Manufacturing method of molybdenum rotating target material for sputtering deposition

A technology of sputtering coating and manufacturing method, which is applied in the direction of sputtering coating, ion implantation coating, vacuum evaporation coating, etc., which can solve the problem of affecting the quality and yield of downstream products, insufficient target density, and target particle splashing and other problems to achieve the effect of good compactness, high yield and simple process

Inactive Publication Date: 2017-08-08

BAOTOU RES INST OF RARE EARTHS

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AI-Extracted Technical Summary

Problems solved by technology

[0003] In order to improve the utilization rate of the target, a tubular rotating target is usually used, so that the target utilization rate can be increased from 30% to 50% of the planar target to 80% of the rotating target. At present, the most commonly used process for forming molybdenum target is traditional powder Metallurgy, the target produced by this process has insufficient density and relatively coarse grains. During use, it is ea...

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Method used

(5) forging: the molybdenum billet after sintering is put into sintering furnace, feeds hydrogen protection, adopts water circulation to cool down, is heated to 1000 ℃, is incubated 1~3h, is the air hammer of 1000 kilograms with impact force after taking out Carry out forging to further increase the density of the molybdenum billet;

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Abstract

The invention discloses a manufacturing method of a molybdenum rotating target material for sputtering deposition. The method includes the steps that high-purity molybdenum powder is evenly filled into a tubular mold, and then is prepared into a tubular powder molybdenum billet by means of extrusion forming; the tubular powder molybdenum billet is put into a cold isostatic press to be pressed, and a molybdenum billet is obtained after isostatic pressing compaction is completed; the formed molybdenum billet is put into a vacuum sintering furnace to be sintered, the sintered molybdenum billet is put into the sintering furnace, hydrogen is connected in for protection, and the molybdenum billet is taken out for repeated hammer forging after heating and heat preservation are completed; the forged molybdenum billet is put into a vacuum annealing furnace for annealing, and then the molybdenum billet is cooled to an indoor temperature along with the furnace; and after the annealed molybdenum billet is machined, the molybdenum rotating target material can be obtained. The molybdenum rotating target material obtained through the method has the characteristics that the relative density is high, machinability is good, the inner grain structure of the target material is uniform and small and tissue defects are avoided.

Application Domain

Vacuum evaporation coatingSputtering coating +1

Technology Topic

CrystalliteTissue defect +8

Examples

Experimental program(3)

Example Embodiment

[0026] Example 1

[0027] A method for manufacturing a molybdenum rotating target for sputtering coating specifically includes the following steps:

[0028] (1) Raw material: The powder used is high-purity molybdenum powder with purity ≥99.95%;

[0029] (2) Mold loading: evenly fill the powder in a tubular stainless steel mold with an outer diameter of 200mm and an inner diameter of 50mm, and press to prepare a tubular powdery molybdenum blank;

[0030] (3) Cold isostatic pressing: Put the tubular powdery molybdenum billet into a cold isostatic press for pressing, the pressing pressure is 180Mpa, and the pressure is maintained for 4 minutes;

[0031] (4) Sintering: Put the formed molybdenum billet into a vacuum sintering furnace, the sintering temperature is 1800℃, the vacuum degree is 2.5×10 -2 Pa, heat preservation for 5h;

[0032] (5) Forging: Put the sintered molybdenum billet into a sintering furnace, pass in hydrogen protection, use water circulation to cool down, heat to 1000℃, keep it for 1~3h, take it out, and forge it with an air hammer with an impact of 1000 kg , Further improve the density of molybdenum billet;

[0033] (6) Annealing: Put the forged molybdenum billet into a vacuum annealing furnace, heat it to 1200°C, keep it for 1 hour, and then cool it to room temperature along with the furnace;

[0034] (7) Mechanical processing: The annealed molybdenum billet is processed on a lathe as required, and then cleaned and dried to obtain a sputtering molybdenum rotating target.

[0035] A high-purity molybdenum rotating target is obtained, with a relative density of 98%, a purity of ≥99.95%, a grain size of 5-15 μm, a N content of 400 ppm, and an O content of 850 ppm.

Example Embodiment

[0036] Example 2:

[0037] A method for manufacturing a molybdenum rotating target for sputtering coating specifically includes the following steps:

[0038] (1) Raw material: The powder used is high-purity molybdenum powder with purity ≥99.95%;

[0039] (2) Mold loading: evenly fill the powder in a tubular stainless steel mold with an outer diameter of 200mm and an inner diameter of 50mm, and press to prepare a tubular powdery molybdenum blank;

[0040] (3) Cold isostatic pressing: Put the tubular powdery molybdenum billet into a cold isostatic press for pressing, the pressing pressure is 200Mpa, and the pressure is maintained for 4 minutes;

[0041] (4) Sintering: Put the formed molybdenum billet into a vacuum sintering furnace, the sintering temperature is 1850℃, and the vacuum degree is 2.5×10 -2 Pa, heat preservation 6h;

[0042] (5) Forging: Put the sintered molybdenum billet into a sintering furnace, pass in hydrogen protection, use water circulation to cool down, heat to 1000℃, keep it for 1~3h, take it out, and forge it with an air hammer with an impact of 1000 kg , Further improve the density of molybdenum billet;

[0043] (6) Annealing: Put the forged molybdenum billet into a vacuum annealing furnace, heat it to 1200°C, keep it for 1 hour, and then cool it to room temperature along with the furnace;

[0044] (7) Mechanical processing: The annealed molybdenum billet is processed on a lathe as required, and then cleaned and dried to obtain a sputtering molybdenum rotating target.

[0045] A high-purity molybdenum rotating target is obtained, the relative density is 98.6%, the purity is ≥99.95%, the N content is 500ppm, and the O content is 800ppm.

Example Embodiment

[0046] Example 3:

[0047] (1) Raw material: The powder used is high-purity molybdenum powder with purity ≥99.95%;

[0048] (2) Mold loading: evenly fill the powder in a tubular stainless steel mold with an outer diameter of 200mm and an inner diameter of 50mm, and press to prepare a tubular powdery molybdenum blank;

[0049] (3) Cold isostatic pressing: Put the tubular powdery molybdenum billet into a cold isostatic press for pressing, the pressing pressure is 250Mpa, and the pressure is maintained for 4 minutes;

[0050] (4) Sintering: Put the formed molybdenum billet into a vacuum sintering furnace, the sintering temperature is 1900℃, and the heat preservation is 8h;

[0051] (5) Forging: Put the sintered molybdenum billet into a sintering furnace, pass in hydrogen protection, use water circulation to cool down, heat to 1000℃, keep it for 1~3h, take it out, and forge it with an air hammer with an impact of 1000 kg , Further improve the density of molybdenum billet;

[0052] (6) Annealing: Put the forged molybdenum billet into a vacuum annealing furnace, heat it to 1200°C, keep it for 1 hour, and then cool it to room temperature along with the furnace;

[0053] (7) Mechanical processing: The annealed molybdenum billet is processed on a lathe as required, and then cleaned and dried to obtain a sputtering molybdenum rotating target.

[0054] Obtain a high-purity molybdenum rotating target with a relative density of 99% and a purity of ≥99.95%.

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PUM

Property	Measurement	Unit
Grain size	5.0 ~ 15.0	µm
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Simple process
Improve yield

Manufacturing method of molybdenum rotating target material for sputtering deposition

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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