CN112710777B - Method for detecting fluoboric acid in mixed acid - Google Patents
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Abstract
The invention relates to a method for detecting fluoboric acid in mixed acid. In the invention, the mixed acid is a mixture of phosphoric acid, nitric acid, acetic acid and fluoboric acid. Firstly, separating other components except phosphoric acid in the mixed acid by using an extracting agent through a mode of multiple extraction, and separately measuring the content of the phosphoric acid; and detecting the content of nitric acid in the mixed acid by a photometric method, calculating the total content of the phosphoric acid, the nitric acid and the fluoroboric acid at the equivalent point by using a potentiometric titrator, and subtracting the components of the phosphoric acid and the nitric acid to obtain the content of the fluoroboric acid. The method indirectly measures the content of the fluoroboric acid, reduces the error of directly measuring the content of the fluoroboric acid by using the ion selective electrode, accurately measures the content of the phosphoric acid in the mixed acid system in an extraction and separation mode, avoids the error of measuring the content of the phosphoric acid by adopting a gravimetric method or a volumetric method, and greatly improves the detection precision of the fluoroboric acid in the mixed acid system.
Description
Technical Field
The invention relates to detection in the field of electronic chemicals and semiconductor wet etching, in particular to a method for detecting fluoboric acid in mixed acid, which can accurately detect the content of a fluoboric acid component.
Background
Wet etching is one of the mainstream etching techniques in semiconductors at present. The etching solution used in wet etching is usually mainly acid and contains fluorine, because fluorine is easily reacted with silicon. The fluoboric acid is generally used for cleaning and corroding agents of metal surface oxides and silicate films, and can also be used as an HF slow release carrier due to the characteristic of hydrolyzing HF, and the content of the fluoboric acid has great influence on the performance of an etching solution product.
The fluoboric acid is mainly compounded with other acids for use, and the detection of the fluoboric acid in mixed acid is always a difficult point, because the ionization energy of boron element is high, so trace analysis instruments such as ICP-MS and the like which need atomic ionization can not detect; and the fluoroboric acid can be slowly decomposed in the aqueous solution to generate hydroxyl fluoroboric acid (HBF3OH) and HF, so that when the BF 4-ion selective electrode method is used for directly detecting, the detection error is large under the influence of temperature, ionic strength, hydrolysis and the like, and the detection deviation is even more than 20%, so that a method for conveniently detecting the content of the fluoroboric acid in the mixed acid needs to be explored.
Except a direct detection method, the content of the fluoboric acid can also be indirectly calculated by measuring the content of other components in the mixed acid, when the fluoboric acid is compounded with phosphoric acid, nitric acid and acetic acid for use, a gravimetric method and a volumetric method are generally adopted for detecting the content of the phosphoric acid, wherein the gravimetric method uses quinoline phosphomolybdate precipitation to calculate the content of the phosphoric acid, the steps are complicated, the attention points are various, the temperature required to be used in the drying stage is high, and the safety risk is high; the volumetric method is less critical in temperature control than the gravimetric method, but has the operation of multiple filtration and washing, and the operation of the alkaline precipitation step is also quite inconvenient.
Based on the method, the phosphoric acid and other components are separated in a multi-extraction mode aiming at the mixed acid system of phosphoric acid, nitric acid, acetic acid and fluoroboric acid, so that the content of the phosphoric acid in the mixed acid system can be accurately measured, and meanwhile, the content of the fluoroboric acid is calculated by utilizing a photometric method and a potentiometric titration method, so that the precision of detecting the content of the fluoroboric acid in the mixed acid system is greatly improved.
Disclosure of Invention
The invention indirectly measures the contents of phosphoric acid, nitric acid and acetic acid by measuring the contents of total acid and other mixed acidsThe content of the fluoboric acid in the fluoboric acid mixed acid system avoids adopting BF4 -The ion selective electrode directly measures the error of the content of the fluoboric acid; through the mode of extracting for many times by the extractant, separate other components except phosphoric acid in the mixed acid, the content of phosphoric acid in the mixed acid system is accurately determined, the error of determining the content of phosphoric acid by adopting a gravimetric method or a volumetric method is avoided, and the detection precision of the fluoboric acid in the mixed acid system is greatly improved.
The invention aims to provide a method for detecting fluoboric acid in mixed acid.
In order to achieve the above object, the technical solution of the present invention provides a method for detecting fluoride ions in mixed acid, comprising the steps of:
s1, weighing a certain amount of mixed acid sample, separating a phosphoric acid component in the mixed acid by using an extracting agent, and determining the content of phosphoric acid by a titration method;
s1, weighing a certain amount of mixed acid sample, and determining the content of a nitric acid component by a photometric method;
s2, weighing a certain amount of mixed acid sample, titrating the sample by using a potentiometric titrator, calculating the total content of the phosphoric acid, the nitric acid and the fluoroboric acid through a first equivalence point, and subtracting the content of the phosphoric acid and the nitric acid determined by S1 and S2 to obtain the content of the fluoroboric acid.
In the detection method, the mixed acid sample in the step S1 is a mixture of phosphoric acid, nitric acid, acetic acid and fluoroboric acid, and the mixed acid sample is diluted by adding NaCl solution with the concentration of 150-250 g/L. According to the preferable scheme, 9-11 g of mixed acid sample is diluted in 50ml of 200g/L NaCl solution to enhance the polarity and improve the extraction efficiency, so that the solution is layered conveniently.
In the detection method, the extractant in the step S1 is ethyl acetate, butyl acetate or chloroform, the mass of the extractant is 9-11 g, and the extraction times are not less than 5.
In the detection method, in step S2, an absorbance standard curve of nitric acid needs to be drawn first, and then the nitric acid content is calculated by using the absorbance of the sample.
In the detection method, in step S3, the mass of a sample is about 0.4500-0.5500 g, the titration solution is NaOH solution with the concentration of about 1mol/L, an equivalence point is set by a potentiometric titrator, and the volume of the titration solution consumed by the equivalence point is recorded.
In the detection method, when the equivalent point appears in the step S3, all H + of one H +, nitric acid and fluoroboric acid ionized by phosphoric acid is consumed, and the H + amount of the fluoroboric acid and the content of the fluoroboric acid can be calculated through the contents of the phosphoric acid and the nitric acid detected in the steps S1 and S2.
The invention has the advantages of
(1) The content of the fluoboric acid in a phosphoric acid, nitric acid, acetic acid and fluoboric acid mixed acid system is indirectly measured by measuring the content of total acid and the content of other mixed acid, thereby avoiding the error of directly measuring the content of the fluoboric acid by adopting a BF 4-ion selective electrode;
(2) through the mode of extracting the extractant for multiple times, other components except the phosphoric acid in the mixed acid are separated, the content of the phosphoric acid in the mixed acid system is accurately determined, the error of determining the content of the phosphoric acid by adopting a gravimetric method or a volumetric method is avoided, and the detection precision of the fluoboric acid in the mixed acid system is greatly improved;
(3) the method is simple and rapid in operation, can be used for simultaneously measuring multiple batches of samples compared with the ion chromatography, is suitable for detecting production samples, and avoids the corrosion of the fluoboric acid to the chromatographic column.
Drawings
FIG. 1 is a standard curve made using a fluoroboric acid solution.
FIG. 2 is a nitric acid absorbance standard curve plotted using a nitric acid solution.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Comparative example 1
This comparative example utilizes BF in accordance with a method of directly measuring the content of fluoroboric acid4 -The ion selective electrode tests the concentration value of the fluoboric acid in the mixed acid at room temperature, compares the concentration value with the theoretical prepared concentration value, and calculates the deviation rate (the difference value between the prepared concentration and the tested concentration in the prepared concentrationProportion of (d). The method comprises the following specific steps:
firstly, preparing a series of fluoroboric acid aqueous solutions with concentration gradients; then, 0.5g of each of the above-mentioned samples was weighed into a 100mL volumetric flask, and pH and ionic strength were adjusted according to the relevant standards at room temperature. Finally, testing the corresponding potential value and drawing BF4 -Standard curve of concentration versus potential.
Taking a mixed acid sample with the production formula of 3.05 percent of fluoboric acid concentration, weighing 0.4g of mixed acid sample, adding the mixed acid sample into a 100mL volumetric flask, adjusting the pH and the ionic strength according to relevant standards at room temperature, and testing a corresponding potential value. And calculating the concentration of the tested fluoboric acid according to the standard curve.
The above standard curve is shown in FIG. 1, and it can be seen that the correlation coefficient is close to 1, which indicates that the method has good capability of quantitative detection of free BF 4-ion, but BF in actual samples4 -The hydrolysis of (2) resulted in a deviation of the detection results, which is shown in Table 1.
Comparative example 2
The content of the total acid and the content of the other mixed acids are measured, and the content of the fluoboric acid in a phosphoric acid, nitric acid, acetic acid and fluoboric acid mixed acid system is indirectly measured, wherein the phosphoric acid is measured by a gravimetric method. The concentration value of the fluoroboric acid obtained by the final test is compared with the theoretical preparation concentration value, and a deviation ratio (the proportion of the difference between the preparation concentration and the test concentration in the preparation concentration) is calculated. The method comprises the following specific steps:
the method comprises the steps of firstly weighing 1g of mixed acid sample with a production formula containing 5.05% of fluoboric acid and 70.1% of phosphoric acid, measuring the content of phosphoric acid according to the national standard GB T2091-2008 weight method, then testing the content of nitric acid by adopting a photometric method, and finally calculating the content of fluoboric acid by subtracting the content of phosphoric acid and nitric acid by utilizing a potentiometric titration result.
The phosphoric acid measured by the gravimetric method has a certain negative deviation, the actual phosphoric acid content of 70.1 percent is 69.6 percent, and finally, in the calculation, the deviations can be fed back to the detection of the content of the fluoboric acid, and the specific deviation is shown in table 1, although the deviation is reduced compared with the content of the fluoboric acid of comparative example 1, the deviation still is 12.1 percent.
Example 1
In this embodiment, phosphoric acid is separated from nitric acid, acetic acid, and fluoroboric acid by extraction, the content of phosphoric acid is titrated separately, the content of nitric acid is measured by a photometric method, and finally, the content of phosphoric acid and nitric acid is subtracted by a potentiometric titration result to calculate the content of fluoroboric acid. The method comprises the following specific steps:
firstly, taking mixed acid containing 5.05 percent of fluoboric acid, 70.1 percent of phosphoric acid, 3.0 percent of nitric acid and 8.5 percent of acetic acid in a production formula, weighing 10g of mixed acid into a plastic separating funnel, adding 50ml of sodium chloride solution with the concentration of 150g/L, adding 10g of ethyl acetate, oscillating and layering, then abandoning an organic phase, extracting for 5 times, completely separating the phosphoric acid from other mixed acid components, transferring an aqueous phase into a plastic beaker, titrating the content of the phosphoric acid in the aqueous phase by using a titrator, and calculating the content of the phosphoric acid as WP70.38%. Then, by utilizing a photometric method, 0.5g of mixed acid sample is weighed to test absorbance, and the content of nitric acid is calculated according to a related absorbance curve, wherein the content of nitric acid is WN＝3.0％。
Finally weighing a sample with the concentration of 0.5g and m in a plastic beaker, adding 40ml of saturated saline solution, selecting a NaOH solution with the concentration of 1mol/L for a titration solution, setting a potential titrator to generate an equivalence point, recording the volume V of the titration solution consumed when the first equivalence point occurs to 4.0984ml, and calculating the fluoroboric acid content W according to the following formulaB。
WB＝(V*C-m*WP/97.994-m*WN/63.01)*87.81/m
Wherein V is the volume of NaOH titration solution consumed when the first equivalence point appears, C is the quantity concentration of NaOH titration solution substances, m is the mass of the weighed mixed acid sample, and W is the weight of the mixed acid samplePPhosphoric acid content, W, calculated for the first stepNThe nitric acid content calculated for the second step.
As shown in table 1, in this embodiment, ethyl acetate is used as an extracting agent, the detection error of the content of phosphoric acid is small, and the deviation ratio of the calculated content of fluoboric acid is lower than that of comparative example 2.
Example 2
As in example 1, the concentration of sodium chloride solution at the time of extraction onlyThe amount was adjusted to 200g/L and set as example 2. The phosphoric acid content measured after the first extraction step is WP70.21%, the second step determines the nitric acid content WN3.0%, the third titration volume V4.1006 ml, and the fluoroboric acid content W was calculated according to the formula in example 1B。
As shown in Table 1, in the present example, butyl acetate was used as the extractant, the concentration of the diluent sodium chloride solution was increased to 200g/L, the detection error of the phosphoric acid content was further reduced, and the deviation ratio of the calculated fluoroboric acid content was lower than that in comparative example 2 and example 1.
Example 3
In the same manner as in example 1, the concentration of the sodium chloride solution was adjusted to 250g/L only in the extraction, and the setting was made in example 3. The phosphoric acid content measured after the first extraction step is WP70.33%, the second step determines the nitric acid content WN3.0%, the third titration volume V4.1001 ml, and the fluoroboric acid content W was calculated according to the formula in example 1B。
As shown in Table 1, in the present example, butyl acetate was used as an extractant, the concentration of the diluent sodium chloride solution was increased to 250g/L, the detection error of the phosphoric acid content was low, and the deviation ratio of the calculated fluoroboric acid content was lower than that in comparative example 2 and example 1, but higher than that in example 2, the concentration of the sodium chloride solution was preferably 200 g/L.
Example 4
As in example 2, only the extractant was adjusted to butyl acetate and set to example 4. The phosphoric acid content measured after the first extraction step is WP70.27%, the second step determines the nitric acid content WN3.0%, the third titration volume V4.1009 ml, and the fluoroboric acid content W was calculated according to the formula in example 1B。
As shown in Table 1, in this example, butyl acetate was used as an extractant, the concentration of the diluent sodium chloride solution was 200g/L, and the detection error of the phosphoric acid content was comparable to that in example 2.
Example 5
Just as in example 2, the extractant was adjusted to chloroform and set to example 5. The phosphoric acid content measured after the first extraction step is WP70.49%, the second step determines the nitric acid content WN＝3.0% of the solution obtained in the third step, the titration volume V was 4.0098ml, and the fluoroboric acid content W was calculated according to the formula in example 1B。
As shown in Table 1, in this example, chloroform was used as an extractant, and the concentration of the diluent sodium chloride solution was 200g/L, and the detection error of the phosphoric acid content was larger than that in the previous example, but still better than that in comparative example 2. According to examples 1 to 5, the extraction effect of ethyl acetate and butyl acetate is better.
Example 6
As in example 2, only at the third titration step, two equivalence points were set to occur and the first equivalence point depletion volume V4.1081 ml and the second equivalence point depletion volume V2 8.3884ml were recorded, respectively. At the first equivalence point, one H + ionized by phosphoric acid, all H + ionized by nitric acid and fluoboric acid are consumed, and at the second equivalence point, the second H + ionized by phosphoric acid and H + ionized by acetic acid are further consumed, so V2 can be used to calculate acetic acid content WCThe formula for calculating the acetic acid content is 8.37 percent
WC＝((V2-V)*C-m*WP/97.994)*60.05/m
The phosphoric acid content measured after the first extraction step is WP70.23%, the second step determines the nitric acid content WN3.0%, the third step was again to calculate the fluoroboric acid content W according to the formula in example 1B。
As shown in Table 1, although two equivalence points are set in the third titration step, the titration solution volume V of the first equivalence point is only needed for calculating the fluoroboric acid content, so that one equivalence point is only needed for titration under the mixed acid system by a person skilled in the art to calculate the fluoroboric acid volume.
Table 1 test results for each comparative example and example
| Grouping | Theoretical value | Test value | Relative deviation of |
| Comparative example 1 | 5.05％ | 3.63％ | 28.1％ |
| Comparative example 2 | 5.05％ | 4.44％ | 12.1％ |
| Example 1 | 5.05％ | 4.73％ | 6.3％ |
| Example 2 | 5.05％ | 4.92％ | 2.6％ |
| Example 3 | 5.05％ | 4.81％ | 4.8％ |
| Example 4 | 5.05％ | 4.87 | 3.6％ |
| Example 5 | 5.05％ | 4.66％ | 7.8％ |
| Example 6 | 5.05％ | 4.90％ | 2.9％ |
It is apparent that the above embodiments are only examples for clearly illustrating and do not limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are therefore intended to be included within the scope of the invention as claimed.
Claims (5)
1. A method for detecting fluoboric acid in mixed acid is characterized by comprising the following steps:
s1, weighing a certain amount of mixed acid sample, separating a phosphoric acid component in the mixed acid by using an extracting agent, measuring the content of phosphoric acid by a titration method, wherein the mixed acid sample is a mixture of phosphoric acid, nitric acid, acetic acid and fluoboric acid, and the extracting agent is ethyl acetate, butyl acetate or chloroform;
s2, weighing a certain amount of mixed acid sample, and determining the content of the nitric acid component by a photometric method;
s3, weighing a certain amount of mixed acid sample, titrating the sample by using a potentiometric titrator, calculating the total content of the phosphoric acid, the nitric acid and the fluoroboric acid through a first equivalence point, and subtracting the content of the phosphoric acid and the nitric acid determined by S1 and S2 to obtain the content of the fluoroboric acid.
2. The method for detecting fluoroboric acid in mixed acid as claimed in claim 1, wherein: in the step S1, the mixed acid sample is diluted by adding NaCl solution with the concentration of 150-250 g/L.
3. The method for detecting fluoroboric acid in mixed acid as claimed in claim 2, wherein: the number of extractions in step S1 is not less than 5.
4. The method for detecting fluoroboric acid in mixed acid as claimed in claim 1, wherein: in step S2, an absorbance standard curve of nitric acid is first drawn, and the nitric acid content is calculated using the absorbance of the sample.
5. The method for detecting fluoroboric acid in mixed acid as claimed in claim 1, wherein: in the step S3, the mass of the mixed acid sample is 0.4500-0.5500 g, the titration solution is NaOH solution with the concentration of 1mol/L, an equivalence point is set by a potentiometric titrator, the volume of the titration solution consumed by the equivalence point is recorded, and when the equivalence point appears, H ionized by phosphoric acid is generated+All of H of nitric acid and fluoroboric acid+The contents of phosphoric acid and nitric acid detected in the steps S1 and S2 are used to calculate the H of the fluoroboric acid+And further calculating the content of the fluoboric acid.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999012026A1 (en) * | 1997-08-28 | 1999-03-11 | Nippon Kasei Chemical Company Limited | Quantitative analysis method, quantitative analyzer, and etching controlling method for mixed acid fluid in etching process, and process for producing said mixed acid fluid |
| CN102167415A (en) * | 2010-02-26 | 2011-08-31 | 三和油化工业株式会社 | Method for separating and recovering phosphoric acid from acetic acid-nitric acid-phosphoric acid series mixed acid waste liquor |
| CN110907509A (en) * | 2019-11-28 | 2020-03-24 | 湖北兴福电子材料有限公司 | Method for detecting hydrofluoric acid in electronic-grade mixed acid |
| CN111855650A (en) * | 2020-07-30 | 2020-10-30 | 青岛科技大学 | Method for determining content of fluosilicic acid, hydrofluoric acid and nitric acid in etching acid |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8945934B2 (en) * | 2012-08-10 | 2015-02-03 | Shenzhen China Star Optoelectronics Technology Co., Ltd. | Potentiometric titration method for measuring concentration of acid mixture of aluminum etchant |
| CN103604856B (en) * | 2013-11-15 | 2015-11-25 | 深圳市华星光电技术有限公司 | A kind of potentiometric titration method of mixed acid solution |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999012026A1 (en) * | 1997-08-28 | 1999-03-11 | Nippon Kasei Chemical Company Limited | Quantitative analysis method, quantitative analyzer, and etching controlling method for mixed acid fluid in etching process, and process for producing said mixed acid fluid |
| CN102167415A (en) * | 2010-02-26 | 2011-08-31 | 三和油化工业株式会社 | Method for separating and recovering phosphoric acid from acetic acid-nitric acid-phosphoric acid series mixed acid waste liquor |
| CN110907509A (en) * | 2019-11-28 | 2020-03-24 | 湖北兴福电子材料有限公司 | Method for detecting hydrofluoric acid in electronic-grade mixed acid |
| CN111855650A (en) * | 2020-07-30 | 2020-10-30 | 青岛科技大学 | Method for determining content of fluosilicic acid, hydrofluoric acid and nitric acid in etching acid |
Non-Patent Citations (2)
| Title |
|---|
| 混合酸中各酸组分的分别测定方法探讨;田云全等;《科技传播》;20110208(第03期);第140-141页 * |
| 混酸(硝酸、磷酸、冰醋酸)的电位滴定分析;陈旗;《浙江化工》;20080115(第01期);第28、31-33页 * |
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Address after: 443007 no.66-3, Yiting Avenue, Yiting District, Yichang City, Hubei Province Patentee after: Hubei Xingfu Electronic Materials Co.,Ltd. Address before: 443007 no.66-3, Yiting Avenue, Yiting District, Yichang City, Hubei Province Patentee before: HUBEI SINOPHORUS ELECTRONIC MATERIALS CO.,LTD. |