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Method for detecting fluoroboric acid in mixed acid

A technology of fluoroboric acid and detection method, which is applied in the measurement of color/spectral properties, chemical analysis by titration, and electrochemical variables of materials, etc. , Improve the detection accuracy, the operation method is simple and fast

Active Publication Date: 2021-04-27
湖北兴福电子材料股份有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] Fluoboric acid is mainly used in combination with other acids. The detection of fluoboric acid in mixed acids has always been a difficult point, because the ionization energy of boron is high, so ICP-MS and other trace analysis instruments that require atom ionization cannot detect; and fluoboric acid in aqueous solution It will slowly decompose in HF to generate hydroxyfluoroboric acid (HBF3OH) and HF. Therefore, when using the BF4-ion selective electrode method for direct detection, the error is large due to the influence of temperature, ionic strength, hydrolysis, etc., and the detection deviation is even more than 20%. Therefore, it is necessary to Exploring a convenient method for detecting the content of fluoboric acid in mixed acid
[0004] In addition to the direct detection method, the content of fluoboric acid can also be indirectly calculated by measuring the content of other components in the mixed acid. When fluoboric acid is used in combination with phosphoric acid, nitric acid, and acetic acid, the detection of phosphoric acid content generally adopts gravimetric and volumetric methods. Among them, the gravimetric method uses quinoline phosphomolybdic acid precipitation to calculate the content of phosphoric acid. The steps are cumbersome, and there are many precautions. In addition, the temperature required in the drying stage is high, and the safety risk is greater; compared with the gravimetric method, the volumetric method has more requirements for temperature control. It is not so harsh, but there are also multiple filtration and washing operations, and the step of alkali dissolution precipitation is also quite inconvenient

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  • Method for detecting fluoroboric acid in mixed acid
  • Method for detecting fluoroboric acid in mixed acid

Examples

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Embodiment 1

[0034] In this example, phosphoric acid is separated from nitric acid, acetic acid, and fluoboric acid by means of extraction, and the content of phosphoric acid is independently titrated, and then the content of nitric acid is tested by photometry. boric acid content. details as follows:

[0035] First take the mixed acid whose production formula contains 5.05% fluoboric acid, 70.1% phosphoric acid, 3.0% nitric acid, and 8.5% acetic acid, weigh 10g in a plastic separatory funnel, add 50ml of sodium chloride solution with a concentration of 150g / L, and add 10g of acetic acid Ethyl ester, discard the organic phase after vibrating and layering, extract like this 5 times, completely separate phosphoric acid from other mixed acid components, then transfer the water phase into a plastic beaker, use a titrator to titrate the phosphoric acid content in the water phase, and calculate the phosphoric acid content as W P =70.38%. Utilize photometry again, take by weighing 0.5g mixed ac...

Embodiment 2

[0041]Same as Example 1, only when the concentration of sodium chloride solution is adjusted to 200g / L during extraction, it is set to Example 2. The phosphoric acid content measured after the first step of extraction is W P =70.21%, the second step measures the nitric acid content W N =3.0%, the third step titration volume V=4.1006ml, according to the formula in the embodiment 1, calculate the content of fluoboric acid W B .

[0042] As shown in Table 1, the present embodiment uses butyl acetate as the extraction agent, the concentration of the diluent sodium chloride solution is increased to 200g / L, and the detection error of the phosphoric acid content is further reduced. Lower than Example 1.

Embodiment 3

[0044] Same as Example 1, only when the concentration of sodium chloride solution is adjusted to 250g / L during extraction, it is set as Example 3. The phosphoric acid content measured after the first step of extraction is W P =70.33%, the second step records the nitric acid content W N =3.0%, the third step titration volume V=4.1001ml, according to the formula in the embodiment 1, calculate the content of fluoboric acid W B .

[0045] As shown in Table 1, the present embodiment uses butyl acetate as the extraction agent, the concentration of the diluent sodium chloride solution is increased to 250g / L, and the detection error of the phosphoric acid content is relatively low. Low with embodiment 1, but higher than embodiment 2, the preferred concentration of sodium chloride solution is 200g / L.

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Abstract

The invention relates to a method for detecting fluoroboric acid in mixed acid. In the invention, the mixed acid is a mixture of phosphoric acid, nitric acid, acetic acid and fluoboric acid. The method comprises the following steps of separating other components except phosphoric acid in the mixed acid by using an extracting agent in a multi-extraction mode, and independently measuring the content of phosphoric acid; and detecting the content of nitric acid in the mixed acid by a photometric method, calculating the total content of phosphoric acid, nitric acid and fluoboric acid at the equivalent point by using a potentiometric titrator, and subtracting the components of phosphoric acid and nitric acid to obtain the content of fluoboric acid. According to the method, the content of fluoroboric acid is indirectly determined, the error of directly determining the content of fluoroboric acid by using an ion selective electrode is reduced, the content of phosphoric acid in the mixed acid system is accurately determined in an extraction separation manner, and the error of determining the content of phosphoric acid by using a gravimetric method or a volumetric method is avoided; and detection precision of fluoroboric acid in the mixed acid system is greatly improved.

Description

technical field [0001] The invention relates to detection in the fields of electronic chemicals and semiconductor wet etching, in particular to a detection method for fluoboric acid in mixed acids, which accurately detects the content of fluoboric acid components. Background technique [0002] Wet etching is one of the mainstream etching techniques in semiconductors at present. The etchant used in wet etching is usually acid-based and contains fluorine, because fluorine easily reacts with silicon. Fluoroboric acid is generally used as a cleaning and corrosive agent for oxides and silicate films on metal surfaces, and because of the characteristics of hydrolyzing HF, it can also be used as a slow-release carrier for HF, and its content has a great impact on the performance of etching solution products . [0003] Fluoboric acid is mainly used in combination with other acids. The detection of fluoboric acid in mixed acids has always been a difficult point, because the ionizat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16G01N21/31G01N27/44
CPCG01N31/16G01N21/31G01N27/44
Inventor 尹印徐子豪李鑫贺兆波张庭万杨阳冯凯王书萍倪高国
Owner 湖北兴福电子材料股份有限公司
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