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Application of Zirconia Grinding Balls in Molybdenum-Niobium Alloy Sputtering Targets

Sep 11,2023
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(1) Molybdenum powder and niobium powder (both with a purity of ≥99.95% and particle sizes of 20μm and 35μm, respectively) were loaded into a ball mill in a weight ratio of 6:1. Palmic acid and zirconia grinding balls (2mm in diameter) were added, and milling was conducted under argon protection. The milling time was 80 minutes, and the milling speed was 1000r/min. After sieving, composite powder with a particle size of 9μm of molybdenum-niobium alloy was obtained. The weight of palmic acid and zirconia grinding balls was 0.02 times the total weight of molybdenum powder and niobium powder, and 8 times, respectively.

(2) The molybdenum-niobium alloy composite powder from step (1) was cold isostatically pressed at a pressure of 200MPa for 5 minutes to obtain a pressed blank.

(3) The pressed blank was sintered in a vacuum sintering furnace at a temperature of 1800°C for 10 hours to obtain a target blank.

(4) The target blank was subjected to mechanical processing to produce molybdenum-niobium alloy sputtering targets. The sputtering targets had a single-phase microstructure, uniform without pores, an average grain size of 50μm, and a density of 9.85g/cm³.

[0023] Example 2

A process for preparing molybdenum-niobium alloy sputtering targets, comprising the following steps:

(1) Molybdenum powder and niobium powder (both with a purity of ≥99.95% and particle sizes of 15μm and 30μm, respectively) were loaded into a ball mill in a weight ratio of 7:1. Zinc stearate and zirconia grinding balls (3mm in diameter) were added, and milling was conducted under argon protection. The milling time was 60 minutes, and the milling speed was 1200r/min. After sieving, composite powder with a particle size of 10μm of molybdenum-niobium alloy was obtained. The weight of zinc stearate and zirconia grinding balls was 0.01 times the total weight of molybdenum powder and niobium powder, and 5 times, respectively.

(2) The molybdenum-niobium alloy composite powder from step (1) was subjected to vacuum treatment and then cold isostatically pressed at a pressure of 150MPa for 10 minutes to obtain a pressed blank.

(3) The pressed blank was sintered in a vacuum sintering furnace at a temperature of 2000°C for 5 hours to obtain a target blank.

(4) The target blank was subjected to mechanical processing to produce molybdenum-niobium alloy sputtering targets. The sputtering targets had a single-phase microstructure, uniform without pores (see Figure 1), an average grain size of 55μm, and a density of 9.86g/cm³.

[0024] Example 3

(1) Molybdenum powder and niobium powder (both with a purity of ≥99.95% and particle sizes of 25μm and 40μm, respectively) were loaded into a ball mill in a weight ratio of 8:1. Zinc stearate and zirconia grinding balls (1mm in diameter) were added, and milling was conducted under argon protection. The milling time was 100 minutes, and the milling speed was 1000r/min. After sieving, composite powder with a particle size of 6μm of molybdenum-niobium alloy was obtained. The weight of zinc stearate and zirconia grinding balls was 0.03 times the total weight of molybdenum powder and niobium powder, and 10 times, respectively.

(2) The molybdenum-niobium alloy composite powder from step (1) was subjected to vacuum treatment, followed by cold isostatic pressing at a pressure of 180MPa for 7 minutes to obtain a pressed blank.

(3) The pressed blank was sintered in a vacuum sintering furnace at a temperature of 2000°C for 8 hours to obtain a target blank.

(4) The target blank was subjected to mechanical processing to produce molybdenum-niobium alloy sputtering targets. The sputtering targets had a single-phase microstructure, uniform without pores (see Figure 2), an average grain size of 45μm, and a density of 9.87g/cm³.

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