CN113504291A - Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) - Google Patents
Sample preparation method and detection method for determining impurities in ultra-high-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The invention relates to a sample preparation method and a detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS, which comprises the following steps: drilling an aluminum wire on an ultra-high purity aluminum sample, cutting the aluminum wire into small sections, arranging a warped part to be in a straight state, cleaning, drying, putting a proper amount of dried sample into a reagent bottle, and dissolving with aqua regia to obtain a sample to be detected; diluting the acid solution of the sample to be tested to a constant volume, analyzing and testing by adopting ICP-MS under an optimized condition, and obtaining the content of the impurity elements in the ultra-high purity aluminum sample by adopting a standard curve method. The sample preparation process of the invention has quick dissolution, can effectively avoid the introduction of pollution, and can effectively eliminate the matrix effect and the background influence of acid through high-power dilution. Meanwhile, the detection method can complete the quantitative determination of dozens of elements within dozens of minutes, and has high detection efficiency.
Description
Technical Field
The invention relates to the technical field of analysis and test of impurity elements in high-purity aluminum materials, in particular to a sample preparation method and a detection method for determining impurities in ultrahigh-purity aluminum by utilizing ICP-MS (inductively coupled plasma-mass spectrometry).
Background
The electronic grade ultra-high purity aluminum (the purity of the aluminum is 99.999 percent or more, 5N or more) has excellent conductivity, ductility, reflectivity and corrosion resistance, and has wide application in the fields of electronic industry and aerospace. High-purity aluminum and aluminum alloy are used as sputtering target raw materials, are widely applied to the fields of semiconductor chips, flat panel displays, solar cells and the like, are used as conductive interconnection lines through sputtering coating, and are one of the most widely used conductive layer thin film materials at present. The quality of the high-purity aluminum directly influences the performance of the high-purity aluminum in the using process, so that the method for quickly, efficiently and accurately detecting the impurities in the high-purity aluminum has important significance.
Because the purity of aluminum in the electronic grade high-purity aluminum is extremely high, the content of other impurity elements is very low, and the total impurity content is less than 10 ppm. The digestion by a general acid-adding wet method needs to dissolve and dilute an aluminum sample in an acid solution. The method has a key problem that the dissolution process of aluminum is slow due to the existence of an oxide layer on the surface of the aluminum, and the detection accuracy is influenced by easily introducing pollution in the long-time sample preparation process. In the traditional method, the massive sample is taken and added with acid to be directly dissolved or microwave digestion is time-consuming and labor-consuming, and the process is very easy to introduce pollution to interfere with the detection accuracy.
Inductively coupled plasma mass spectrometry (ICP-MS) is an inorganic element and isotope analysis and test technology, and a high-sensitivity analysis technology is formed by combining the high-temperature ionization characteristic of inductively coupled plasma with the advantage of sensitive and rapid scanning of a mass spectrometer by using a unique interface technology.
Disclosure of Invention
The invention designs a sample preparation method and a detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS, which solve the technical problems that: (1) provided are a method for reliably and rapidly detecting impurity elements contained in a high-purity aluminum material and a method for preparing a sample thereof. (2) A detection method is provided, which can effectively avoid the introduction of pollution, can effectively eliminate the matrix effect and the background influence of acid, and can complete the quantitative determination of multiple elements in a short time.
In order to solve the technical problems, the invention adopts the following scheme:
a sample preparation method and a detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS comprise the following steps:
and 4, analyzing the standard solution containing the element to be detected by ICP-MS under an optimized condition to obtain a standard curve, diluting the sample to be detected obtained in the step 3 by using an acid solution to a constant volume, and analyzing and testing by ICP-MS under the same condition to obtain the content of the impurity element in the sample solution.
Further, the tool for drilling the aluminum wire in the step 1 is a common electric drill, the thickness of the aluminum wire is 0.1mm-1mm, and the width of the aluminum wire is 0.5mm-5 mm; the length of the aluminum wire cut into small sections is 0.2cm-2 cm;
the cleaning steps in step 2 are as follows: firstly, ultrasonically cleaning an ultra-pure aluminum wire A to be detected for 1min-10min by using absolute ethyl alcohol, ultrasonically cleaning for 1min-6min by using mixed acid, and finally rinsing for 3-5 times by using ultra-pure water; the drying is to blow the ultra-pure aluminum wire A to be tested to dryness by a nitrogen blowing instrument in a dust-free environment after the cleaning step is completed on the ultra-pure aluminum wire A to be tested, and then obtain an ultra-pure aluminum wire B to be tested;
the mass of the ultra-high purity aluminum wire B to be detected selected in the step 3 is 0.1g-0.5 g; the used amount of the aqua regia is immersed in the ultra-high purity aluminum wire B to be detected, and the volume of the aqua regia is not more than 1 ml;
and 4, preparing the standard solution which is purchased commercially and contains the element to be detected or is prepared by a laboratory, covering the content of the impurity element in the sample to be detected in the concentration gradient range of the standard solution, diluting the sample to be detected obtained in the step 3 with an acid solution to a constant volume, and analyzing and testing by ICP-MS under the same condition to obtain the content of the impurity element in the sample solution.
Further, the mixed acid in the mixed acid ultrasonic cleaning in the step 2 comprises the following mixture ratio: nitric acid: hydrochloric acid: ultrapure water ═ 1: (2-5): (4-7); the proportion is volume ratio; the mass fractions of the concentrated nitric acid and the concentrated hydrochloric acid are 65-68% and 36-38% respectively; the ultrasonic power of the ultrasonic cleaning in the step 2 is 100W-1000W.
Further, the specific steps of step 4 are as follows:
step 4.1, taking a proper amount of standard solution mother liquor, diluting with an acid solution and fixing the volume to obtain a multi-element mixed standard solution with the target concentration of 100 ppb;
step 4.2, drawing a standard curve by using a standard addition method, introducing a blank experiment into an ICP-MS (inductively coupled plasma-mass spectrometry) analysis, and analyzing under an optimized condition to obtain 0 point data; then, 100. mu.l, 150. mu.l and 250. mu.l of the mixed standard solution prepared in the step 4.1 are respectively added into the blank, and ICP-MS analysis is introduced to obtain data of 0.2ppb, 0.5ppb and 1ppb respectively;
and 4.3, diluting the sample solution to be tested prepared in the step 3 to a constant volume according to the conditions of the standard curve test, and introducing the sample solution to be tested into ICP-MS analysis and test.
Further, the acid solution for diluting to constant volume in the step 4 is: dilute nitric acid solution with the mass fraction of 2% or hydrochloric acid solution with the mass fraction of 2%.
Further, the dilution multiple in the step 4.3 is 1000-2000 times.
Furthermore, the thickness of the aluminum wire is 0.1mm-0.5mm, and the width of the aluminum wire is 0.5mm-2 mm.
Furthermore, the length of the aluminum wire cut into small sections is 0.2cm-1 cm.
Further, the ultrasonic cleaning time of the ethanol is 2min-5 min; ultrasonic cleaning with mixed acid for 2-4 min.
Further, the ultrasonic power of the ultrasonic cleaning in the step 2 is 500W-800W.
Calculating the content of the impurity elements in the ultra-high purity aluminum sample according to the standard curve by using the test result obtained in the step 4, wherein the unit of the detection result is ppb, and the unit of the calculated content of the impurity elements is ppm, and the calculation method comprises the following steps:
the content of the impurity element in the ultra-high purity aluminum sample is the content of the impurity element in the solution of the sample to be detected multiplied by the dilution factor/1000.
The sample preparation method and the detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS have the following beneficial effects:
(1) according to the sample preparation method and the sample preparation process of the detection method for detecting the impurities in the ultra-high purity aluminum by utilizing ICP-MS, the dissolution is rapid, the introduction of pollution can be effectively avoided, and the matrix effect and the background influence of acid can be effectively eliminated by high-power dilution.
(2) The sample preparation method and the detection method for detecting the impurities in the ultra-high-purity aluminum by utilizing the ICP-MS can detect the contents of more than 20 impurities in the high-purity aluminum at one time, and more elements can be simultaneously detected correspondingly to the increase of the element types in the standard solution. The method can complete the quantitative determination of dozens of elements within ten minutes, and has very high detection efficiency.
(3) The sample preparation method and the detection method for measuring the impurities in the ultra-high purity aluminum by utilizing the ICP-MS have the advantages of high sensitivity, high speed, simple spectral line and less interference compared with the spectral technology. The method can realize simple, convenient, rapid and accurate analysis and test on the impurity elements in the high-purity aluminum with the purity of 5N or above.
Drawings
FIG. 1: the optimized standard curve diagram of lithium, beryllium and boron elements under the ICP-MS test condition is obtained;
FIG. 2: the optimized standard curve diagram of sodium, magnesium and silicon elements under the ICP-MS test condition is obtained;
FIG. 3: the invention optimizes the standard curve chart of phosphorus and potassium elements under the ICP-MS test condition;
FIG. 4: the invention optimizes the calcium element standard curve chart under the ICP-MS test condition;
FIG. 5: the optimized standard curve graphs of titanium, vanadium and chromium elements under the ICP-MS test condition are obtained;
FIG. 6: the optimized standard curve diagram of manganese, iron and cobalt elements under the ICP-MS test condition is obtained;
FIG. 7: the optimized standard curve diagram of nickel, copper and zinc elements under the ICP-MS test condition;
FIG. 8: the invention optimizes the standard curve chart of zinc, gallium and zirconium elements under the ICP-MS test condition;
FIG. 9: the invention optimizes the standard curve chart of arsenic, molybdenum and selenium under the ICP-MS test condition;
FIG. 10: the optimized standard curve diagram of lead, silver and cadmium elements under the ICP-MS test condition is obtained;
FIG. 11: the optimized standard curve diagram of cesium, barium and gold elements under the ICP-MS test condition is obtained;
FIG. 12: the optimized standard curve chart of bismuth and uranium elements under the ICP-MS test condition is provided.
Detailed Description
The invention is further described with reference to the following drawings and specific examples:
examples
The invention relates to a sample preparation method and a detection method for detecting impurities in ultra-high purity aluminum by utilizing ICP-MS, wherein the sample preparation method comprises the following working conditions:
million-grade dust-free laboratory, temperature 25 deg.C, humidity 30% -50%. The used reagent is a spectral pure reagent, the water is ultrapure water, and the resistivity is more than or equal to 18M omega cm; the vessels used were PFA, all of which were boiled with a hydrochloric acid solution and cleaned with ultrapure water.
The invention relates to a sample preparation method and a detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS, which comprises the following steps:
and 4, analyzing the standard solution containing the element to be detected by ICP-MS under an optimized condition to obtain a standard curve, diluting the sample to be detected obtained in the step 3 by using an acid solution to a constant volume, and analyzing and testing by ICP-MS under the same condition to obtain the content of the impurity element in the sample solution.
Sampling by using a common electric drill, wherein the thickness of the drilled aluminum wire is 0.3mm, the width of the drilled aluminum wire is 2mm, and the aluminum wire is in a curled shape; cutting the aluminum wire into small sections with the length of 1cm by using Polytetrafluoroethylene (PTFE) tweezers before cleaning, and finishing and straightening the warped parts to obtain the ultra-pure aluminum wire A to be detected.
The cleaning step in step 2 is specifically as follows: firstly, ultrasonically cleaning an ultra-pure aluminum wire A to be detected for 2min by using absolute ethyl alcohol, ultrasonically cleaning for 2min by using mixed acid, and finally washing for 5 times by using ultra-pure water; and after the cleaning step is finished, blow-drying by using a nitrogen blowing instrument in a dust-free environment, and then obtaining the ultra-pure aluminum wire B to be detected.
The mass of the ultra-pure aluminum wire B to be detected selected in the step 3 is 0.1 g; the amount of the used aqua regia is immersed in the ultra-high purity aluminum wire B to be detected, the volume of the used aqua regia is not more than 1ml, and the aluminum wire is completely soaked by slight shaking. Weighing, peeling and zeroing the reagent bottle on a balance before putting the ultra-pure aluminum wire B to be detected. The volume ratio of the mixed acid in the ultrasonic cleaning of the mixed acid in the step 2 is as follows: nitric acid: hydrochloric acid: ultrapure water 1: 5: 6; the concentrated nitric acid and the concentrated hydrochloric acid are directly purchased and respectively comprise 65-68% of concentrated nitric acid and 36-38% of concentrated hydrochloric acid by mass fraction. The ultrasonic power of the ultrasonic cleaning in the step 2 is 600W.
The standard solution in the step 4 is a commercially purchased standard solution containing the element to be detected or a standard solution prepared by a laboratory, and the concentration gradient range of the standard solution covers the content of the impurity element in the sample to be detected.
The specific steps of step 4 are as follows:
and 4.1, taking a proper amount of standard solution mother liquor, diluting with 2% dilute nitric acid to a constant volume to obtain a multi-element mixed standard solution with the target concentration of 100 ppb.
Step 4.2, drawing a standard curve by using a standard addition method, introducing a blank experiment into an ICP-MS (inductively coupled plasma-mass spectrometry) analysis, and analyzing under an optimized condition to obtain 0 point data; then, 100. mu.l, 150. mu.l and 250. mu.l of the mixed standard solution prepared in the step 4.1 are respectively added into the blank, and ICP-MS analysis is introduced to obtain data of 0.2ppb, 0.5ppb and 1ppb respectively;
the standard solution of the invention contains the following list of elements: li, Be, B, Na, Mg, Si, P, S, K, Ca, Ti, V, Ga, Zr, As, Mo, Se, Ag, Cd, Cs, Ba, Ce, U, Ge, Nb, Re, Ta, W, Co, Cr, Fe, Mn, Ni, Pb, Rb, Zn. The inclusion elements may vary depending on the original standard solution used or the self-formulation conditions.
And 4.3, diluting the sample solution to be tested prepared in the step 3 by 1500 times according to the test conditions of the standard curve, and introducing the diluted sample solution into ICP-MS for analysis and test.
Calculating the content of impurity elements in the ultra-high purity aluminum sample according to the standard curve by using the test result obtained in the step 4, wherein the unit of the test result is ppb, and the unit of the content of the impurity elements obtained by calculation is ppm, and the calculation method comprises the following steps:
the content of the impurity element in the ultra-high purity aluminum sample is the content of the impurity element in the solution of the sample to be detected multiplied by the dilution factor/1000.
The method provided by the invention can be used for verifying the accuracy of the method through standard curve data.
And (3) performing data acquisition on the standard solution by adopting the optimized ICP-MS test conditions to obtain standard curve data, wherein the linear correlation of the corresponding element standard curve is very good, and the linear correlation coefficient R is more than 0.99 as shown in attached figures 1-12, so that the accuracy of the method is proved.
Table 1 shows the test results of the samples to be tested, which accurately quantifies 29 elements contained in the samples to be tested, the content of impurity elements in the samples is within the concentration gradient range of the standard solution, and the standard recovery rates are all within the range of 100 +/-20%, thus proving the reliability of the method.
And after the test result is converted according to the dilution times and normalized, the purity of the ultra-high purity aluminum sample is 99.9991%, which is consistent with the purity of the detection result of a glow discharge mass spectrometer. This result further demonstrates the reliability of the inventive method.
TABLE 1 results of sample measurement (unit: ppb)
TABLE 2 Glow Discharge Mass Spectrometry (GDMS) detection data control
The sample preparation method and the detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS have the following beneficial effects:
(1) according to the sample preparation method and the sample preparation process of the detection method for detecting the impurities in the ultra-high purity aluminum by utilizing ICP-MS, the dissolution is rapid, the introduction of pollution can be effectively avoided, and the matrix effect and the background influence of acid can be effectively eliminated by high-power dilution.
(2) The sample preparation method and the detection method for detecting the impurities in the ultra-high-purity aluminum by utilizing the ICP-MS can detect the contents of more than 20 impurities in the high-purity aluminum at one time, and more elements can be simultaneously detected correspondingly to the increase of the element types in the standard solution. The method can complete the quantitative determination of dozens of elements within ten minutes, and has very high detection efficiency.
(3) The sample preparation method and the detection method for measuring the impurities in the ultra-high purity aluminum by utilizing the ICP-MS have the advantages of high sensitivity, high speed, simple spectral line and less interference compared with the spectral technology. The method can realize simple, convenient, rapid and accurate analysis and test on the impurity elements in the high-purity aluminum with the purity of 5N or above.
The present invention has been described in connection with the specific embodiments, and it is to be understood that the invention is not limited to the above-described embodiments, and various modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A sample preparation method and a detection method for determining impurities in ultra-high purity aluminum by utilizing ICP-MS are characterized by comprising the following steps:
step 1, drilling an aluminum wire on an ultra-high purity aluminum original sample, cutting the aluminum wire into small sections, and arranging a warped part to be in a straight state to obtain an ultra-high purity aluminum wire A to be detected;
step 2, cleaning the ultra-high purity aluminum wire A to be detected obtained in the step 1, and then drying to obtain an ultra-high purity aluminum wire B to be detected;
step 3, taking a proper amount of the ultra-high purity aluminum wire B sample to be detected obtained in the step 2, and dissolving the sample in a PFA reagent bottle by using aqua regia to obtain a sample to be detected;
and 4, analyzing the standard solution containing the element to be detected by ICP-MS under an optimized condition to obtain a standard curve, diluting the sample to be detected obtained in the step 3 by using an acid solution to a constant volume, and analyzing and testing by ICP-MS under the same condition to obtain the content of the impurity element in the sample solution.
2. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 1, wherein:
the tool for drilling the aluminum wire in the step 1 is a common electric drill, and the aluminum wire is 0.1mm-1mm in thickness and 0.5mm-5mm in width; the length of the aluminum wire cut into small sections is 0.2cm-2 cm;
the cleaning steps in step 2 are as follows: firstly, ultrasonically cleaning an ultra-pure aluminum wire A to be detected for 1min-10min by using absolute ethyl alcohol, ultrasonically cleaning for 1min-6min by using mixed acid, and finally rinsing for 3-5 times by using ultra-pure water; the drying is to blow the ultra-pure aluminum wire A to be tested to dryness by a nitrogen blowing instrument in a dust-free environment after the cleaning step is completed on the ultra-pure aluminum wire A to be tested, and then obtain an ultra-pure aluminum wire B to be tested;
the mass of the ultra-high purity aluminum wire B to be detected selected in the step 3 is 0.1g-0.5 g; the used amount of the aqua regia is immersed in the ultra-high purity aluminum wire B to be detected, and the volume of the aqua regia is not more than 1 ml;
and 4, preparing the standard solution which is purchased commercially and contains the element to be detected or is prepared by a laboratory, covering the content of the impurity element in the sample to be detected in the concentration gradient range of the standard solution, diluting the sample to be detected obtained in the step 3 with an acid solution to a constant volume, and analyzing and testing by ICP-MS under the same condition to obtain the content of the impurity element in the sample solution.
3. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 1 or 2, characterized in that: the mixed acid in the mixed acid ultrasonic cleaning in the step 2 comprises the following mixture ratio: nitric acid: hydrochloric acid: ultrapure water ═ 1: (2-5): (4-7); the proportion is volume ratio; the mass fractions of the concentrated nitric acid and the concentrated hydrochloric acid are 65-68% and 36-38% respectively; the ultrasonic power of the ultrasonic cleaning in the step 2 is 100W-1000W.
4. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 3, wherein: the specific steps of the step 4 are as follows:
step 4.1, taking a proper amount of standard solution mother liquor, diluting with an acid solution and fixing the volume to obtain a multi-element mixed standard solution with the target concentration of 100 ppb;
step 4.2, drawing a standard curve by using a standard addition method, introducing a blank experiment into an ICP-MS (inductively coupled plasma-mass spectrometry) analysis, and analyzing under an optimized condition to obtain 0 point data; then, 100. mu.l, 150. mu.l and 250. mu.l of the mixed standard solution prepared in the step 4.1 are respectively added into the blank, and ICP-MS analysis is introduced to obtain data of 0.2ppb, 0.5ppb and 1ppb respectively;
and 4.3, diluting the sample solution to be tested prepared in the step 3 to a constant volume according to the conditions of the standard curve test, and introducing the sample solution to be tested into ICP-MS analysis and test.
5. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 1, 2 or 4, characterized in that: the acid solution for diluting and fixing the volume in the step 4 is as follows: dilute nitric acid solution with the mass fraction of 2% or hydrochloric acid solution with the mass fraction of 2%.
6. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 5, wherein: the dilution multiple in the step 4.3 is 1000-2000 times.
7. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 6, wherein: the thickness of the aluminum wire is 0.1mm-0.5mm, and the width of the aluminum wire is 0.5mm-2 mm.
8. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 6, wherein: the length of the aluminum wire cut into small sections is 0.2cm-1 cm.
9. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 6, wherein: the ultrasonic cleaning time of the ethanol is 2min-5 min; ultrasonic cleaning with mixed acid for 2-4 min.
10. The sample preparation method and detection method for determining impurities in ultra-high purity aluminum by ICP-MS according to claim 6, wherein: the ultrasonic power of the ultrasonic cleaning in the step 2 is 500W-800W.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113933376A (en) * | 2021-10-27 | 2022-01-14 | 雅邦绿色过程与新材料研究院南京有限公司 | Semiconductor solvent ICP-MS determination method based on multiple dilution method |
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