Method for detecting components of aluminum-scandium alloy target material and application thereof

Abstract

The application discloses a kind of aluminum scandium alloy target material component detection method and application thereof, belong to alloy detection technical field.The detection method includes the following steps: aluminum scandium alloy target material is placed in suspension smelting furnace, and with 200~300kw / min Speed regulation power to 350~550kw is melted, after alloy melt is fully melted 20s~50s inside test and record corresponding melt temperature, and with aluminum scandium alloy target material theoretical melting point is compared, obtains aluminum scandium alloy target material component information;The detection method provided by the application can be nondestructive, quickly, low-cost to obtain the component information in aluminum scandium alloy target material;And the aluminum scandium alloy target material component detection method of the application can be applied to actual aluminum scandium target blank production process, so as to help quickly, accurately, efficiently and low-cost to produce specific scandium content aluminum scandium target blank;Meanwhile, the detection method provided by the application is simple to operate, and can be beneficial to practical production.

Description

Technical Field

[0001] This invention belongs to the field of alloy detection technology, and particularly relates to a method for detecting the composition of aluminum-scandium alloy targets and its application. Background Technology

[0002] Melting point is a crucial factor in the research of metallic materials. Determining a material's melting point not only allows for the assessment of its purity and composition by comparing it with the theoretical melting point, but also provides significant guidance for practical industrial applications. Aluminum-scandium alloy sputtering targets are primarily used in specialized fields, such as the fabrication of micro-electromechanical systems (MEMS) integrating micro-sensors, actuators, signal processing and control circuits, interface circuits, communication, and power supplies. Currently, commercially available aluminum-scandium sputtering targets come in various compositions, primarily based on Sc content, including 9.6wt%, 13wt%, 15wt%, 20wt% to 22.7wt%, and 30wt%, among others. The Sc content needs to be controlled with a precision ranging from 0.3wt% to 0.5wt%.

[0003] Currently, the determination of Sc content in aluminum-scandium alloy targets is carried out using ICP-OES, titration, or XRF spectroscopy. Chinese invention patent CN113237871A describes a method for detecting AlSc alloy composition, which involves heating AlSc alloy and mixed acid to obtain a mixed solution, and then testing it using ICP-OES. This method can simultaneously detect the two main elements, Al and Sc, with high accuracy. Another document discloses another detection method, which involves dissolving the aluminum-scandium alloy target sample in hydrochloric acid, using xylenol orange as an indicator, and titrating it with disodium ethylenediaminetetraacetate standard solution within a certain acidity range to determine the scandium content in the aluminum-scandium alloy (Shi Lixin, Analysis of Scandium Element Content in Aluminum-Scandium Intermediate Alloy, Light Alloy Processing Technology [J], 2014, 42(2)60~63).

[0004] In actual production, aluminum scandium target billets often require melting and casting, followed by titration or ICP-OES sampling to test the Sc content. If the results are satisfactory, further processing continues; otherwise, the composition is adjusted or the billet is discarded. This process is costly and time-consuming, severely impacting production efficiency. Furthermore, most aluminum scandium alloy targets with the aforementioned compositions are cast using a suspension melting furnace with rapid cooling, as illustrated in CN201911138528.4 (a method for preparing aluminum alloy targets), CN201911133830.0 (a method for preparing aluminum scandium alloy targets), and CN201910728796.5 (aluminum scandium alloy targets and their preparation method). Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide a rapid, accurate, non-destructive, and low-cost method for detecting the composition of aluminum-scandium alloy targets and its application.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a method for detecting the composition of an aluminum-scandium alloy target, the method comprising the following steps: placing the aluminum-scandium alloy target in a suspension melting furnace, and adjusting the power to 350-550 kW at a speed of 200-300 kW / min for melting; testing the melt temperature within 20-50 seconds after the aluminum-scandium alloy target is fully melted, recording the corresponding melt temperature, and comparing it with the theoretical melting point of the aluminum-scandium alloy target to obtain the composition information of the aluminum-scandium alloy target.

[0007] The present invention provides a method for detecting the composition of aluminum-scandium alloy targets, which can obtain the composition information of aluminum-scandium alloy targets non-destructively, quickly and at low cost, without the need to take out a portion for testing after the target blank is prepared. By selecting a specific melting power and the speed at which the melting power is reached, and by selecting an appropriate testing time, the present invention can obtain the corresponding melt temperature that has a clear relationship with the aluminum-scandium alloy target, thereby obtaining the corresponding aluminum-scandium alloy target content information. The theoretical basis of this invention is twofold. First, according to the binary phase diagram of aluminum-scandium alloys, different scandium contents correspond to different alloy melting points. Therefore, theoretically, the scandium content in aluminum-scandium alloy targets can be determined by the alloy melting point. Second, a significant drawback of vacuum electromagnetic levitation melting technology is that after the corresponding metal or alloy is melted, further increasing the heating power cannot significantly increase the temperature of the molten pool. Experiments have shown that the temperature hardly increases after exceeding the melting point by 100-150°C. Based on the above two theoretical foundations and raw materials, this invention determines the alloy composition by measuring the temperature of the alloy melt, thereby achieving rapid, low-cost, and non-destructive detection of the composition of aluminum-scandium alloy targets.

[0008] As a preferred embodiment of the detection method for aluminum-scandium alloy target material of the present invention, the detection method includes the following steps: placing the aluminum-scandium alloy target material in a suspension melting furnace, and adjusting the power to 500 kW at a speed of 250 kW / min for melting; testing the melt temperature within 30 seconds after the aluminum-scandium alloy target material is fully melted, recording the corresponding melt temperature, and comparing it with the theoretical melting point of the aluminum-scandium alloy target material to obtain the component information of the aluminum-scandium alloy target material.

[0009] The inventors discovered that when the specific power change rate, final melting power, and test time after full melting are taken at the above-mentioned values, the accuracy of the obtained detection method is higher.

[0010] As a preferred embodiment of the detection method for aluminum-scandium alloy target material components described in this invention, the process of comparing with the theoretical melting point of aluminum-scandium alloy target material is as follows: add 90 to 110°C to the theoretical melting point to obtain the corresponding temperature range. If the measured melt temperature is within the obtained temperature range, then the scandium content in the aluminum-scandium alloy target material is the scandium content value corresponding to the theoretical melting point.

[0011] For example, the theoretical melting point of an aluminum-scandium alloy sputtering target (scandium content of 9.6 wt%) is 960℃. Adding 90 to 110℃ to its theoretical melting point gives a corresponding temperature range of 1050 to 1070℃. The theoretical melting point of an aluminum-scandium alloy sputtering target (scandium content of 13 wt%) is 1000℃. Adding 90 to 110℃ to its theoretical melting point gives a corresponding temperature range of 1090 to 1110℃. If the measured melt temperature is 1060℃, it falls within the 1050 to 1070℃ range, meaning the scandium content in the tested aluminum-scandium alloy sputtering target is 9.6 wt%. If the measured melt temperature is 1090℃, it falls within the 1090 to 1110℃ range, meaning the scandium content in the tested aluminum-scandium alloy sputtering target is 13 wt%.

[0012] In a preferred embodiment of the method for detecting the composition of the aluminum-scandium alloy target material described in this invention, the melting time is 5-6 minutes.

[0013] The inventors discovered that, within the aforementioned melting time range, by combining the melting power and power adjustment rate of this invention, it is possible to ensure that the added aluminum-scandium alloy target material reaches a fully melted state.

[0014] As a preferred embodiment of the method for detecting the composition of aluminum-scandium alloy target material according to the present invention, before placing the aluminum-scandium alloy target material in the suspension melting furnace, the method further includes a step of cutting the aluminum-scandium alloy target material into pieces.

[0015] In a preferred embodiment of the method for detecting the components of the aluminum-scandium alloy target material according to the present invention, the shearing involves shearing the aluminum-scandium alloy target material into fragments with a diameter of 1 to 5 cm.

[0016] Further cutting the aluminum-scandium alloy target into smaller pieces and then smelting it can ensure a more uniform dispersion of components, thereby helping to further improve the accuracy of detection.

[0017] In addition, the present invention also provides an application of the method for detecting the composition of the aluminum-scandium alloy target in the preparation of aluminum-scandium target blanks.

[0018] The actual production process of aluminum scandium target billet includes a melting step. By using the detection method of the present invention during the melting process, the scandium content information in the actual alloy can be obtained. If it is found that the content is inconsistent with the specific aluminum scandium target billet composition to be obtained, the composition can be adjusted by adding or subtracting scandium or aluminum composition, thereby achieving a fast, convenient and efficient aluminum scandium target billet production process.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0020] This invention provides a method for detecting the composition of aluminum-scandium alloy targets. This method can obtain the composition information of aluminum-scandium alloy targets non-destructively, rapidly, and at low cost, without the need to take a portion for testing after the target blank is prepared. By selecting a specific melting power and the speed at which the melting power is reached, and by selecting an appropriate testing time, this invention can obtain the corresponding melt temperature that has a clear relationship with the aluminum-scandium alloy target, thereby obtaining the corresponding aluminum-scandium alloy target content information. Furthermore, the method for detecting the composition of aluminum-scandium alloy targets provided by this invention can be applied to the actual production process of aluminum-scandium target blanks, thereby helping to produce aluminum-scandium target blanks with specific scandium contents quickly, accurately, efficiently, and at low cost. At the same time, the detection method provided by this invention is simple to operate and can be beneficial for practical production. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the binary phase diagram of an aluminum-scandium alloy.

[0022] Figure 2 This is a schematic diagram showing the relationship between the theoretical melting point and the melt temperature of aluminum-scandium alloys.

[0023] Figure 3 This is a schematic diagram of the process for testing melt temperature. Detailed Implementation

[0024] To better illustrate the purpose, technical solution, and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0025] This invention provides a method for detecting the composition of an aluminum-scandium alloy target. The method includes the following steps: placing the aluminum-scandium alloy target in a suspension melting furnace and adjusting the power to 350-550 kW at a speed of 200-300 kW / min for melting; testing the melt temperature within 20-50 seconds after the aluminum-scandium alloy target is fully melted; recording the corresponding melt temperature; comparing it with the theoretical melting point of the aluminum-scandium alloy target; analyzing the comparison results; and obtaining the composition information of the aluminum-scandium alloy target.

[0026] according to Figure 1 The schematic diagram of the aluminum-scandium alloy binary phase diagram shows the scandium content and corresponding theoretical melting point of a specific aluminum-scandium alloy target. Table 1 records the composition information, theoretical melt, and corresponding casting temperature (i.e., the theoretical melting point plus 90-110°C mentioned in this invention) of some commonly used aluminum-scandium target blanks. The relationship between other scandium content information and theoretical melting point can be further obtained through analysis of the schematic diagram of the aluminum-scandium alloy binary phase diagram; and the corresponding curves are plotted, such as... Figure 2 As shown;

[0027] Table 1

[0028]

[0029]

[0030] Specifically, a schematic diagram for testing the melt temperature is shown below. Figure 3 As shown, the aluminum-scandium alloy target is placed in a water-cooled crucible within a suspension melting furnace. During the melting process, the state of the melt after complete melting is as follows. Figure 3 As shown, the temperature of the melt was measured using a thermometer within 20–50 seconds after complete melting, obtaining the corresponding melt temperature, which is also the casting temperature in the subsequent target preparation process. Then, the obtained melt temperature was compared with the casting temperature. If it fell within the range of the casting temperature, the scandium content corresponding to the theoretical melting point of the casting temperature was the actual scandium content value in the tested aluminum-scandium alloy target. Table 1 and... Figure 2 The table only lists some of the scandium content values; other specific values ​​can be obtained through analysis of the binary phase diagram.

[0031] Example 1

[0032] This invention provides a method for detecting the composition of an aluminum-scandium alloy target. The method includes the following steps: 5.4 kg of an aluminum-scandium alloy target with a nominal scandium content of 15 wt% is placed in a water-cooled crucible in a suspension melting furnace. Vacuum is activated, followed by the introduction of argon gas. The power is adjusted from 250 kW / min to 500 kW for melting. It is observed that the oxide scale is completely broken and the melt is completely melted at 330 s during melting. The melt temperature is tested at 30 s after complete melting, and the corresponding melt temperature is recorded.

[0033] Example 2

[0034] The only difference between this embodiment and Embodiment 1 is that the aluminum-scandium alloy target is cut into pieces with a diameter of 1-5 cm before being placed in the water-cooled crucible in the suspension melting furnace.

[0035] Example 3

[0036] The only difference between this embodiment and Embodiment 1 is that the power is adjusted from 300 kW / min to 500 kW for smelting.

[0037] Example 4

[0038] The only difference between this embodiment and Embodiment 1 is that the power is adjusted from 200 kW / min to 500 kW for smelting.

[0039] Comparative Example 1

[0040] The only difference between the comparative example and Example 1 is that the power is adjusted from 100 kW / min to 500 kW for smelting.

[0041] Comparative Example 2

[0042] The only difference between the comparative example and Example 4 is that the power is adjusted to 500 kW at a speed of 500 kW / min for smelting.

[0043] Comparative Example 3

[0044] The only difference between the comparative example and Example 4 is that the power was adjusted from 250 kW / min to 100 kW for smelting.

[0045] Comparative Example 4

[0046] The only difference between the comparative example and Example 1 is that the power was adjusted from 250 kW / min to 700 kW for smelting.

[0047] Comparative Example 5

[0048] The only difference between the comparative example and Example 1 is that the melt temperature was tested at 60 seconds after complete melting.

[0049] Comparative Example 6

[0050] The only difference between the comparative example of this invention and Example 1 is that the melt temperature was tested 2 seconds after complete melting.

[0051] Example of effect

[0052] This example records the melt temperature obtained in Examples 1-4 and Comparative Examples 1-6, and the corresponding scandium content in the aluminum-scandium alloy target determined based on the melt temperature, and compares it with the content obtained by ICP-OES testing; wherein the scandium content in the aluminum-scandium alloy target used in this invention, as determined by ICP-OES testing, is 15 wt%; specifically, the deviation is calculated as follows: deviation = |(scandium content value obtained by this invention) - (scandium content value obtained by ICP-OES testing)|; the specific results are shown in Table 2;

[0053] Table 2

[0054]

[0055]

[0056] As can be seen from Table 2, the detection method obtained by adopting the technical solution of the present invention has a small deviation, with the deviation value being within 0.4wt%, which can meet the control of the deviation of scandium component content in aluminum-scandium alloy targets in production.

[0057] As can be seen from Examples 1, 3-4 and Comparative Examples 1-4, changing the speed of power adjustment or the final power value will affect the accuracy of the detection method. When the selected power adjustment speed and the final power adjustment are not within the range given by the present invention, the test results of the detection method deviate significantly from the results obtained by the conventional method. In particular, when the final power is not within the range of the present invention, the deviation reaches 1 wt%.

[0058] As can be seen from Example 1 and Comparative Examples 5-6, the choice of the testing time point is also extremely important. If the temperature test is performed shortly after full melting or long after full melting, the accuracy of the detection method will be significantly reduced.

[0059] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of the present invention and not to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for detecting the composition of an aluminum-scandium alloy target, characterized in that, The detection method includes the following steps: placing the aluminum-scandium alloy target in a suspension melting furnace, and adjusting the power to 350-550 kW at a speed of 200-300 kW / min for melting; testing the melt temperature within 20-50 seconds after the aluminum-scandium alloy target is fully melted, recording the corresponding melt temperature, and comparing it with the theoretical melting point of the aluminum-scandium alloy target to obtain the composition information of the aluminum-scandium alloy target; The process of comparing the theoretical melting point of the aluminum-scandium alloy sputtering target is as follows: add 90~110℃ to the theoretical melting point to obtain the corresponding temperature range. If the measured melt temperature is within the obtained temperature range, then the scandium content in the aluminum-scandium alloy sputtering target is the scandium content value corresponding to the theoretical melting point.

2. The method for detecting the composition of the aluminum-scandium alloy target material according to claim 1, characterized in that, The detection method includes the following steps: placing the aluminum-scandium alloy target in a suspension melting furnace and adjusting the power to 500 kW at a speed of 250 kW / min for melting; testing the melt temperature within 30 seconds after the aluminum-scandium alloy target is fully melted; recording the corresponding melt temperature; and comparing it with the theoretical melting point of the aluminum-scandium alloy target to obtain the composition information of the aluminum-scandium alloy target.

3. The method for detecting the composition of the aluminum-scandium alloy target material according to claim 1, characterized in that, The melting time is 5-6 minutes.

4. The method for detecting the composition of the aluminum-scandium alloy target material according to claim 1, characterized in that, Before placing the aluminum-scandium alloy target in the suspension melting furnace, the process also includes the step of cutting the aluminum-scandium alloy target into pieces.

5. The method for detecting the composition of the aluminum-scandium alloy target material according to claim 4, characterized in that, The shearing process involves cutting the aluminum-scandium alloy target into pieces with a diameter of 1-5 cm.

6. The application of the method for detecting the composition of aluminum-scandium alloy target material as described in any one of claims 1 to 5 in the preparation of aluminum-scandium target blanks.

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