Method for preparing high-temperature alloy powder sample by glow discharge mass spectrometry

Abstract

The invention belongs to the technical field of analysis and detection, and particularly relates to a method for preparing a glow discharge mass spectrometry high-temperature alloy powder sample. The method comprises the following steps: (1) melting a proper amount of indium in an inert gas atmosphere; (2) adding high-temperature alloy powder into the molten indium, and uniformly stirring by using a magnetic stirrer; and (3) pouring the mixed sample and indium into a mold, cooling and solidifying, and treating the sample into a proper size. According to the method for preparing the glow discharge mass spectrometry high-temperature alloy powder sample, the uniformity of the sample can be guaranteed, it is guaranteed that the sample can be detected for multiple times, the accuracy and repeatability of the sample are improved, and the problems that powder is prone to falling off and pollutes equipment in a conventional method are solved.

Description

Technical Field

[0001] The invention belongs to the technical field of analysis and detection, and particularly relates to a method for preparing a glow discharge mass spectrometry high-temperature alloy powder sample. Background Art

[0002] Powder metallurgy high temperature alloy is a high temperature alloy prepared by powder metallurgy. Compared with traditional cast and forged high temperature alloy, it has the advantages of uniform organization, no macroscopic segregation, high yield strength, good fatigue performance, etc. It overcomes the segregation (unevenness) produced by conventional processes. Each particle of the pre-alloyed powder used is a microscopic ingot. Alloy segregation can only occur within a small range of powder particles, which can improve the comprehensive performance of the alloy, reduce the amount of cutting, and improve the utilization rate of the alloy. In particular, as the composition of high temperature alloys becomes increasingly complex and the size of parts continues to increase, powder metallurgy high temperature alloys show greater superiority. Powder high temperature alloys are mainly used to manufacture high temperature load-bearing rotating parts such as turbine disks, compressor disks, drum shafts, sealing disks, sealing rings, and guide wheels of aircraft engines.

[0003] Glow discharge mass spectrometry can accurately determine the content of all elements from ppb to matrix in one scan. It is widely used in impurity detection of high-purity metals, semiconductor materials and aerospace materials. It can analyze both needle-shaped samples and block samples. For powder sample detection, it is bonded with indium for analysis.

[0004] At present, the general method for preparing powder samples for glow discharge mass spectrometer detection is to place the powder on an indium sheet and press the powder to stick it to the indium sheet. There are the following problems in preparing sample indium sheets in this way: the indium sheet is oxidized during the sample preparation process, which will interfere with the sample during the detection process; the uneven distribution of powder due to uneven powder spreading and uniform force on the sample will affect the uniformity and repeatability of sample detection; the powder is not firmly bonded and enters the equipment to contaminate the equipment, interfere with the detection, and even damage the equipment. Summary of the invention

[0005] In view of the above problems, the present invention provides a method for preparing high-temperature alloy powder samples by glow discharge mass spectrometry, which solves the problem that uneven powder distribution caused by uneven powder spreading and uniform force on sample pressing affects the uniformity and repeatability of sample detection.

[0006] The technical solution of the present invention is: A method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, characterized in that it comprises the following steps: Step (1), take 5.8 indium, wash it with 10%-30% nitric acid for 10min-20min, soak it in distilled water for 30 minutes, then wash it with distilled water for 3-5 times, and melt the treated indium in an inert gas Ar atmosphere; Step (2), taking 0.3g-0.5g of high temperature alloy powder and adding it to molten indium in an inert gas Ar atmosphere, and stirring it fully with a magnetic stirrer to mix the high temperature alloy powder and indium evenly, so as to avoid inaccurate results due to uneven distribution of the sample; Step (3), in an inert gas Ar atmosphere, pour the evenly mixed liquid in step (2) into a mold to cool and solidify, and process and obtain a sample of a size suitable for detection. The sample size is: 20mm-25mm in length, 20mm-25mm in width, and 2mm-5mm in thickness. Directly using a mold to solidify and shape can reduce the loss of indium sheets and save costs.

[0007] Furthermore, in the above-mentioned method for preparing a high-temperature alloy powder sample for glow discharge mass spectrometry, the purity of indium in step (1) is ≥99.9999%, and the oxide on the surface of indium can be removed by washing with nitric acid; and the immersion and washing with distilled water can fully wash away impurities such as nitric acid and indium nitrate remaining on the surface of indium, thereby reducing interference.

[0008] Furthermore, in the above-mentioned method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, steps (1) to (3) are carried out in an inert gas Ar atmosphere, which effectively eliminates the interference of gases in the air on the detection.

[0009] Furthermore, in the above-mentioned method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, the type and size of the high-temperature alloy powder are not limited and is applicable to all high-temperature alloy powders.

[0010] Advantages and beneficial effects of the present invention: The present invention prepares a glow discharge mass spectrometry high-temperature alloy powder sample, has simple operation, and can effectively avoid the problems of large differences in test results caused by uneven sample distribution, unstable test results, and easy powder contamination of equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 The variation trend of Ni concentration in the sample (GH3230 powder) prepared in implementation 1 of the present invention during the analysis test; Figure 2 The variation trend of Ni concentration in the sample (GH3230 powder) prepared in implementation 2 of the present invention in the analysis test; Figure 3 The variation trend of Ni concentration in the sample (GH3230 powder) prepared in implementation 3 of the present invention in the analysis test; Figure 4 The variation trend of Ni concentration in the sample (GH3230 powder) prepared in implementation 4 of the present invention in the analysis test; Figure 5 This is the changing trend of Ni concentration in the sample (GH3230 powder) prepared by directly spreading powder on indium sheet during the analysis test. DETAILED DESCRIPTION

[0012] The specific implementation modes of the present invention are further described in detail below in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention but cannot be used to limit the scope of the present invention.

[0013] Example 1

[0014] This embodiment provides a method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, taking high-temperature alloy powder GH3230 as an example, comprising the following steps: Step (1), taking 5.8 g of indium with a purity of ≥99.9999%, washing it with 10% nitric acid for 20 minutes, soaking it with distilled water for 30 minutes, and then washing it with distilled water for 5 times, and melting the treated indium in an inert gas Ar atmosphere; Step (2), taking 0.1 g of high-temperature alloy powder and adding it to molten indium in an inert gas Ar atmosphere, and stirring it thoroughly with a magnetic stirrer to mix the high-temperature alloy powder and indium evenly; Step (3), in an inert gas Ar atmosphere, pour the evenly mixed liquid in step (2) into a mold to cool and solidify, and process to obtain a sample of a size suitable for detection, the sample size is: 20 mm long, 20 mm wide, and 2 mm thick.

[0015] The samples prepared in Example 1 were tested and analyzed, and the variation trend of Ni concentration in the test was analyzed. Figure 1 shown.

[0016] Example 2

[0017] This embodiment provides a method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, taking high-temperature alloy powder GH3230 as an example, comprising the following steps: Step (1), taking 5.8 g of indium with a purity of ≥99.9999%, washing it with 10% nitric acid for 20 minutes, soaking it with distilled water for 30 minutes, and then washing it with distilled water for 5 times, and melting the treated indium in an inert gas Ar atmosphere; Step (2), taking 0.2 g of high-temperature alloy powder and adding it into molten indium in an inert gas Ar atmosphere, and stirring it fully with a magnetic stirrer to mix the high-temperature alloy powder and indium evenly; Step (3), in an inert gas Ar atmosphere, pour the evenly mixed liquid in step (2) into a mold to cool and solidify, and process to obtain a sample of a size suitable for detection, the sample size is: 20 mm long, 20 mm wide, and 2 mm thick.

[0018] The samples prepared in Example 2 were tested and analyzed, and the trend of Ni concentration in the test was analyzed. Figure 2 shown.

[0019] Example 3

[0020] This embodiment provides a method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, taking high-temperature alloy powder GH3230 as an example, comprising the following steps: Step (1), taking 5.8 g of indium with a purity of ≥99.9999%, washing it with 10% nitric acid for 20 minutes, soaking it with distilled water for 30 minutes, and then washing it with distilled water for 5 times, and melting the treated indium in an inert gas Ar atmosphere; Step (2), taking 0.3 g of high-temperature alloy powder and adding it into molten indium in an inert gas Ar atmosphere, and stirring it fully with a magnetic stirrer to mix the high-temperature alloy powder and indium evenly; Step (3), in an inert gas Ar atmosphere, pour the evenly mixed liquid in step (2) into a mold to cool and solidify, and process to obtain a sample of a size suitable for detection, the sample size is: 20 mm long, 20 mm wide, and 2 mm thick.

[0021] The samples prepared in Example 3 were tested and analyzed, and the trend of Ni concentration in the test was analyzed. Figure 3 shown.

[0022] Example 4

[0023] This embodiment provides a method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, taking high-temperature alloy powder GH3230 as an example, comprising the following steps: Step (1), taking 5.8 g of indium with a purity of ≥99.9999%, washing it with 10% nitric acid for 20 minutes, soaking it with distilled water for 30 minutes, and then washing it with distilled water for 5 times, and melting the treated indium in an inert gas Ar atmosphere; Step (2), taking 0.5 g of high-temperature alloy powder and adding it into molten indium in an inert gas Ar atmosphere, and stirring it fully with a magnetic stirrer to mix the high-temperature alloy powder and indium evenly; Step (3), in an inert gas Ar atmosphere, pour the evenly mixed liquid in step (2) into a mold to cool and solidify, and process to obtain a sample of a size suitable for detection, the sample size is: 20 mm long, 20 mm wide, and 2 mm thick.

[0024] The samples prepared in Example 4 were tested and analyzed, and the variation trend of Ni concentration in the test was analyzed. Figure 4 shown.

[0025] Example 5

[0026] This embodiment provides a method for preparing a high-temperature alloy powder sample by glow discharge mass spectrometry, taking high-temperature alloy powder GH3230 as an example, comprising the following steps: Step (1), taking 5.8 g of indium with a purity of ≥99.9999%, washing it with 10% nitric acid for 20 min, soaking it in distilled water for 30 min, and then washing it with distilled water for 5 times, and pressing it into a sheet with a length of 20 mm, a width of 20 mm, and a thickness of 2 mm in an inert gas Ar atmosphere; Step (2), taking 0.2 g of high temperature alloy powder, spreading the powder on the indium sheet in step (1) in an inert gas Ar atmosphere and compacting it to obtain a sample to be tested; The samples prepared in Example 5 were tested and analyzed, and the trend of Ni concentration in the test was analyzed. Figure 5 shown.

[0027] contrast Figure 1 , Figure 2 , Figure 3 and Figure 4 Compared with the Ni concentration (signal intensity), the mass of high-temperature alloy powder should be controlled at 0.3g-0.5g. When the powder mass is less than 0.3g, the sample is reduced after several tests, resulting in a decrease in element intensity and failure to detect.

[0028] contrast Figure 3 and Figure 5 , when the method of directly spreading powder on the indium sheet is adopted ( Figure 5 ) is likely to cause uneven powder distribution. As the sputtering time increases, the Ni concentration (signal intensity) will gradually decrease. This is caused by the gradual reduction of powder during the sputtering process, resulting in a weakening of the signal. When this method is used to melt the powder sample and the indium sheet together ( Figure 3 ), the Ni concentration (signal intensity) changes very little over time, and the results are stable. Figures 1 to 5 The comparison shows that this method can avoid the problem of unstable results caused by direct powder spreading, and at the same time avoid the powder entering the equipment due to loose bonding.

Claims

1. A method for preparing high temperature alloy powder samples by glow discharge mass spectrometry, characterized in that: The following steps are involved: Step (1), take 5.8 indium, wash it with 10%-30% nitric acid for 10min-20min, soak it in distilled water for 30 minutes, then wash it with distilled water for 3-5 times, and melt the treated indium in an inert gas Ar atmosphere; Step (2), taking 0.3 g to 0.5 g of high temperature alloy powder and adding it to molten indium in an inert gas Ar atmosphere, and stirring it thoroughly with a magnetic stirrer to mix the high temperature alloy powder and indium evenly; Step (3), in an inert gas Ar atmosphere, pour the evenly mixed liquid in step (2) into a mold to cool and solidify, and process and obtain a sample of a size suitable for detection, the sample size is: 20mm-25mm in length, 20mm-25mm in width, and 2mm-5mm in thickness.

2. The method for preparing high temperature alloy powder samples by glow discharge mass spectrometry according to claim 1, characterized in that: The purity of indium in step (1) is ≥99.9999%.

3. The method for preparing high temperature alloy powder samples by glow discharge mass spectrometry according to claim 1, characterized in that: The type and size of the high temperature alloy powder are not limited.

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