A molybdenum-silicon alloy tubular target, its preparation method and application

By using molybdenum disilicide powder and silicon powder as raw materials, combined with ball milling and hot isostatic pressing, the problems of uniform composition of molybdenum-silicon target and preparation of large-size tubular target were solved, realizing the preparation of high-performance molybdenum-silicon alloy tubular target, meeting the application requirements of high-end photomasks.

CN122081871APending Publication Date: 2026-05-26KONFOONG MATERIALS INTERNATIONAL CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
KONFOONG MATERIALS INTERNATIONAL CO LTD
Filing Date
2026-02-27
Publication Date
2026-05-26

AI Technical Summary

Technical Problem

Existing molybdenum-silicon targets face technical bottlenecks in terms of compositional uniformity and the fabrication of large-size tubular targets, making it difficult to meet the application requirements of high-end photomasks.

Method used

Using molybdenum disilicide powder and silicon powder as raw materials, and controlling the particle size and purity, combined with ball milling and hot isostatic pressing, large-size molybdenum-silicon alloy tubular targets with high density and uniform phase distribution are prepared.

Benefits of technology

Large-size molybdenum-silicon alloy tubular targets with good internal uniformity and high density were prepared, which are suitable for high-end photomask applications. The length can reach 200~300mm, the diameter can reach 100~150mm, and the density can reach over 96%.

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Abstract

This invention relates to a molybdenum-silicon alloy tubular target, its preparation method, and its application. The preparation method includes the following steps: (1) mixing molybdenum disilicide powder and silicon powder to obtain a mixed powder; (2) sequentially subjecting the mixed powder to cladding welding, degassing treatment, and hot isostatic pressing treatment, and removing the cladding to obtain the molybdenum-silicon alloy tubular target. This invention uses molybdenum disilicide powder and silicon powder as raw materials to reduce the amount of silicon powder used, reduce the risk of product cracking, and decrease the difficulty of subsequent processing; and successfully prepares a large-size tubular molybdenum-silicon alloy target with high density and uniform phase distribution by combining hot isostatic pressing treatment.
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Description

Technical Field

[0001] This invention relates to the field of target preparation technology, and in particular to a molybdenum-silicon alloy tubular target, its preparation method, and its application. Background Technology

[0002] In the fields of semiconductor manufacturing, flat panel displays, and microelectronic devices, photomasks are the core component of photolithography processes, and their quality directly determines the accuracy of pattern transfer and the performance of the devices. With the continuous shrinking of integrated circuit feature sizes and the development of display panels towards higher resolutions, higher requirements are placed on the material properties of photomasks, especially low defect rates, high resistance to laser damage, and excellent dimensional stability. Traditional photomasks typically use chromium (Cr) as the absorber layer material, but it is prone to thermal deformation and film peeling under high-energy laser irradiation, and has limited compatibility with advanced photolithography technologies such as extreme ultraviolet (EUV). Therefore, molybdenum-silicon composite materials, due to their unique performance advantages, have gradually become an important candidate material for the absorber layer of photomasks.

[0003] Molybdenum-silicon targets, when sputtered, produce thin films with high absorption coefficients, low stress, good etch selectivity, and excellent resistance to laser damage, making them particularly suitable for ArF excimer laser (193nm) and EUV (13.5nm) lithography technologies. Furthermore, the good chemical stability of molybdenum-silicon films reduces contamination during the manufacturing process, and their uniform microstructure facilitates the precise transfer of nanoscale patterns, thus meeting the manufacturing requirements for process nodes below 5nm and high-resolution display panels.

[0004] However, existing molybdenum-silicon targets still face technical bottlenecks in terms of compositional uniformity, and the preparation of large-size tubular molybdenum-silicon alloy targets is even more difficult. There is currently little research on this topic, and there is an urgent need to optimize the target preparation process to further improve film performance and target utilization.

[0005] CN105483624A discloses a method for manufacturing a molybdenum-silicon target. The method includes: providing molybdenum powder and silicon powder; mixing the molybdenum powder and silicon powder using a mixing process to form a mixed powder; using a cold pressing process to form a molybdenum-silicon target blank; and using a vacuum hot pressing sintering process to form a molybdenum-silicon target. The manufacturing method using this scheme can obtain molybdenum-silicon targets with high density, but it is only applicable to planar circular molybdenum-silicon targets and has certain limitations for preparing large-size tubular molybdenum-silicon targets.

[0006] In summary, there is a need to develop a method for preparing molybdenum-silicon alloy tubular targets so that the prepared molybdenum-silicon alloy tubular targets can meet the application requirements of high-end photomasks. Summary of the Invention

[0007] To address the aforementioned technical problems, this invention provides a molybdenum-silicon alloy tubular target, its preparation method, and its application. By using molybdenum disilicide powder and silicon powder as raw materials, reducing the amount of silicon powder used, and combining hot isostatic pressing treatment, a large-size tubular molybdenum-silicon alloy target with high density and uniform phase distribution is prepared.

[0008] To achieve this objective, the present invention adopts the following technical solution: In a first aspect, the present invention provides a method for preparing a molybdenum-silicon alloy tubular target, the method comprising the following steps: (1) Mix molybdenum disilicide powder and silicon powder to obtain a mixed powder; (2) The mixed powder is subjected to encapsulation welding, degassing treatment and hot isostatic pressing treatment in sequence, and the molybdenum-silicon alloy tubular target is obtained after removing the encapsulation.

[0009] The low packing density and poor formability of silicon powder greatly increase the difficulty of preparing large-size molybdenum-silicon alloy tubular targets with high silicon content. This invention uses molybdenum disilicide powder and silicon powder as raw materials to reduce the amount of silicon powder used, thereby reducing the risk of product cracking and the difficulty of subsequent processing. In addition, the density difference between molybdenum disilicide and silicon is much smaller than the density difference between molybdenum and silicon. Using molybdenum disilicide powder and silicon powder as raw materials makes it easier to mix them evenly, so as to prepare a target with better microstructure and phase uniformity.

[0010] As a preferred technical solution of the present invention, the molar ratio of molybdenum disilicide powder and silicon powder in step (1) is 1:(1~4), for example, it can be 1:1, 1.5, 1:2, 1:2.5, 1:3, 1:3.5 or 1:4, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0011] Preferably, the particle size of the molybdenum disilicide powder is 10~15μm, for example, it can be 10μm, 11μm, 12μm, 13μm, 14μm or 15μm, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0012] Preferably, the purity of the molybdenum disilicide powder is ≥99.95%, for example, it can be 99.95%, 99.96%, 99.97%, 99.98% or 99.99%, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0013] Preferably, the particle size of the silicon powder is 20~25μm, for example, it can be 20μm, 21μm, 22μm, 23μm, 24μm or 25μm, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0014] Preferably, the purity of the silicon powder is ≥99.999%, for example, it can be 99.999%, 99.9992%, 99.9994%, 99.9996% or 99.9998%, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0015] This invention improves the mixing uniformity and packing density of the mixed powder by selecting the particle size and reasonable gradation of the two raw material powders, reduces the dimensional shrinkage rate during sintering, and successfully prepares a large-size tubular molybdenum-silicon alloy target with high density and uniform phase distribution by hot isostatic pressing.

[0016] As a preferred embodiment of the present invention, the mixing is carried out in a ball mill.

[0017] Preferably, the rotational speed of the ball mill is 10~15 r / min, for example, it can be 10 r / min, 11 r / min, 12 r / min, 13 r / min, 14 r / min or 15 r / min, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0018] Preferably, the ball milling time is 24 to 48 hours, for example, 24 hours, 30 hours, 36 hours, 42 hours or 48 hours, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0019] Preferably, the diameter of the grinding balls used in the ball milling process is 10~25mm, for example, it can be 10mm, 15mm, 20mm or 25mm, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0020] In this invention, zirconium oxide balls of different diameters are used to ball mill and mix molybdenum disilicide powder and silicon powder to increase the mixing effect of molybdenum disilicide powder and silicon powder and improve the mixing uniformity.

[0021] Preferably, the ratio of the mass of the grinding ball to the total mass of the molybdenum disilicide powder and silicon powder is 1:(2~4), for example, it can be 1:2, 1:2.5, 1:3, 1:3.5 or 1:4, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0022] As a preferred technical solution of the present invention, the sheath welding is performed using a tubular stainless steel sheath.

[0023] Preferably, the temperature of the degassing treatment is 300~400℃, for example, it can be 300℃, 320℃, 340℃, 360℃, 380℃ or 400℃, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0024] As a preferred technical solution of the present invention, the temperature of the hot isostatic pressing treatment is 750~950℃, for example, it can be 750℃, 800℃, 850℃, 900℃ or 950℃, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0025] This invention aims to prepare large-sized tubular molybdenum-silicon alloy targets with high density and uniform phase distribution by limiting the hot isostatic pressing (HIP) temperature to 750~950℃. If the HIP temperature is less than 750℃, insufficient diffusion between powder particles will result in the inability to completely eliminate porosity, leading to low density of the target material. At the same time, the reaction between molybdenum disilicide powder and silicon powder will be incomplete, resulting in uneven target composition, weak grain boundary bonding, high brittleness of the target material, and easy breakage during subsequent processing. If the HIP temperature is greater than 950℃, the high temperature will accelerate grain boundary migration, forming coarse grains, which will increase the brittleness of the target material.

[0026] Preferably, the pressure of the hot isostatic pressing treatment is 90~120MPa, for example, it can be 90MPa, 100MPa, 110MPa or 120MPa, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0027] This invention aims to prepare large-sized tubular molybdenum-silicon alloy targets with high density and uniform phase distribution by limiting the hot isostatic pressing (HIP) pressure to 90-120 MPa. If the HIP pressure is less than 90 MPa, the bonding between particles will be insufficient, and the pores will not be completely closed, resulting in low density of the target. At the same time, the reaction between molybdenum disilicide powder and silicon powder will be incomplete, resulting in uneven composition of the target. Furthermore, local sintering under low pressure will lead to a wide grain size distribution, affecting the thermal shock stability of the target. If the HIP pressure is greater than 120 MPa, the excessive pressure may cause grain crushing or abnormal growth, affecting the mechanical properties of the target.

[0028] Preferably, the hot isostatic pressing treatment time is 4 to 8 hours, for example, it can be 4 hours, 5 hours, 6 hours, 7 hours or 8 hours, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0029] As a preferred technical solution of the present invention, the method of removing the casing includes plasma cutting and / or machining.

[0030] Preferably, the machining includes any one or a combination of at least two of turning, milling, or grinding, wherein typical but non-limiting combinations include: a combination of turning and milling, a combination of turning and grinding, a combination of milling and grinding, and a combination of turning, milling, and grinding.

[0031] As a preferred technical solution of the present invention, the preparation method includes the following steps: (1) Molybdenum disilicide powder and silicon powder are mixed in a molar ratio of 1:(1~4) in a ball mill at a speed of 10~15 r / min for 24~48 h to obtain a mixed powder; wherein the particle size of the molybdenum disilicide powder is 10~15 μm and the purity is ≥99.95%; the particle size of the silicon powder is 20~25 μm and the purity is ≥99.999%; (2) The mixed powder is subjected to encapsulation welding, degassing treatment at a temperature of 300~400℃ and hot isostatic pressing treatment at a temperature of 750~950℃, a pressure of 90~120MPa and a time of 4~8h in sequence. After removing the encapsulation, the molybdenum-silicon alloy tubular target is obtained.

[0032] In a second aspect, the present invention provides a molybdenum-silicon alloy tubular target, which is prepared by the preparation method described in the first aspect.

[0033] The molybdenum-silicon alloy tubular target provided by this invention has good internal uniformity and high density, and can be made into large-size tubular targets, meeting the high-performance requirements of tubular targets.

[0034] As a preferred technical solution of the present invention, the molar ratio of molybdenum to silicon in the molybdenum-silicon alloy tubular target is 1:(3~6), for example, it can be 1:3, 1:4, 1:5 or 1:6, but it is not limited to the listed values. Other unlisted values ​​within the above range are also applicable.

[0035] Thirdly, the present invention provides an application of the molybdenum-silicon alloy tubular target according to the second aspect, wherein the molybdenum-silicon alloy tubular target is used as a photomask.

[0036] Using the aforementioned molybdenum-silicon alloy tubular target as raw material, a photomask can be prepared, which can meet the application requirements of high-end photomasks.

[0037] Compared with the prior art, the present invention has at least the following beneficial effects: This invention uses molybdenum disilicide powder and silicon powder as raw materials, reducing the amount of silicon powder used, lowering the risk of product cracking and the difficulty of subsequent processing; and combines hot isostatic pressing to prepare large-size tubular molybdenum-silicon alloy targets with high density and uniform phase distribution. The length of the tubular molybdenum-silicon alloy targets can reach 200~300mm and the diameter can reach 100~150mm, and the density of the molybdenum-silicon alloy targets can reach more than 96%. Attached Figure Description

[0038] Figure 1 This is a process flow diagram for preparing molybdenum-silicon alloy tubular targets provided in Embodiment 1 of the present invention. Detailed Implementation

[0039] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments. However, the following examples are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention is determined by the claims.

[0040] Example 1 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target, see [link to documentation]. Figure 1 The preparation method includes the following steps: (1) Molybdenum disilicide powder and silicon powder are mixed in a molar ratio of 1:2. The mixing is carried out in a ball mill at a speed of 12 r / min for 36 h to obtain the mixed powder. The molybdenum disilicide powder has a particle size of 12 μm and a purity of 99.98%; the silicon powder has a particle size of 22 μm and a purity of 99.999%; the grinding balls used in the ball milling process include zirconia balls with diameters of 10 mm, 20 mm and 25 mm, with a mass ratio of 1:2.5:2.5, and the mass ratio of the grinding balls to the total mass of the molybdenum disilicide powder and silicon powder is 1:3. (2) The mixed powder is subjected to encapsulation welding, degassing at 350°C and hot isostatic pressing at 850°C, 100MPa and 7h, and the encapsulation is removed by plasma cutting to obtain the molybdenum-silicon alloy tubular target; the molar ratio of molybdenum to silicon in the molybdenum-silicon alloy tubular target is 1:4. The sheath welding is performed using a tubular stainless steel sheath.

[0041] Example 2 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target, the method comprising the following steps: (1) Molybdenum disilicide powder and silicon powder are mixed in a molar ratio of 1:1. The mixing is carried out in a ball mill at a speed of 15 r / min for 24 h to obtain the mixed powder. The molybdenum disilicide powder has a particle size of 15 μm and a purity of 99.95%; the silicon powder has a particle size of 25 μm and a purity of 99.9994%; the grinding balls used in the ball milling process include zirconia balls with diameters of 10 mm, 20 mm and 25 mm, with a mass ratio of 1:2:3, and the mass ratio of the grinding balls to the total mass of the molybdenum disilicide powder and silicon powder is 1:2. (2) The mixed powder is subjected to encapsulation welding, degassing at 300°C and hot isostatic pressing at 950°C, 120MPa and 4h, and the encapsulation is removed by turning to obtain the molybdenum-silicon alloy tubular target; the molar ratio of molybdenum to silicon in the molybdenum-silicon alloy tubular target is 1:3. The sheath welding is performed using a tubular stainless steel sheath.

[0042] Example 3 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target, the method comprising the following steps: (1) Molybdenum disilicide powder and silicon powder are mixed in a molar ratio of 1:4. The mixing is carried out in a ball mill at a speed of 10 r / min for 48 h to obtain the mixed powder. The molybdenum disilicide powder has a particle size of 10 μm and a purity of 99.99%; the silicon powder has a particle size of 20 μm and a purity of 99.9998%; the grinding balls used in the ball milling process include zirconia balls with diameters of 10 mm, 20 mm and 25 mm, with a mass ratio of 1:3:2, and the mass ratio of the grinding balls to the total mass of the molybdenum disilicide powder and silicon powder is 1:4. (2) The mixed powder is subjected to encapsulation welding, degassing at 400°C and hot isostatic pressing at 750°C, 90MPa and 8h, and the encapsulation is removed by grinding to obtain the molybdenum-silicon alloy tubular target; the molar ratio of molybdenum to silicon in the molybdenum-silicon alloy tubular target is 1:6. The sheath welding is performed using a tubular stainless steel sheath.

[0043] Example 4 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the molar ratio of molybdenum disilicide powder and silicon powder mixed in step (1) is adjusted from 1:2 to 1:0.5, that is, the molar ratio of molybdenum to silicon in the prepared molybdenum-silicon alloy tubular target is 1:2.5. All other aspects are the same as in Embodiment 1.

[0044] Example 5 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the molar ratio of molybdenum disilicide powder and silicon powder mixed in step (1) is adjusted from 1:2 to 1:6, that is, the molar ratio of molybdenum to silicon in the prepared molybdenum-silicon alloy tubular target is 1:8. All other aspects are the same as in Embodiment 1.

[0045] Example 6 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the particle size of molybdenum disilicide powder in step (1) is adjusted from 12 μm to 3 μm. All other aspects are the same as in Embodiment 1.

[0046] Example 7 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the particle size of molybdenum disilicide powder in step (1) is adjusted from 12 μm to 30 μm. All other aspects are the same as in Embodiment 1.

[0047] Example 8 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the particle size of the silicon powder in step (1) is adjusted from 22 μm to 5 μm. All other aspects are the same as in Embodiment 1.

[0048] Example 9 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the particle size of the silicon powder in step (1) is adjusted from 22 μm to 40 μm. All other aspects are the same as in Embodiment 1.

[0049] Example 10 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the temperature of the hot isostatic pressing treatment in step (2) is adjusted from 850°C to 700°C. All other aspects are the same as in Embodiment 1.

[0050] Example 11 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the temperature of the hot isostatic pressing treatment in step (2) is adjusted from 850°C to 1100°C. All other aspects are the same as in Embodiment 1.

[0051] Example 12 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the pressure of the hot isostatic pressing in step (2) is adjusted from 100MPa to 80MPa. All other aspects are the same as in Embodiment 1.

[0052] Example 13 This embodiment provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Embodiment 1 is that the pressure of the hot isostatic pressing in step (2) is adjusted from 100MPa to 150MPa. All other aspects are the same as in Embodiment 1.

[0053] Comparative Example 1 This comparative example provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Example 1 is that the molybdenum disilicide powder is replaced with a mixture of molybdenum powder and silicon powder with the same molybdenum and silicon content as the molybdenum disilicide powder. All other aspects are the same as in Example 1.

[0054] Comparative Example 2 This comparative example provides a method for preparing a molybdenum-silicon alloy tubular target. The only difference from Example 1 is that the hot isostatic pressing treatment is replaced by cold isostatic pressing treatment with the same pressure and time. All other aspects are the same as in Example 1.

[0055] The uniformity of phase distribution of the molybdenum-silicon alloy tubular targets prepared in Examples 1-13 and Comparative Examples 1-2 was detected by SEM. The uniformity was divided into three levels: "uniform", "relatively uniform" and "non-uniform".

[0056] The density of the molybdenum-silicon alloy tubular target was measured using the Archimedes displacement method. The density of the molybdenum-silicon alloy tubular target was then calculated using the formula: density (%) = measured density / theoretical density × 100%. The results are shown in Table 1.

[0057] Table 1 The test results show that: (1) As can be seen from Examples 1 to 3, the present invention uses molybdenum disilicide powder and silicon powder as raw materials, reduces the amount of silicon powder, and combines hot isostatic pressing to make the raw materials fully alloyed and the alloy phase and matrix evenly distributed, thus preparing a large-size tubular molybdenum-silicon alloy target with a density of up to 96%.

[0058] (2) As can be seen from Examples 1 and 4-9, the present invention improves the mixing uniformity and compaction density of the mixed powder by selecting the particle size and reasonable gradation of the two raw material powders, reduces the dimensional shrinkage rate during sintering, and successfully prepares a large-size tubular molybdenum-silicon alloy target material with high density and uniform phase distribution by hot isostatic pressing. If the particle size selection or gradation is unreasonable, the raw material reaction will be insufficient, and large particles of raw material will cause black spots on the product surface. The phase distribution is relatively uniform.

[0059] (3) As can be seen from Examples 1 and 10-11, the hot isostatic pressing temperature of step (2) in Example 1 is 850℃, and the molybdenum-silicon alloy tubular target material prepared therefrom has a uniform phase distribution and a density of 96%. The hot isostatic pressing temperature of step (2) in Example 10 is 700℃, and the molybdenum-silicon alloy tubular target material prepared therefrom has a relatively uniform phase distribution and a density of 83%. The hot isostatic pressing temperature of step (2) in Example 11 is 1100℃, and the molybdenum-silicon alloy tubular target material prepared therefrom has a relatively uniform phase distribution. With a density of 92%, it can be seen that by limiting the hot isostatic pressing (HIP) temperature to 750~950℃, this invention can prepare large-sized tubular molybdenum-silicon alloy targets with high density and uniform phase distribution. If the HIP temperature is too low, the diffusion between powder particles will be insufficient, and the porosity cannot be completely eliminated, resulting in low target density. At the same time, the reaction between molybdenum disilicide powder and silicon powder will be incomplete, resulting in uneven target composition. If the HIP temperature is too high, the high temperature will accelerate grain boundary migration, forming coarse grains, which will increase the brittleness of the target.

[0060] (4) As can be seen from Examples 1 and 12-13, the hot isostatic pressing pressure in step (2) of Example 1 is 100 MPa, and the molybdenum-silicon alloy tubular target material prepared therefrom has a uniform phase distribution and a density of 96%. In Example 12, the hot isostatic pressing pressure in step (2) is 80 MPa, and the molybdenum-silicon alloy tubular target material prepared therefrom has a relatively uniform phase distribution and a density of 81%. In Example 13, the hot isostatic pressing pressure in step (2) is 150 MPa, and the molybdenum-silicon alloy tubular target material prepared therefrom has a relatively uniform phase distribution. The density is 91%, indicating that by limiting the hot isostatic pressing (HIP) pressure to 90-120 MPa, this invention can prepare large-sized tubular molybdenum-silicon alloy targets with high density and uniform phase distribution. If the HIP pressure is too low, the bonding between particles will be insufficient and the pores will not be completely closed, resulting in low density of the target material. At the same time, the reaction between molybdenum disilicide powder and silicon powder will be incomplete, resulting in uneven composition of the target material. If the HIP pressure is too high, the excessive pressure may cause grain crushing or abnormal growth, affecting the mechanical properties of the target material.

[0061] (5) As can be seen from Example 1 and Comparative Examples 1-2, the present invention uses molybdenum disilicide powder and silicon powder as raw materials, and combines hot isostatic pressing to prepare a large-size tubular molybdenum-silicon alloy target with high density and uniform phase distribution.

[0062] In summary, this invention uses molybdenum disilicide powder and silicon powder as raw materials, and combines hot isostatic pressing to prepare large-size tubular molybdenum-silicon alloy targets with high density and uniform phase distribution. The length of the tubular molybdenum-silicon alloy targets can reach 200~300mm, the diameter can reach 100~150mm, and the density of the molybdenum-silicon alloy targets can reach more than 96%.

[0063] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for preparing a molybdenum-silicon alloy tubular target, characterized in that, The preparation method includes the following steps: (1) Mix molybdenum disilicide powder and silicon powder to obtain a mixed powder; (2) The mixed powder is subjected to encapsulation welding, degassing treatment and hot isostatic pressing treatment in sequence, and the molybdenum-silicon alloy tubular target is obtained after removing the encapsulation.

2. The preparation method according to claim 1, characterized in that, The molar ratio of molybdenum disilicide powder to silicon powder in step (1) is 1:(1~4); Preferably, the particle size of the molybdenum disilicide powder is 10~15μm; Preferably, the purity of the molybdenum disilicide powder is ≥99.95%; Preferably, the particle size of the silicon powder is 20~25μm; Preferably, the purity of the silicon powder is ≥99.999%.

3. The preparation method according to claim 1 or 2, characterized in that, The mixing is carried out in a ball mill; Preferably, the rotational speed of the ball mill is 10~15 r / min; Preferably, the ball milling time is 24~48 hours; Preferably, the diameter of the grinding balls used in the ball milling process is 10~25mm; Preferably, the ratio of the mass of the grinding ball to the total mass of the molybdenum disilicide powder and silicon powder is 1:(2~4).

4. The preparation method according to any one of claims 1-3, characterized in that, The sheath welding is performed using a tubular stainless steel sheath; Preferably, the temperature of the degassing treatment is 300~400℃.

5. The preparation method according to any one of claims 1-4, characterized in that, The temperature for hot isostatic pressing is 750~950℃; Preferably, the pressure of the hot isostatic pressing treatment is 90~120MPa; Preferably, the hot isostatic pressing treatment takes 4 to 8 hours.

6. The preparation method according to any one of claims 1-5, characterized in that, The methods for removing the casing include plasma cutting and / or machining; Preferably, the machining includes any one or a combination of at least two of turning, milling, or grinding.

7. The preparation method according to any one of claims 1-6, characterized in that, The preparation method includes the following steps: (1) Molybdenum disilicide powder and silicon powder are mixed in a molar ratio of 1:(1~4) in a ball mill at a speed of 10~15 r / min for 24~48 h to obtain a mixed powder; wherein the particle size of the molybdenum disilicide powder is 10~15 μm and the purity is ≥99.95%; the particle size of the silicon powder is 20~25 μm and the purity is ≥99.999%; (2) The mixed powder is subjected to encapsulation welding, degassing treatment at a temperature of 300~400℃ and hot isostatic pressing treatment at a temperature of 750~950℃, a pressure of 90~120MPa and a time of 4~8h in sequence. After removing the encapsulation, the molybdenum-silicon alloy tubular target is obtained.

8. A molybdenum-silicon alloy tubular target, characterized in that, The molybdenum-silicon alloy tubular target is prepared using the preparation method described in any one of claims 1-7.

9. The molybdenum-silicon alloy tubular target according to claim 8, characterized in that, The molar ratio of molybdenum to silicon in the molybdenum-silicon alloy tubular target is 1:(3~6).

10. An application of the molybdenum-silicon alloy tubular target according to claim 8 or 9, characterized in that, The molybdenum-silicon alloy tubular target is used as a photomask.

Citation Information

Patent Citations

  • Manufacturing method for molybdenum-silicon target and combination thereof

    CN105483624A