the purity of metal organic precursor materials in the prior art has always been a difficult problem in the industry. At present, the main method for detecting the purity of tetrakis(dimethylamino)titanium is nuclear magnetic resonance hydrogen spectroscopy. For example, patent CN115073514B, a new preparation method of tetrakis(dimethylamino)titanium, mentioned that the purity of tetrakis(dimethylamino)titanium was quantitatively tested using the nuclear magnetic resonance spectrometer NMR hydrogen spectrum area normalization method.

[0004] Patent CN103193818A discloses a method for synthesizing tetrakis(dimethylamino)titanium. The yield of synthesizing tetrakis(dimethylamino)titanium is 73%, which is determined by nuclear magnetic hydrogen spectrum.

[0005] However, the current nuclear magnetic resonance hydrogen spectroscopy method has the following significant defects when performing purity analysis of tetrakis(dimethylamino)titanium: the nuclear magnetic resonance spectrometer used in the method is expensive, is mainly used for molecular structure characterization of compounds, has low accuracy in purity quantitative analysis, and the quantitative operation is complicated. The use of solvents pollutes the environment, and the subsequent maintenance costs are high, which cannot meet the requirements for rapid and accurate testing of the content of tetrakis(dimethylamino)titanium.

[0006] Gas chromatography is a chromatographic technique used in organic chemistry to separate and analyze compounds that are easily volatile and do not decompose. Typical uses of gas chromatography include testing the purity of a particular compound and separating the components in a mixture (and also determining the relative content of each component). Therefore, gas chromatography is usually used in the prior art to determine the purity of some compounds.

[0007] However, due to the active nature of tetrakis(dimethylamino)titanium, it is easily hydrolyzed and decomposed after contact with air. At the same time, it is easy to react with the fillers and coatings in conventional chromatographic columns, resulting in low separation efficiency when tetrakis(dimethylamino)titanium is subjected to gas chromatography analysis, irregular chromatographic peaks are formed, and the test data cannot be used. Invention Technology

[0008] The technical purpose of the present invention is to provide a gas chromatography content determination method of tetrakis(dimethylamino)titanium with fast analysis speed, high accuracy, low detection cost and good environmental protection through the type of chromatographic column and the setting of chromatographic condition parameters, so as to overcome the problems of complex testing process, poor accuracy, high cost and environmental pollution in the prior art.

[0009] To achieve the above object, the present invention adopts the following technical scheme: a method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography, which adopts gas chromatography for detection, and the specific steps are: Step 1: In an inert atmosphere glove box, tetrakis(dimethylamino)titanium with a mass concentration of not less than 99.9% is diluted with a solvent, n-hexane, to prepare a tetrakis(dimethylamino)titanium sample with a known concentration as a standard; Step 2: In an inert atmosphere glove box, use a sampling needle to draw the standard product prepared in step 1 and inject it into the injection port of the gas chromatograph, and inject 4-7 times continuously. Under the action of the inert carrier gas, the sample is separated by a weak polar chromatographic column and then enters the FID detector for detection to obtain a gas chromatogram of the standard product; The injection port temperature of the gas chromatograph was 200-280°C, the split ratio was 30:1, the weak polarity chromatographic column used was an HP-5 chromatographic column with a specification of 30m*320μm*0.25μm, the column flow rate was 3-5mL / min, and the flow rate was constant. The column box temperature was 120°C, maintained for 2 minutes, and then heated to 280°C at a heating rate of 20°C / min and maintained for 4 minutes. Step 3: Analyze the gas chromatogram of the standard product obtained in step 2 by using the area normalization method, calculate the correction factor, and input the correction factor into the calibration table of the gas chromatograph; Step 4: In an inert atmosphere glove box, transfer the tetrakis(dimethylamino)titanium sample to be tested into a sample bottle as a sample to be tested; Step 5, repeat the operation of step 2, and replace the standard prepared in step 1 sucked by the injection needle with the sample to be tested prepared in step 4, and finally obtain a gas chromatogram of the sample to be tested; Step 6: Use the correction factor area normalization method to quantify the gas chromatogram of the sample to be tested obtained in step 5, so as to calculate the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested.

[0010] Furthermore, in step 1, step 2 and step 4, the inert atmosphere glove box needs to maintain O2<0.01ppm and H2O<0.01ppm.

[0011] Furthermore, in step 2 and step 5, the injection needle is a 10 μL injection needle with a minimum scale of 0.2 μL.

[0012] Furthermore, in step 2 and step 5, the injection process must be completed within 30 seconds.

[0013] Furthermore, in step 2 and step 5, the injection operation needs to be performed after the gas chromatograph is stabilized, and the injection needle needs to be purged with an inert gas before each use to dry the inside and outside of the injection needle, and the inert carrier gas is helium.

[0014] Furthermore, in step 2 and step 5, during the continuous injection operation, the injection volume for each injection is 0.4-0.8 μL.

[0015] Furthermore, in step 2 and step 5, the temperature of the FID detector is 300° C., air: 400 mL / min, hydrogen: 30 mL / mmin, tail blowing: 20 mL / min.

[0016] Furthermore, in step three, the sample bottle is a 2 mL quartz bottle with a corrosion-resistant bottle cap.

[0017] Furthermore, in step 3, the specific operation of calculating the correction factor using the area normalization method is: In the gas chromatogram of the standard product obtained in step 2, select two peak areas with deviations within 1% and integrate them to obtain the integral area A of n-hexane. 正己烷 , the integral area A of tetrakis(dimethylamino)titanium in the standard 标 , the n-hexane correction factor f is calculated by formula (1) and formula (2): 正己烷 and tetrakis(dimethylamino)titanium correction factor f 标 ; In the formula, f 正己烷 is the correction factor for n-hexane; C 正己烷 A is the mass percentage concentration of n-hexane in the standard; 正己烷 is the integrated area of ​​n-hexane in the standard; f 标 is the correction factor for tetrakis(dimethylamino)titanium; C 标 A is the mass percentage concentration of tetrakis(dimethylamino)titanium in the standard; 标 is the integrated area of ​​tetrakis(dimethylamino)titanium in the standard.

[0018] Furthermore, in step six, the specific operation of using the correction factor area normalization method for quantification is as follows: In the gas chromatogram of the sample to be tested obtained in step 5, select two peak areas with a deviation within 1% for integration to obtain the integrated area A of tetrakis(dimethylamino)titanium in the sample to be tested. i , the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested can be calculated by formula (3); Wherein, χ% is the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested; A i is the integrated area of ​​tetrakis(dimethylamino)titanium in the sample to be tested.

[0019] Beneficial effects of the present invention: (1) The present invention provides a method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography, which has simple steps and is easy to operate. The gas chromatography method can be used to quickly and accurately determine the content of tetrakis(dimethylamino)titanium in the sample to be detected. The method itself achieves rapid and efficient detection of tetrakis(dimethylamino)titanium by selecting a specific type of chromatographic column and limiting the chromatograph condition parameters. Compared with the nuclear magnetic hydrogen spectroscopy method in the prior art, the method has a fast analysis speed, simple operation, accurate results, low detection cost, and does not require refrigerants and highly polluting solvents, and can quickly guide the production and purification of tetrakis(dimethylamino)titanium.

[0020] (2) The gas chromatography content determination method of tetrakis(dimethylamino)titanium of the present invention creatively selects gas chromatography to determine the content of tetrakis(dimethylamino)titanium in the sample in view of the technical shortcomings of the prior art, such as complex testing process, poor accuracy, high detection cost and serious environmental pollution. Due to the active nature of tetrakis(dimethylamino)titanium in the sample to be tested, it is easily hydrolyzed and decomposed when exposed to air, and it is easy to react with the filler and coating in the chromatographic column, resulting in decreased separation efficiency and irregular chromatographic peaks. The present application adopts specific process fine control and condition parameter definition. Among them, the injection port temperature of 200-280°C can effectively ensure that the tetrakis(dimethylamino)titanium in the injected product is fully vaporized and not decomposed, and the flow rate of 3-5mL / min of the chromatographic column also ensures the effective separation between different compounds in the sample. The effective definition of these parameters is the key to achieving the technical purpose of the present application.

[0021] (3) A gas chromatography content determination method of tetrakis(dimethylamino)titanium of the present invention sets the injection port temperature to 200-280°C, ensuring uniform gasification of the sample. An injection port temperature higher than 280°C will cause tetrakis(dimethylamino)titanium to decompose into dimethylamine, and a temperature lower than 200°C will not allow the sample to be fully gasified. The flow rate of the chromatographic column is limited to 3-5 mL / min. If the flow rate of the chromatographic column is set to a conventional 1 mL / min or so, the chromatographic peak will be tailed and irregular in shape. The unique selection of a high column flow rate of 3-5 mL / min is conducive to promoting the smooth removal of tetrakis(dimethylamino)titanium from the chromatographic column without causing tailing and deformation of the chromatographic peak. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The gas chromatogram of 70.68% tetrakis(dimethylamino)titanium standard in Example 1;

[0023] Figure 2 This is the gas chromatogram of the 78.41% tetrakis(dimethylamino)titanium sample to be tested in Example 1. DETAILED DESCRIPTION

[0024] In order to enable those skilled in the art to better understand and implement the technical solution of the present invention, the present invention is further described below in conjunction with specific examples and data, but the examples are not intended to limit the present invention.

[0025] The experimental methods and detection methods described in the following embodiments are conventional methods unless otherwise specified; the reagents and materials are commercially available unless otherwise specified.

[0026] A method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography is provided, which aims to solve the problem that the nuclear magnetic resonance hydrogen spectrum method in the prior art is complicated and inaccurate. To solve this problem, a method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography of the present invention specifically comprises the following steps: 1. Transfer tetrakis(dimethylamino)titanium to a 2 mL sample vial in an inert atmosphere glove box, purge a 10 μL syringe with high-purity nitrogen, and keep the syringe dry.

[0027] The inert atmosphere glove box maintains an environment of O2<0.01ppm and H2O<0.01ppm, the 2mL sample bottle is a quartz bottle with a corrosion-resistant bottle cap, and the 10μL injection needle is a special injection needle with a minimum scale of 0.2μL.

[0028] 2. Rapidly inject the sample into the inlet of the gas chromatograph. After separation by the weak polarity chromatographic column under the action of the carrier gas, it enters the chromatographic detector for detection to obtain a gas chromatogram.

[0029] Among them, the chromatograph parameters are as follows: the inlet is a split / splitless inlet, the inlet temperature is: 200-280°C, the split ratio is: 30:1, the sample volume is: 0.4-0.8μL, the column box temperature is: 120°C, keep for 2min, increase the temperature to 280°C at 20°C / min, and keep for 4min; the carrier gas is helium; the chromatographic column is: HP-530m*320μm*0.25μm, the column flow rate is: 3-5mL / min, constant flow rate; the detector is a FID detector, the detector temperature: 300°C, air: 400mL / min, hydrogen: 30mL / mmin, tail blowing: 20mL / min.

[0030] 3. Quantitative analysis was performed using the correction factor area normalization method to calculate the mass percentage of tetrakis(dimethylamino)titanium in the sample.

[0031] The specific steps of the correction factor area normalization method are as follows: 99.9% pure tetrakis(dimethylamino)titanium is diluted with n-hexane solvent to a certain proportion of standard product, and after the instrument is stable, 0.4 μL of standard product is injected into the injection port of the gas chromatograph each time, and the injection is continuous for 4-7 times, and the peak areas with deviations within 1% are selected for integration, and the integral area A of n-hexane is calculated. 正己烷 , the integral area A of tetrakis(dimethylamino)titanium in the standard 标 , the n-hexane correction factor f is calculated by the formula 正己烷 and tetrakis(dimethylamino)titanium correction factor f 标 ; and input the correction factor into the calibration table of the gas chromatograph; Then, in an inert atmosphere glove box, use a sampling needle to draw the sample to be tested. After the instrument is stable, inject 0.4 μL of the sample to be tested into the injection port of the gas chromatograph each time. Inject 4-7 times continuously, select 2 peak areas with a deviation within 1% for integration, and obtain the integrated area A of tetrakis(dimethylamino)titanium in the sample to be tested. i , and then calculate the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested through the formula.

[0032] The calculation formula is as follows: Among them, f 正己烷 is the n-hexane correction factor; C 正己烷 is the mass percentage concentration of n-hexane in the standard; A 正己烷 is the integrated area of ​​n-hexane in the standard; f 标 is the tetrakis(dimethylamino)titanium correction factor; C 标 is the mass percentage concentration of tetrakis(dimethylamino)titanium in the standard; A 标 is the integrated area of ​​tetrakis(dimethylamino)titanium in the standard; χ% is the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested; A i is the integrated area of ​​tetrakis(dimethylamino)titanium in the sample to be tested.

[0033] A gas chromatography content determination method of tetrakis(dimethylamino)titanium of the present invention comprises the following steps: taking the tetrakis(dimethylamino)titanium product to be tested into a sample bottle in an anhydrous and oxygen-free glove box, using a micro-syringe to accurately and quickly transfer the sample and inject it into a gas chromatograph, separating it through a weak polarity chromatographic column, detecting it using an FID detector, and finally using a correction factor normalization method to quantitatively calculate the tetrakis(dimethylamino)titanium. In the technical scheme of the present invention, the flow rate of the chromatographic column plays a key role in the separation of the sample, and the temperature setting of the chromatograph injection port is also very important. If the injection port temperature is too low, the sample cannot be gasified, and if the injection port temperature is set too high, the sample will decompose. Selecting a suitable chromatographic column and setting suitable gas chromatography parameters are the key points of the present application. The detection method of the present invention has fast analysis speed, simple operation, accurate results, low detection cost, does not require refrigerants and highly polluted solvents, and can quickly guide the production and purification of tetrakis(dimethylamino)titanium.

[0034] Embodiment 1: A method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography specifically comprises the following steps: 1) Device status: Ready The instrument used was GC-7890A, and the prepared method of tetrakis(dimethylamino)titanium was called up. The equipment status reached the following parameters to be ready: injection port temperature 250℃, split ratio: 30:1. Chromatographic column: HP-530m*320μm*0.25μm, flow rate: 3mL / min, constant flow rate. Column box parameters: initial temperature 120℃, hold for 2min, increase the temperature to 280℃ at 20℃ / min, hold for 4min. FID detector, detector temperature: 300℃, air: 400mL / min, hydrogen: 30mL / mmin, tail blowing: 20mL / min.

[0035] 2) Sample preparation The O2<0.01ppm and H2O<0.01ppm contents in the glove box meet the requirements. Transfer the sample to a 2mL quartz bottle in the glove box and tighten the cap.

[0036] 3) Standard sample preparation A certain amount of 99.9% tetrakis(dimethylamino)titanium standard was transferred into the glove box, and diluted with n-hexane solvent to prepare a tetrakis(dimethylamino)titanium solution with a mass percentage concentration of 70.68%.

[0037] 4) Sampling and calculation Use a dry injection needle to transfer 0.4 μL of 70.68% tetrakis(dimethylamino)titanium solution and quickly inject it into the injection port. Inject 5 times in succession. After the target peak is stable, select 2 peak areas with a deviation within 1% for integration to obtain the integral area A of n-hexane. 正己烷 , the integral area A of tetrakis(dimethylamino)titanium in the standard 标 , the n-hexane correction factor f is calculated by formula (1) and formula (2): 正己烷 and tetrakis(dimethylamino)titanium correction factor f 标 .

[0038] In the formula, f 正己烷 is the correction factor for n-hexane; C 正己烷 A is the mass percentage concentration of n-hexane in the standard; 正己烷 is the integrated area of ​​n-hexane in the standard; f 标 is the correction factor for tetrakis(dimethylamino)titanium; C 标 A is the mass percentage concentration of tetrakis(dimethylamino)titanium in the standard; 标 is the integrated area of ​​tetrakis(dimethylamino)titanium in the standard. The gas chromatogram of the standard is shown in the attached figure. Figure 1 shown.

[0039] Use a dry injection needle to transfer 0.4 μL of the sample to be tested and quickly inject it into the injection port. Inject the sample 5 times continuously. After the target peak is stable, select 2 peak areas with a deviation within 1% for integration to obtain the integrated area A of tetrakis(dimethylamino)titanium in the sample to be tested. i , the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested can be calculated by formula (3); Wherein, χ% is the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested; A i is the integrated area of ​​tetrakis(dimethylamino)titanium in the sample to be tested.

[0040] The mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested in this embodiment is calculated to be 78.41%. The gas chromatogram of the sample to be tested is shown in the attached figure. Figure 2 shown.

[0041] exist Figure 1 and Figure 2 In the figure, A represents n-hexane, and B represents tetrakis(dimethylamino)titanium. The data and calculation results are shown in Table 1 below.

[0042] Table 1 Tetrakis(dimethylamino)titanium calibration

[0043] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been described as a preferred embodiment as above, it is not used to limit the present invention. Any technician familiar with the profession can make some changes or modifications to the above-mentioned technical contents without departing from the scope of the technical solution of the present invention, which are equivalent embodiments of equivalent changes. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A gas chromatography content determination method of tetrakis(dimethylamino)titanium, characterized in that: Gas chromatography was used for detection, and the specific steps were as follows: Step 1: In an inert atmosphere glove box, tetrakis(dimethylamino)titanium with a mass concentration of not less than 99.9% is diluted with a solvent, n-hexane, to prepare a tetrakis(dimethylamino)titanium sample with a known concentration as a standard; Step 2: In an inert atmosphere glove box, use a sampling needle to draw the standard product prepared in step 1 and inject it into the injection port of the gas chromatograph, and inject 4-7 times continuously. Under the action of the inert carrier gas, the sample is separated by a weak polar chromatographic column and then enters the FID detector for detection to obtain a gas chromatogram of the standard product; The injection port temperature of the gas chromatograph was 200-280°C, the split ratio was 30:1, the weak polarity chromatographic column used was an HP-5 chromatographic column with a specification of 30m*320μm*0.25μm, the column flow rate was 3-5mL / min, and the flow rate was constant. The column box temperature was 120°C, maintained for 2 minutes, and then heated to 280°C at a heating rate of 20°C / min and maintained for 4 minutes. Step 3: Analyze the gas chromatogram of the standard product obtained in step 2 by using the area normalization method, calculate the correction factor, and input the correction factor into the calibration table of the gas chromatograph; Step 4: In an inert atmosphere glove box, transfer the tetrakis(dimethylamino)titanium sample to be tested into a sample bottle as a sample to be tested; Step 5, repeat the operation of step 2, and replace the standard prepared in step 1 sucked by the injection needle with the sample to be tested prepared in step 4, and finally obtain a gas chromatogram of the sample to be tested; Step 6: Use the correction factor area normalization method to quantify the gas chromatogram of the sample to be tested obtained in step 5, so as to calculate the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested.

2. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 1, step 2 and step 4, the inert atmosphere glove box needs to maintain O2<0.01ppm and H2O<0.01ppm.

3. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 2 and step 5, the injection needle is a 10 μL injection needle with a minimum scale of 0.2 μL.

4. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 2 and step 5, the injection process must be completed within 30 seconds.

5. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 2 and step 5, the injection operation needs to be performed after the gas chromatograph is stabilized, and the injection needle needs to be purged with an inert gas before each use to dry the inside and outside of the injection needle. The inert carrier gas is helium.

6. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 2 and step 5, during the continuous injection operation, the injection volume for each injection is 0.4 to 0.8 μL.

7. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 2 and step 5, the temperature of the FID detector is 300° C., air: 400 mL / min, hydrogen: 30 mL / mmin, tail blowing: 20 mL / min.

8. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step three, the sample bottle is a 2 mL quartz bottle with a corrosion-resistant bottle cap.

9. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 1, characterized in that: In step 3, the specific operation of calculating the correction factor using the area normalization method is: In the gas chromatogram of the standard product obtained in step 2, select two peak areas with deviations within 1% and integrate them to obtain the integral area A of n-hexane. 正己烷 , the integral area A of tetrakis(dimethylamino)titanium in the standard 标 , the n-hexane correction factor f is calculated by formula (1) and formula (2): 正己烷 and tetrakis(dimethylamino)titanium correction factor f 标 ; In the formula, f 正己烷 is the correction factor for n-hexane; C 正己烷 A is the mass percentage concentration of n-hexane in the standard; 正己烷 is the integrated area of ​​n-hexane in the standard; f 标 is the correction factor for tetrakis(dimethylamino)titanium; C 标 A is the mass percentage concentration of tetrakis(dimethylamino)titanium in the standard; 标 is the integrated area of ​​tetrakis(dimethylamino)titanium in the standard.

10. The method for determining the content of tetrakis(dimethylamino)titanium by gas chromatography according to claim 9, characterized in that: In step six, the specific operation of using the correction factor area normalization method for quantification is as follows: In the gas chromatogram of the sample to be tested obtained in step 5, select two peak areas with a deviation within 1% for integration to obtain the integrated area A of tetrakis(dimethylamino)titanium in the sample to be tested. i , the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested can be calculated by formula (3); Wherein, χ% is the mass percentage of tetrakis(dimethylamino)titanium in the sample to be tested; A i is the integrated area of ​​tetrakis(dimethylamino)titanium in the sample to be tested.

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