A tellurium target, a preparation method and application thereof

Abstract

The present disclosure provides a tellurium target and a preparation method and application thereof, and belongs to the technical field of target material preparation. The preparation method of the tellurium target comprises the following steps: S1: a mold containing a tellurium block is loaded into a crucible, vacuum sealing is performed, and the obtained crucible is placed in a vertical heating furnace; S2: then heating to 600-700 DEG C, heat preservation for 30-90 min; S3: after the heat preservation is completed, the crucible is rotated at a rotation speed of 5-10 r / min and cooled to room temperature at a cooling rate of 0.05-0.5 mm / min, thereby obtaining the tellurium target. The present disclosure controls the temperature, time, rotation speed and cooling rate of heat preservation to obtain a tellurium target with high density, thereby improving the electrical conductivity, thermal conductivity and strength of the tellurium target.

Description

Technical Field

[0001] This disclosure relates to a method for preparing a target material, specifically a tellurium target and its preparation method and application. Background Technology

[0002] The shift of high-tech materials from bulk materials to thin films has led to the rapid development of coated devices. Sputtering is one of the main techniques for preparing thin film materials. Sputtering involves bombarding a solid surface with accelerated ions, causing the ions to exchange momentum with atoms on the solid surface, resulting in the atoms leaving the solid and depositing onto the substrate. The bombarded solid is the source material used for sputtering to deposit the thin film, and is usually called the target.

[0003] Tellurium has two allotropes: amorphous tellurium, which is a black powder, and crystalline tellurium, which is silvery-white, has a metallic luster, and a hexagonal crystal system. It is an important semiconductor with a bandgap of 0.34 eV, and is mainly used in metallurgy, electronics, chemical industry, and glass production. For tellurium sputtering targets, density is a crucial factor affecting quality: high-density targets have advantages such as good electrical and thermal conductivity, and high strength. Using such targets for film deposition results in low sputtering power, high film formation rate, less film cracking, long target life, and low resistivity and high light transmittance in the sputtered film.

[0004] Due to the low melting point of tellurium, the hot pressing temperature cannot be too high in the powder vacuum hot pressing method, so high-density targets cannot be obtained. The casting method is difficult to remove pores, which also leads to low density of the target material. The relative density of tellurium targets prepared by the above two methods is about 94-97%. Summary of the Invention

[0005] The purpose of this disclosure is to overcome the shortcomings of the prior art and provide a tellurium target, its preparation method and application.

[0006] To achieve the above objectives, the technical solution adopted in this disclosure is as follows: Firstly, a method for preparing a tellurium target is provided, comprising the following steps:

[0007] S1: The mold containing the tellurium block is placed into the crucible, vacuum sealed, and the resulting crucible is placed in a vertical heating furnace;

[0008] S2: Then heat to 600-700℃ and keep warm for 30-90 minutes;

[0009] S3: After the heat preservation is completed, the crucible is cooled to room temperature at a rotation speed of 5-10 r / min and a cooling rate of 0.05-0.5 mm / min to obtain the tellurium target.

[0010] In one embodiment, the insulation temperature is 620-650°C.

[0011] In one embodiment, the heat preservation time is 40-60 minutes.

[0012] In one embodiment, the cooling rate is 0.1-0.3 mm / min.

[0013] In one embodiment, the rotational speed is 6-8 r / min.

[0014] In one embodiment, the heating rate is 3-5°C / min.

[0015] In one embodiment, the mold is a graphite mold.

[0016] In one embodiment, the purity of the tellurium block is 5N.

[0017] On the other hand, a tellurium target is provided, which is prepared by the tellurium target preparation method described above.

[0018] On the other hand, the application of the aforementioned tellurium target in the preparation of thin film materials is provided.

[0019] Compared with the prior art, the beneficial effects of this disclosure are as follows: This disclosure uses the crucible falling melting method to prepare tellurium targets, and improves the density conductivity, thermal conductivity and strength of tellurium targets by selecting specific parameters. Detailed Implementation

[0020] To better illustrate the purpose, technical solutions, and advantages of this disclosure, the following description, in conjunction with specific embodiments and comparative examples, aims to provide a detailed understanding of the content of this disclosure, rather than limiting it. All other embodiments obtained by those skilled in the art without inventive effort are within the scope of protection of this disclosure. Unless otherwise specified, the experimental reagents and instruments involved in the implementation of this disclosure are all commonly used reagents and instruments.

[0021] In a first aspect, a method for preparing a tellurium target is provided, comprising the following steps:

[0022] S1: The mold containing the tellurium block is placed into the crucible, vacuum sealed, and the resulting crucible is placed in a vertical heating furnace;

[0023] S2: Then heat to 600-700℃ and keep warm for 30-90 minutes;

[0024] S3: After the heat preservation is completed, the crucible is cooled to room temperature at a rotation speed of 5-10 r / min and a cooling rate of 0.05-0.5 mm / min to obtain the tellurium target.

[0025] This disclosure employs a crucible melting and falling method to prepare tellurium targets, and obtains high-density tellurium targets by controlling the holding temperature, time, rotation speed, and cooling rate, thereby improving the electrical conductivity, thermal conductivity, and strength of the tellurium targets.

[0026] In this document, the heat preservation temperature can be, but is not limited to, 600℃, 605℃, 610℃, 615℃, 620℃, 625℃, 630℃, 635℃, 640℃, 645℃, 650℃, 655℃, 660℃, 665℃, 670℃, 675℃, 680℃, 685℃, 690℃, 695℃, or 700℃. The heat preservation time can be, but is not limited to, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, 65 min, 70 min, 75 min, 80 min, 85 min, or 90 min.

[0027] In this study, when the holding temperature is below 600℃ or the holding time is less than 30 minutes, the tellurium block cannot completely melt. During the cooling process, the tellurium target contains solid matter, leading to a decrease in its density. While holding temperatures above 700℃ or holding times above 90 minutes have no significant impact on the tellurium target density, it results in resource waste. Setting the temperature to 600-700℃ and holding for 30-90 minutes ensures complete melting of the tellurium block. Furthermore, when the holding temperature is 620-650℃ or the holding time is 40-60 minutes, the resulting tellurium target has an even higher density.

[0028] In this document, the cooling rate can be 0.05 mm / min, 0.08 mm / min, 0.1 mm / min, 0.13 mm / min, 0.15 mm / min, 0.17 mm / min, 0.2 mm / min, 0.22 mm / min, 0.25 mm / min, 0.28 mm / min, 0.3 mm / min, 0.33 mm / min, 0.35 mm / min, 0.38 mm / min, 0.4 mm / min, 0.42 mm / min, 0.45 mm / min, 0.47 mm / min, or 0.5 mm / min, but this disclosure is not limited to these rates. When the cooling rate is less than 0.05 mm / min, the preparation efficiency of the tellurium target decreases significantly. When the cooling rate is greater than 0.5 mm / min, the excessively rapid cooling prevents gas from escaping from the melt, leading to pores or uneven surfaces in the tellurium target. Furthermore, the excessively rapid cooling rate prevents the pressure generated by heating from being fully released from the tellurium target, resulting in cracks. Therefore, both factors reduce the density of the tellurium target. This paper preferably uses a cooling rate of 0.1-0.3 mm / min to obtain a tellurium target with high density.

[0029] In this paper, the rotation speed can be, but is not limited to, 5 r / min, 5.3 r / min, 5.5 r / min, 5.7 r / min, 6 r / min, 6.3 r / min, 6.5 r / min, 6.8 r / min, 7 r / min, 7.2 r / min, 7.5 r / min, 7.7 r / min, 8 r / min, 8.3 r / min, 8.5 r / min, 8.9 r / min, 9 r / min, 9.1 r / min, 9.4 r / min, 9.7 r / min, and 10 r / min.

[0030] In this document, the heating rate can be, but is not limited to, 3.0℃ / min, 3.1℃ / min, 3.2℃ / min, 3.3℃ / min, 3.4℃ / min, 3.5℃ / min, 3.6℃ / min, 3.7℃ / min, 3.8℃ / min, 3.9℃ / min, 4.0℃ / min, 4.1℃ / min, 4.2℃ / min, 4.3℃ / min, 4.4℃ / min, 4.5℃ / min, 4.6℃ / min, 4.7℃ / min, 4.8℃ / min, 4.9℃ / min, or 5.0℃ / min.

[0031] In one embodiment, the mold is a graphite mold.

[0032] In one embodiment, the mold is a square mold or a round mold.

[0033] In one embodiment, the purity of the tellurium block is 5N.

[0034] In one embodiment, the crucible is a quartz crucible.

[0035] On the other hand, a tellurium target is provided, which is prepared by the tellurium target preparation method described above.

[0036] On the other hand, the application of the aforementioned tellurium target in the preparation of thin film materials is provided.

[0037] The molds used in the following examples and comparative examples are the same.

[0038] Example 1

[0039] This embodiment provides a method for preparing a tellurium target, including the following steps:

[0040] S1: Put 5N tellurium blocks into a circular mold, put the mold containing the tellurium blocks into a quartz crucible, vacuum seal it, and place the resulting crucible in a vertical heating furnace with the crucible placed vertically.

[0041] S2: Then heat to 650℃ at a heating rate of 5℃ / min and hold for 30min;

[0042] S3: After the heat preservation is completed, the crucible is rotated at a speed of 10 r / min and cooled to room temperature at a cooling rate of 0.2 mm / min. After cooling, the quartz crucible is broken, the tellurium billet is taken out of the mold, and then machined to obtain the tellurium target.

[0043] Example 2

[0044] This embodiment provides a method for preparing a tellurium target, including the following steps:

[0045] S1: Put 5N tellurium blocks into a circular mold, put the mold containing the tellurium blocks into a quartz crucible, vacuum seal it, and place the resulting crucible in a vertical heating furnace with the crucible placed vertically.

[0046] S2: Then heat to 600℃ at a heating rate of 3℃ / min and hold for 90min;

[0047] S3: After the heat preservation is completed, the crucible is rotated at a speed of 5 r / min and cooled to room temperature at a cooling rate of 0.05 mm / min. After cooling, the quartz crucible is broken, the tellurium billet is taken out from the mold, and then machined to obtain the tellurium target.

[0048] Example 3

[0049] This embodiment provides a method for preparing a tellurium target, including the following steps:

[0050] S1: Put 5N tellurium blocks into a circular mold, put the mold containing the tellurium blocks into a quartz crucible, vacuum seal it, and place the resulting crucible in a vertical heating furnace with the crucible placed vertically.

[0051] S2: Then heat to 620℃ at a heating rate of 4℃ / min and hold for 50min;

[0052] S3: After the heat preservation is completed, the crucible is rotated at a speed of 8r / min and cooled to room temperature at a cooling rate of 0.1mm / min. After cooling, the quartz crucible is broken, the tellurium billet is taken out from the mold, and then machined to obtain the tellurium target.

[0053] Example 4

[0054] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the heat preservation temperature is 650℃.

[0055] Example 5

[0056] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the heat preservation temperature is 700℃.

[0057] Example 6

[0058] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the heat preservation temperature is 600℃.

[0059] Example 7

[0060] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the heat preservation time is 60 minutes.

[0061] Example 8

[0062] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the heat preservation time is 40 minutes.

[0063] Example 9

[0064] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the heat preservation time is 30 minutes.

[0065] Example 10

[0066] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in Embodiment 3 is that the cooling rate is 0.3 mm / min.

[0067] Example 11

[0068] This embodiment provides a method for preparing a tellurium target. The only difference between the method for preparing the tellurium target in this embodiment and that in embodiment 3 is that the cooling rate is 0.5 mm / min.

[0069] Comparative Example 1

[0070] This comparative example provides a method for preparing a tellurium target. The only difference between this comparative example and Example 3 is that the heat preservation temperature is 550°C.

[0071] Comparative Example 2

[0072] This comparative example provides a method for preparing a tellurium target. The only difference between this comparative example and Example 3 is that the heat preservation time is 25 min.

[0073] Comparative Example 3

[0074] This comparative example provides a method for preparing a tellurium target. The only difference between this comparative example and Example 3 is that the cooling rate is 0.6 mm / min.

[0075] Comparative Example 4

[0076] This comparative example provides a method for preparing a tellurium target, including the following steps:

[0077] S1: Place the 5N tellurium block into a circular mold, place the mold containing the tellurium block into a quartz crucible, vacuum seal it, and place the resulting crucible in a horizontal heating furnace with the crucible placed horizontally.

[0078] S2: Then heat to 620℃ at a heating rate of 4℃ / min and hold for 50min;

[0079] S3: After the heat preservation is completed, the crucible is rotated at a speed of 8r / min and cooled to room temperature at a cooling rate of 0.1mm / min. After cooling, the quartz crucible is broken, the tellurium billet is taken out from the mold, and then machined to obtain the tellurium target.

[0080] Performance testing: The relative density of the tellurium targets obtained in each embodiment and comparative example was tested using the Archimedes displacement method. The test results are shown in Table 1 below.

[0081] Table 1

[0082]

[0083]

[0084] As shown in Table 1, the tellurium target in this paper has a high relative density.

[0085] Comparing Examples 3-6 and Comparative Example 1, it can be seen that the insulation temperature affects the relative density of the tellurium target. When the insulation temperature is 620-650℃, the relative density of the tellurium target is higher.

[0086] Comparing Examples 3, 7-9 and Comparative Example 2, it can be seen that the holding time affects the relative density of the tellurium target. When the holding time is 40-60 min, the relative density of the tellurium target is higher.

[0087] Comparing Examples 3, 10-11 and Comparative Example 3, it can be seen that the cooling rate affects the relative density of the tellurium target. When the cooling rate is 0.1-0.3 mm / min, the relative density of the tellurium target is higher.

[0088] Comparing Example 3 and Comparative Example 4, it can be seen that the relative density of the tellurium target obtained by horizontal sintering is significantly reduced.

[0089] Finally, it should be noted that the above embodiments are used to illustrate the technical solutions of this disclosure and not to limit the scope of protection of this disclosure. Although this disclosure 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 this disclosure without departing from the substance and scope of the technical solutions of this disclosure.

Claims

1. A method for preparing a tellurium target, characterized in that, Includes the following steps: S1: The mold containing the tellurium block is placed into the crucible, vacuum sealed, and the resulting crucible is placed in a vertical heating furnace; S2: Then heat to 600-700℃ and keep warm for 30-90 minutes; S3: After the heat preservation is completed, the crucible is cooled to room temperature at a rotation speed of 5-10 r / min and a cooling rate of 0.1-0.5 mm / min to obtain the tellurium target.

2. The preparation method according to claim 1, characterized in that, The insulation temperature is 620-650℃.

3. The preparation method according to claim 1, characterized in that, The heat preservation time is 40-60 minutes.

4. The preparation method according to claim 1, characterized in that, The cooling rate is 0.1-0.3 mm / min.

5. The preparation method according to claim 1, characterized in that, The rotational speed is 6-8 r / min.

6. The preparation method according to claim 1, characterized in that, The heating rate is 3-5℃ / min.

7. The preparation method according to claim 1, characterized in that, The mold is a graphite mold.

8. The preparation method according to claim 1, characterized in that, The purity of the tellurium block is 5N.

9. A tellurium target, characterized in that, The tellurium target is prepared using the tellurium target preparation method as described in any one of claims 1-8.

10. The use of the tellurium target as described in claim 9 in the preparation of thin film materials.

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