A method for preparing a large-size molybdenum-niobium planar target

Abstract

The invention discloses a method for preparing a large-size molybdenum-niobium planar target, which comprises 1) a powder granulation step, 2) a hot isostatic pressing step, 3) a thermal deformation step and a cleaning processing step. Through the preparation method of the present invention, a large-size target material with uniform structure composition, small average grain size, low oxygen content, high purity and high density is produced. The large-size target material prepared by the preparation method of the present invention meets the requirements of the sputtering target Material coating requirements.

Description

technical field

[0001] The invention relates to the technical field of metal target material production for coating sputtering in electronic industries such as liquid crystal displays, and in particular to a method for preparing a large-size molybdenum-niobium planar target material. Background technique

[0002] At present, molybdenum-niobium alloy, as the key material for making FPD, has been widely used in LCD source matrix liquid crystal display, TFT flexible display, touch screen display and OLED and other application fields. Compared with pure molybdenum target, adding a certain proportion of niobium to molybdenum can increase the pixels of liquid crystal display by more than two times, and molybdenum-niobium alloy also has excellent electrical conductivity, oxidation resistance and low coating stress. It is widely used as an important target for wiring in flat panel displays. With the continuous development of LCD TVs, tablet computers and mobile phones at home and a...

Examples

preparation example Construction

[0045] A method for preparing a large-size molybdenum-niobium planar target, Figure 1 to Figure 6 As shown, including 1) powder granulation step, 2) hot isostatic pressing step and 3) hot deformation step, large-sized molybdenum-niobium targets are obtained, and large-size molybdenum-niobium targets refer to lengths ranging from 1000mm to 4000mm molybdenum-niobium target.

[0046] Since molybdenum-niobium alloy belongs to replacement solid solution, because of its high melting point and high temperature brittleness, it is difficult to be prepared by smelting, casting or pressure processing. At present, most of them are prepared by powder metallurgy. Although sintering can quickly achieve densification, the sintering porosity is high and the density is low. The density is about 95% of the theoretical value, and it is difficult to meet the theoretical density requirement of more than 99%. Molybdenum and niobium sintered in a hydrogen atmosphere are easy to absorb hydrogen, resu...

specific Embodiment approach 1

[0071] 1.1) In the mixing step, high-purity molybdenum powder with a purity of ≥99.95%, an oxygen content of ≤1500ppm, and a particle size of 4 to 8 microns and a high-purity niobium powder with a purity of ≥99.9% and a particle size of 10 to 80 microns are used, according to the niobium content of 12at The % ratio is placed in a V-shaped mixer, and under the condition of vacuuming and filling with argon for 30 minutes, the high-purity molybdenum powder and high-purity niobium powder are fully mixed for 6 hours to obtain molybdenum-niobium mixed powder.

[0072] 1.2) In the compaction step, the molybdenum-niobium mixed powder is pressed into a compact by a four-column press. The 800T four-column press is selected. The size of the compact is 150*mm150mm*40mm, and the theoretical value of the density of the compact reaches 48%.

[0073] 1.3) Hydrogen pre-sintering step, put the block into a hydrogen atmosphere heating furnace for 3 hours and set the temperature in the heating fur...

specific Embodiment approach 2

[0080] 1.1) In the mixing step, high-purity molybdenum powder with a purity of ≥99.95%, an oxygen content of ≤1500ppm, and a particle size of 4 to 8 microns and a high-purity niobium powder with a purity of ≥99.9% and a particle size of 10 to 80 microns are used, and the niobium content is 5 at The % ratio is placed in a V-shaped mixer, and under the condition of vacuuming and filling with argon for 30 minutes, the high-purity molybdenum powder and high-purity niobium powder are fully mixed for 5 hours to obtain molybdenum-niobium mixed powder.

[0081] 1.2) In the compacting step, the molybdenum-niobium mixed powder is pressed into a compact by a four-column press. A 600T four-column press is selected. The size of the compact is 150*150*30mm, and the theoretical value of the density of the compact reaches 40%.

[0082] 1.3) Hydrogen pre-sintering step, put the block into a hydrogen atmosphere heating furnace for 2 hours, set the temperature in the heating furnace at 950°C, and...

technical field

[0001] The invention relates to the technical field of metal target material production for coating sputtering in electronic industries such as liquid crystal displays, and in particular to a method for preparing a large-size molybdenum-niobium planar target material. Background technique

[0002] At present, molybdenum-niobium alloy, as the key material for making FPD, has been widely used in LCD source matrix liquid crystal display, TFT flexible display, touch screen display and OLED and other application fields. Compared with pure molybdenum target, adding a certain proportion of niobium to molybdenum can increase the pixels of liquid crystal display by more than two times, and molybdenum-niobium alloy also has excellent electrical conductivity, oxidation resistance and low coating stress. It is widely used as an important target for wiring in flat panel displays. With the continuous development of LCD TVs, tablet computers and mobile phones at home and a...

Examples

preparation example Construction

[0045] A method for preparing a large-size molybdenum-niobium planar target, Figure 1 to Figure 6 As shown, including 1) powder granulation step, 2) hot isostatic pressing step and 3) hot deformation step, large-sized molybdenum-niobium targets are obtained, and large-size molybdenum-niobium targets refer to lengths ranging from 1000mm to 4000mm molybdenum-niobium target.

[0046] Since molybdenum-niobium alloy belongs to replacement solid solution, because of its high melting point and high temperature brittleness, it is difficult to be prepared by smelting, casting or pressure processing. At present, most of them are prepared by powder metallurgy. Although sintering can quickly achieve densification, the sintering porosity is high and the density is low. The density is about 95% of the theoretical value, and it is difficult to meet the theoretical density requirement of more than 99%. Molybdenum and niobium sintered in a hydrogen atmosphere are easy to absorb hydrogen, resu...

specific Embodiment approach 1

[0071] 1.1) In the mixing step, high-purity molybdenum powder with a purity of ≥99.95%, an oxygen content of ≤1500ppm, and a particle size of 4 to 8 microns and a high-purity niobium powder with a purity of ≥99.9% and a particle size of 10 to 80 microns are used, according to the niobium content of 12at The % ratio is placed in a V-shaped mixer, and under the condition of vacuuming and filling with argon for 30 minutes, the high-purity molybdenum powder and high-purity niobium powder are fully mixed for 6 hours to obtain molybdenum-niobium mixed powder.

[0072] 1.2) In the compaction step, the molybdenum-niobium mixed powder is pressed into a compact by a four-column press. The 800T four-column press is selected. The size of the compact is 150*mm150mm*40mm, and the theoretical value of the density of the compact reaches 48%.

[0073] 1.3) Hydrogen pre-sintering step, put the block into a hydrogen atmosphere heating furnace for 3 hours and set the temperature in the heating fur...

specific Embodiment approach 2

[0080] 1.1) In the mixing step, high-purity molybdenum powder with a purity of ≥99.95%, an oxygen content of ≤1500ppm, and a particle size of 4 to 8 microns and a high-purity niobium powder with a purity of ≥99.9% and a particle size of 10 to 80 microns are used, and the niobium content is 5 at The % ratio is placed in a V-shaped mixer, and under the condition of vacuuming and filling with argon for 30 minutes, the high-purity molybdenum powder and high-purity niobium powder are fully mixed for 5 hours to obtain molybdenum-niobium mixed powder.

[0081] 1.2) In the compacting step, the molybdenum-niobium mixed powder is pressed into a compact by a four-column press. A 600T four-column press is selected. The size of the compact is 150*150*30mm, and the theoretical value of the density of the compact reaches 40%.

[0082] 1.3) Hydrogen pre-sintering step, put the block into a hydrogen atmosphere heating furnace for 2 hours, set the temperature in the heating furnace at 950°C, and...

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