CN-122012997-A - Superfine crystal aluminum silicon copper target material and preparation method thereof

CN122012997ACN 122012997 ACN122012997 ACN 122012997ACN-122012997-A

Abstract

The invention relates to the technical field of nonferrous metal materials and targets, and provides an ultrafine-grain aluminum-silicon-copper target and a preparation method thereof. The superfine crystal aluminum silicon copper target material provided by the invention comprises, by mass, 1-2% of Si, 0.5-1% of Cu, the balance of Al, and less than or equal to 10ppm of oxygen, wherein the grain size of the superfine crystal aluminum silicon copper target material is less than or equal to 1 mu m. The invention combines accurate parameter matching through the composite process of oxygen control casting, equal channel extrusion, cold rolling and low temperature annealing to obtain the superfine crystal aluminum silicon copper target material with uniform and fine grain size, low oxygen content, high density and excellent mechanical property and sputtering property, can meet the strict requirements of high-end coating on the evenness and the electrical consistency of the film, has simple process flow and good product quality stability, and is suitable for industrial mass production.

Inventors

WEN MING
Shi Chenqi
LI SHIQI
Yang Tianshuo
TANG KE
SHEN YUE
WANG CHUANJUN
XU YANTING
LI SIXIE
TANG QI

Assignees

云南省贵金属新材料控股集团股份有限公司
贵研先进新材料(上海)有限公司
云南贵金属实验室有限公司
昆明贵金属研究所

Dates

Publication Date: 20260512
Application Date: 20260209

Claims (10)

1. The superfine crystal aluminum silicon copper target is characterized by comprising, by mass, 1-2% of Si, 0.5-1% of Cu and the balance of Al, wherein the grain size of the superfine crystal aluminum silicon copper target is less than or equal to 1 mu m, and the oxygen content is less than or equal to 10ppm.
2. The ultra-fine grain aluminum silicon copper target according to claim 1, wherein the density of the ultra-fine grain aluminum silicon copper target is more than or equal to 99.5%, the hardness is 75-100 HV, and the elongation is more than or equal to 10%.
3. The method for preparing the superfine crystal aluminum silicon copper target material as claimed in claim 1 or 2, which is characterized by comprising the following steps: Sequentially introducing hydrogen to deoxidize and deoxidize rare earth elements to the molten metal, casting and cooling, and cutting off the part of the ingot head containing rare earth oxides to obtain qualified ingots; And sequentially carrying out homogenization treatment, equal channel extrusion, cold rolling processing and annealing treatment on the qualified cast ingot to obtain the superfine crystal aluminum silicon copper target material, wherein the included angle of channels of a die used for equal channel extrusion is 90-120 degrees, the total deformation of the cold rolling processing is 80-95%, and the annealing treatment temperature is 200-300 ℃.
4. The preparation method of the aluminum alloy, according to claim 3, is characterized in that the raw materials are industrial pure aluminum, silicon powder and electrolytic copper, wherein the purity of the industrial pure aluminum is more than or equal to 99.999%, the purity of the silicon powder is more than or equal to 99.999%, the purity of the electrolytic copper is more than or equal to 99.999%, the smelting temperature is 720-760 ℃, the stirring speed is 300-500 r/min, and the stirring time is 5-10 min; the time for introducing hydrogen and deoxidizing is 5-10 min, and the hydrogen pressure is 0.05-0.3 Pa, wherein the rare earth elements comprise one or more of lanthanum, cerium and yttrium; The temperature of the homogenization treatment is 480-520 ℃ and the heat preservation time is 4-6 h.
5. The preparation method according to claim 3, wherein the material of the die for the equal channel extrusion is hard alloy, and the surface roughness Ra is less than or equal to 0.2 μm; the extrusion speed of the equal channel extrusion is 2-5 mm/s, the number of equal channel extrusion passes is 2-4, the cast ingot is rotated for 90 degrees after each pass of extrusion, the cast ingot and the die are respectively preheated before the equal channel extrusion, the preheating temperature is 100-200 ℃, and the heat preservation time is 1-2 h.
6. The method according to claim 3, wherein the cold rolling process has a pass deformation of 20 to 30% and a rolling speed of 0.5 to 1.5m/s.
7. The method according to claim 3, wherein the heat preservation time of the annealing treatment is 2-4 hours.
8. The method of claim 3, further comprising machining the resulting target after the annealing.
9. The use of the ultra-fine grain aluminum silicon copper target material according to claim 1 or 2 or the ultra-fine grain aluminum silicon copper target material prepared by the preparation method according to any one of claims 3-8 in magnetron sputtering coating.
10. The use according to claim 9, wherein the magnetron sputtering coating comprises the preparation of a semiconductor interconnect layer, a display panel electrode layer or a solar cell coating layer.

Description

Superfine crystal aluminum silicon copper target material and preparation method thereof Technical Field The invention relates to the technical field of nonferrous metal materials and targets, in particular to an ultrafine grain aluminum silicon copper target and a preparation method thereof. Background In the integrated circuit interconnection material system, aluminum has long-term dominant metallization process of more than 90 nm process nodes by virtue of excellent electrical conductivity, thermal conductivity, process compatibility and economy, and remains important in the display and packaging fields. However, as process linewidths enter the nanoscale, pure aluminum interconnect materials expose electromigration (electromigration) and stress migration (stress migration) resulting in reliability problems that can cause void accumulation, interface failure, and open wire, which are key obstacles restricting their further miniaturization applications. By introducing a small amount of Si and Cu elements into aluminum to form Al-Si, al-Cu and Al-Si-Cu systems, the strength and the conductivity can be cooperatively improved. The Si element is mainly used for inhibiting the growth of crystal grains and improving the thermal expansion matching, while the Cu element can strengthen solid solution, improve electromigration resistance and promote grain boundary stabilization. The Al-Si-Cu alloy target material can be used for preparing functional films such as semiconductor interconnection layers, display panel electrode layers and the like. Compared with the target material with a coarse crystal structure, the target material with fine grains has obviously improved sputtering rate due to the greatly increased grain boundary. Thus, improvements in the microstructure of Al-Si-Cu alloy targets, such as fine grains obtained by process control, can increase the sputtering rate. The related art discloses a preparation method of a fine-grain high-purity aluminum-silicon-copper alloy target blank for sputtering, wherein the fine-grain high-purity aluminum-silicon-copper alloy target blank for sputtering is obtained by preparing a master alloy, melting the master alloy and high-purity aluminum, refining on line, filtering in a bipolar mode and casting. However, this solution only mentions that the aluminum-silicon-copper alloy target prepared by the method has an equiaxed crystal structure and uniform components, and does not relate to specific grain sizes. Another related technology discloses a high-purity aluminum-silicon-copper target material, a preparation method and application thereof, wherein the aluminum-silicon-copper target material is obtained through the steps of homogenizing annealing, multidirectional forging, solution treatment, longitudinal and transverse alternate cold rolling, recrystallization annealing, rough machining, binding, finish machining, surface treatment and the like, and precipitation phases of the target material are uniformly distributed, and the average grain size is about 100 mu m. At present, the traditional technology of casting-forging-hot rolling-cold rolling-annealing is mostly adopted in the existing preparation method of the aluminum-silicon-copper target, but the existing preparation method has the obvious defects that cast alloy is easy to generate component segregation, coarse casting grains, looseness, air holes and the like, the subsequent hot rolling/cold rolling is difficult to completely eliminate, the grain size of the target is large (usually 50-80 mu m), the structure uniformity is poor, and the sputtering performance is still poor. In addition, in the prior art, the oxygen content of the target is not regulated, the oxide in the aluminum-silicon-copper target is an insulating high-resistance phase, sputtering ignition and voltage-current fluctuation are easy to trigger, the damage process is stable, the sputtering threshold is high, and the sputtering rate can be reduced and fluctuated. Meanwhile, oxide particles splash to introduce thin film impurity defects, so that targets can be ablated, the utilization rate is reduced, a cavity is polluted, and equipment loss is increased. In view of the foregoing, there is a need to provide an aluminum-copper-silicon target with small grain size, low oxygen content and excellent sputtering performance, so as to meet the requirements of high-end coating. Disclosure of Invention In view of the above, the invention provides an ultrafine grain aluminum silicon copper target and a preparation method thereof. The superfine crystal aluminum silicon copper target provided by the invention has the advantages that the grain size is smaller than 1 mu m, the oxygen content is less than or equal to 10ppm, the grain size is uniform, the density is high, the mechanical property is good, and the sputtering performance is excellent. In order to achieve the above object, the present invention provides the following technical solutions: The super