Molybdenum-nickel-based multi-element alloy rotary target material and preparation method thereof

A multi-element alloy and rotating target technology, which is applied in metal material coating process, ion implantation plating, coating, etc., can solve problems such as difficult target preparation, removal, sputtering coating arcing, etc., and achieve obvious market competition The effect of reducing power and sintering cost and improving comprehensive performance

Active Publication Date: 2021-10-01
NANJING DAMAI SCI&TECH IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Because the melting point of molybdenum is as high as 2620°C, the density is 10.2g / cm 3 , while the melting point of aluminum is 660°C and the density is 2.7g / cm 3 , the difference in melting point and density between the two is large, and the vacuum melting method is easy to shrinkage and segregation, which cannot guarantee the uniformity of the product structure and composition, and produces a variety of brittle phases, the product is easy to crack, and it is impossible to prepare large-size targets.
If it is prepared by hot pressing sintering, although this method can avoid alloy composition segregation to a certain extent, the hot pressing process cannot remove oxygen, nitrogen and other gaseous impurity elements, which will lead to excessive impurities and oxygen content in the product, resulting in sputtering Arcing during the coating process; in addition, due to the limitation of hot pressing and sintering equipment, it is difficult to prepare targets longer than 1.5 meters

Method used

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  • Molybdenum-nickel-based multi-element alloy rotary target material and preparation method thereof
  • Molybdenum-nickel-based multi-element alloy rotary target material and preparation method thereof
  • Molybdenum-nickel-based multi-element alloy rotary target material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of Mo 40 Ni 30 Ti 15 al 15

[0029] S1. Use Mo powder with a particle size of 3-7um, an oxygen content of ≤1000ppm, and a purity greater than 99.95%; Ni powder is electrolytic nickel powder, with a purity of greater than 99.9%, a particle size of 6-12um, and an oxygen content of ≤2000ppm; atomized and granulated Ti 50 al 50 Alloy powder, particle size 35-60um, oxygen content ≤3000ppm. Mix according to the above atomic ratio, put it in a vacuum furnace at 1000°C, and the vacuum degree is not less than 10 -2 Pa was subjected to vacuum deoxidation purification treatment for 2h.

[0030] S2. The vacuum-treated powder is mixed by mechanical ball milling, the ball-to-material ratio is 3:1, the rotation speed is 170 R / M, and the argon gas protection ball mill is mixed for 12 hours. The inner lining and balls of the ball mill are made of pure molybdenum.

[0031] S3. Fill the ball mill powder into the tubular mold cavity. The powder filling process uses a vib...

Embodiment 2

[0038] Preparation of Mo 52 Ni 25 Ti 15 al 8

[0039] S1. Use Mo powder with a particle size of 3-7um, an oxygen content of ≤1000ppm, and a purity greater than 99.95%; Ni powder is electrolytic nickel powder, with a purity of greater than 99.9%, a particle size of 6-12um, and an oxygen content of ≤2000ppm; atomized and granulated Ti 70 al 30 Alloy powder, particle size 35-60um, oxygen content ≤3000ppm. Mix according to the above atomic ratio, place in a vacuum furnace at 1030°C, and the vacuum degree is not less than 10 - 2 Pa was subjected to vacuum deoxidation purification treatment for 5h.

[0040] S2. The vacuum-treated powder is mixed by mechanical ball milling, the ball-to-material ratio is 3:1, the rotation speed is 180 R / M, and the argon gas protection ball mill is mixed for 10 hours. The inner lining and balls of the ball mill are made of pure molybdenum.

[0041] S3. Fill the ball mill powder into the tubular mold cavity. The whole powder filling process uses...

Embodiment 3

[0048] Preparation of coating samples, where the target material is Mo 45 -Ni 30 -Ti 15 -Al 10 .

[0049] S1. Use Mo powder with a particle size of 3-7um, an oxygen content of ≤1000ppm, and a purity greater than 99.95%; Ni powder is electrolytic nickel powder, with a purity of greater than 99.9%, a particle size of 6-12um, and an oxygen content of ≤2000ppm; atomized and granulated Ti50AL50at% alloy Powder, particle size 35-60um, oxygen content ≤3000ppm. By atomic ratio Mo 45 -Ni 30 -Ti 15 -Al 10 at% mixed, placed in a vacuum furnace at 1000 ° C, the vacuum degree is not less than 10 -2 pa for vacuum deoxidation purification treatment 1H.

[0050] S2. The vacuum-treated powder is mixed by mechanical ball milling, the ball-to-material ratio is 3:1, the rotation speed is 170 R / M, and the argon gas protection ball mill is mixed for 8 hours. The inner lining and balls of the ball mill are made of pure molybdenum.

[0051] S3. Fill the ball mill powder into the tubular mol...

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Abstract

The invention discloses a molybdenum-nickel-based multi-element alloy rotary target material and a preparation method thereof. The atomic composition of the rotary target material is Mo100-x-y-zNixTiyAlz, X, Y and Z represent the atomic composition percentage, X is larger than or equal to 10 and smaller than or equal to 40, Y is larger than or equal to 1 and smaller than or equal to 20, and Z is larger than or equal to 1 and smaller than or equal to 18. The preparation method comprises the steps of mixing molybdenum powder, electrolytic nickel powder and titanium-aluminum pre-alloy powder in proportion, then carrying out deoxidation and purification treatment, ball milling and mixing, powder filling and compaction treatment, cold isostatic pressing forming, demolding, vacuum horizontal sintering, rotary swaging treatment and annealing treatment to obtain a molybdenum-nickel-titanium-aluminum alloy pipe ingot, and finally slicing the molybdenum-nickel-titanium-aluminum alloy pipe ingot through machining to prepare the molybdenum-nickel-titanium-aluminum alloy target material. According to the preparation method, introduction of impurity elements can be reduced in the preparation process, the produced target material is uniform in component, free of segregation and fine in grain, the density can reach a theoretical value of 99% or above, and the coating requirement of a current large-size sputtering target material can be completely met.

Description

technical field [0001] The invention belongs to a magnetron sputtering metal target, in particular to a large-size molybdenum-nickel-titanium-aluminum quaternary alloy tubular sputtering target and a preparation method thereof. Background technique [0002] With the enlargement and high precision of flat-panel displays, copper is used as the main wiring film material of thin-film transistors (TFTs) for FPD drive components. Copper metallization has been widely developed in the TFT-LCD industry. In TFT liquid crystal displays, due to the low adhesion of copper to glass substrates, copper needs an adhesive metal film layer as the bottom layer or cover layer, such as Mo, Ti, Nb, Ni, Ta, Cr and other metal film layers. When different metals and copper are placed in the etchant, a typical galvanic reaction occurs, and the copper is weakened after drying or partially stained on the metal surface, resulting in poor performance and display quality of the thin film transistor. There...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35B22F1/00B22F3/04B22F3/10B22F3/17B22F3/24B22F9/04C21D1/30C22F1/18C22C27/04B22F5/12
CPCC23C14/3407C23C14/35C23C14/3414B22F9/04B22F3/04B22F3/1007B22F3/1017B22F3/172B22F3/24C21D1/30C22F1/18C22C27/04B22F5/106B22F2009/043B22F2003/248B22F2003/247Y02E30/10
Inventor 吴宇宁卿海标
Owner NANJING DAMAI SCI&TECH IND CO LTD
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