CN110592406A - Preparation method of high-purity aluminum-copper alloy target blank for sputtering - Google Patents
Preparation method of high-purity aluminum-copper alloy target blank for sputtering Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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Abstract
The invention relates to a preparation method of a high-purity aluminum-copper alloy target blank for sputtering. A preparation method of a high-purity aluminum-copper alloy target blank for sputtering comprises the following steps: s10: carrying out vacuum melting on high-purity aluminum with the purity of 99.999-99.9995% and high-purity copper with the purity of more than 99.999% to obtain intermediate alloy liquid: s20: smelting a high-purity aluminum ingot with the purity of more than 99.9995 wt% and the intermediate alloy liquid at the smelting temperature of 720-800 ℃, controlling the temperature of the alloy liquid to reach 730 +/-5 ℃ after the alloy liquid is completely molten, and standing and preserving the temperature for 15 min; s30: carrying out furnace refining; s40: carrying out online refining; s50: performing bipolar filtration; s60: and (4) performing phi 120-164mm bar blank casting to obtain the high-purity aluminum-copper alloy target blank for sputtering. The invention relates to a preparation method of a high-purity aluminum-copper alloy target blank for sputtering, which is characterized in that a high-purity aluminum-copper alloy bar with low impurity element content and uniform structure is prepared by using an ultra-high-purity aluminum raw material and a high-purity aluminum-copper intermediate alloy through semi-continuous casting.
Description
Technical Field
The invention belongs to the technical field of sputtering targets, and particularly relates to a preparation method of a high-purity aluminum-copper alloy target blank for sputtering.
Background
Sputtering is one of the main techniques for preparing thin film materials, and utilizes ions generated by an ion source to form an ion beam flow with high-speed flow through accelerated aggregation in vacuum, so as to bombard the surface of a solid, and kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, so that the atoms on the surface of the solid are separated from the solid and are deposited on the surface of a substrate. The bombarded solid is the starting material for depositing thin films by sputtering, known as the sputtering target.
The aluminum electronic film has the advantages of low resistivity (room temperature is 2.7 mu omega cm), easy deposition, easy etching, mature process and the like, and can be widely applied to the electronic information fields of integrated circuits, discrete devices, novel display and the like as an electrode or interconnection line material. In the pure aluminum process, problems of aluminum spike, Stress Migration (SM), Electromigration (EM) and the like are caused due to the solid-state mutual solubility of silicon and aluminum, and finally, the device failure and the yield are reduced. Studies have shown that the above problems can be solved by adding alloying elements to aluminum. In the early stage, in order to eliminate aluminum peak and improve the stress migration resistance of aluminum, a proper amount of Si element is added into high-purity aluminum, and an AlSi alloy is developed; in order to improve the electromigration resistance of aluminum, a proper amount of Cu element is added into high-purity aluminum, and AlCu and AlSiCu alloy is developed; with the development of an aluminum process, barrier layer films of Ti, Ta, Mo and the like are prepared on the outer layer of the aluminum film, so that the aluminum film is not in direct contact with a silicon substrate, Si does not need to be added into high-purity aluminum, and the electric conductivity of the aluminum material is reduced due to the existence of Si, so that AlCu alloy can be directly used. Therefore, AlCu alloys are currently the most common conductive interconnect materials. With the rapid updating of products in the semiconductor industry, aluminum-silicon products are gradually replaced by aluminum-copper and aluminum-silicon-copper products due to poor performance. Fig. 1 is a main process flow for preparing a target material for the semiconductor industry.
The target material restricts the physical and mechanical properties of the sputtered film. The coating quality is influenced, so the target quality evaluation is strict, and the following requirements are mainly met:
1) low impurity content and high purity. The purity of the target material affects the uniformity of the film.
2) High compactness. The high-density target has the advantages of good electrical conductivity and thermal conductivity, high strength and the like, and when the target is used for coating, the sputtering power is small, the film forming rate is high, the film is not easy to crack, the service life of the target is long, and the resistivity and the light transmittance of the sputtered film are low.
3) The components and the tissue structure are uniform. The uniformity of the target material components is an important guarantee for the stable quality of the coating.
4) The grain size is fine. The finer the grain size of the target, the more uniform the thickness distribution of the sputtered film, and the faster the sputtering rate.
Patent CN105296945B (an aluminum alloy sputtering target and its preparation method): the invention discloses an aluminum alloy sputtering target material and a preparation method thereof, belonging to the technical field of sputtering target material preparation. The aluminum alloy sputtering target material consists of Al, Cu and refractory metal, and the raw material is a high-purity raw material. The aluminum alloy sputtering target is prepared by the processes of smelting, thermal mechanical treatment, forming and the like. The purity of the prepared aluminum alloy sputtering target material is more than 99.995%, the crystal grains are fine and uniform, the size of the crystal grains is controlled within 200 mu m, the comprehensive performance is excellent, and the method can be used for preparing high-reliability and high-stability aluminum films. However, the purity of the raw materials used in the technology is only 99.995%, the content of impurity elements is high, the uniformity of the film is influenced, and the technology is directly cast after smelting without refining and filtering procedures, so that the impurity and gas elements in the target blank are high, and the sputtering effect is influenced.
In the research on the preparation process of the high-purity aluminum-copper alloy in the prior art (article number: 1002-. However, in this test, when 6N high purity copper plate and 6N high purity aluminum were used for melting, the raw material cost was high, the melting temperature was high, and the low melting point metal was easily burned.
Patent CN105525149A (a preparation method of aluminum alloy sputtering target material): the invention discloses a preparation method of an aluminum alloy sputtering target material, which comprises the following steps: (1) casting an aluminum alloy ingot by adopting cold die magnetic stirring; (2) carrying out partial homogenization heat treatment on the aluminum alloy cast ingot to form a precipitate with the diameter of 1-2 mu m in the material; (3) carrying out multidirectional die forging on the cast ingot, and refining grains; (4) performing intermediate annealing treatment to eliminate forging stress; (5) cold rolling is carried out, crystal grains are further refined, and the orientation content of a sputtering surface {200} is enhanced; (6) and (4) carrying out recrystallization annealing to obtain the aluminum alloy sputtering target material with uniform and refined recrystallized microstructure. The aluminum alloy target material obtained by the method has fine grains and obviously improved microstructure uniformity. However, in this invention, an aluminum alloy ingot is cast by magnetic stirring using a cold die, and the grain structure is refined by multi-directional die forging, cold rolling and recrystallization annealing. Because the blank casting process flow in the invention is not clear, compared with the method adopting vacuum melting, the method is more beneficial to controlling the purity and uniformity of the components of the aluminum liquid.
In view of this, the present invention provides a new method for preparing a high-purity aluminum-copper alloy target blank for sputtering.
Disclosure of Invention
The invention provides a preparation method of a high-purity aluminum-copper alloy target blank for sputtering.
In order to realize the purpose, the adopted technical scheme is as follows:
a preparation method of a high-purity aluminum-copper alloy target blank for sputtering comprises the following steps:
s10: melting high-purity aluminum with the purity of 99.999-99.9995% and high-purity copper with the purity of more than 99.999% in a vacuum melting furnace, controlling the melting temperature at 800-: the content of copper element in the intermediate alloy liquid 1 is 20-25 wt%;
s20: adding a high-purity aluminum ingot with the purity of more than 99.9995 wt% and the intermediate alloy liquid into an intermediate frequency smelting furnace for smelting, wherein the smelting temperature is 720-800 ℃, stirring uniformly after complete melting, controlling the temperature of the alloy liquid to 730 +/-5 ℃, standing and preserving heat for 15min to obtain intermediate alloy liquid 2;
s30: refining the intermediate alloy liquid 2 in a furnace by adopting high-purity argon, and standing for 20min after refining to obtain intermediate alloy liquid 3;
s40: carrying out on-line refining on the intermediate alloy liquid 3 by adopting high-purity argon to obtain an intermediate alloy liquid 4;
s50: carrying out bipolar filtration on the intermediate alloy liquid 4 to obtain an intermediate alloy liquid 5;
s60: and (3) casting the intermediate alloy liquid 5 into a bar blank with the diameter of phi 120-.
Further, in the step S10, the stirring time is not less than 15 min;
in the step S20, the stirring time is not less than 15 min.
Further, in S20, standing and preserving heat for 15min, sampling and detecting the content of copper element, if the content meets the mass ratio of 0.4-0.6%, starting refining in the furnace, and if the content does not meet the mass ratio, secondarily adding the intermediate alloy to adjust to the required ratio.
Further, in the step S30, the flow rate of argon gas is 3 to 5m3The refining time is 25-40min, and the refining temperature is 730-.
Further, in the step S40, the flow rate of argon gas is 3 to 5m3H, refining time of 15-20min, and refining temperature of 730-.
Further, in S50, bipolar filtration refers to in-line filtration using a 40PPI and a 50PPI porosity filter plate.
Further, in S60, a semi-continuous casting machine is used to perform water cooling for casting the phi 120-.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention uses high-purity aluminum raw material with purity of more than 99.999-99.9995 wt% and high-purity copper with purity of more than 99.999 wt% to prepare high-purity aluminum-copper intermediate alloy through vacuum melting and electromagnetic stirring so as to control the uniformity of components.
2. The casting process of the invention controls three casting parameters, such as the temperature of the aluminum liquid, the casting speed, the flow rate and the liquid level of the cooling water, the casting mode and the like, so that the bar product has uniform components and uniform grain structure, and the bar has no casting defects such as inclusion, shrinkage cavity and the like.
3. The high-purity Al-0.5 wt% Cu target blank for sputtering prepared by the invention has extremely low trace impurity element content and good sputtering film-forming property.
4. The high-purity Al-0.5 wt% Cu target blank has uniform components and internal tissues. The bar has no defect with the size more than 0.8mm inside, and has fine and uniform crystal grains and high sputtering rate.
Drawings
FIG. 1 is a main process flow for the preparation of targets for the semiconductor industry;
FIG. 2 is a microstructure of cast AL-25% Cu high purity aluminum bronze master alloy of example 1 (polished non-corroded 100X);
FIG. 3 is a macroscopically eroded microstructure of an AL-0.5% Cu target blank cast in accordance with example 1;
FIG. 4 shows the microstructure of cast AL-0.5% Cu target blank (electropolishing and coating 50X) of example 1;
FIG. 5 is a macroscopic corrosion feather grain structure of an AL-0.5% Cu target blank cast at a casting temperature above 690 ℃;
FIG. 6 is a cast AL-0.5% Cu target blank feather grain microstructure (electropolishing and coating 100X) at a casting temperature above 690 ℃;
FIG. 7 is a cast AL-0.5% Cu target blank feathered microstructure (electropolished and coated 50X) at a casting temperature below 670 ℃.
Detailed Description
In order to further illustrate the preparation method of the high-purity aluminum-copper alloy target blank for sputtering according to the present invention and achieve the intended purpose, the following detailed description of the preparation method of the high-purity aluminum-copper alloy target blank for sputtering according to the present invention, with reference to the preferred embodiments, the structure, the characteristics and the effects thereof, will be made as follows. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The following will describe in detail a method for preparing a high-purity aluminum-copper alloy target blank for sputtering with reference to specific embodiments:
the technical scheme of the invention is as follows:
s10: melting high-purity aluminum with the purity of 99.999-99.9995% and high-purity copper with the purity of more than 99.999% in a vacuum melting furnace, controlling the melting temperature at 800-: the content of copper element in the intermediate alloy liquid 1 is 20-25 wt%.
S20: adding a high-purity aluminum ingot with the purity of more than 99.9995 wt% and the intermediate alloy liquid into an intermediate frequency smelting furnace for smelting, wherein the smelting temperature is 720-800 ℃, stirring uniformly after complete melting, controlling the temperature of the alloy liquid to 730 +/-5 ℃, standing and preserving heat for 15min to obtain intermediate alloy liquid 2.
S30: and refining the intermediate alloy liquid 2 in a furnace by adopting high-purity argon, and standing for 20min after refining to obtain intermediate alloy liquid 3.
S40: and refining the intermediate alloy liquid 3 on line by adopting high-purity argon to obtain an intermediate alloy liquid 4.
The alloy liquid is subjected to double refining of furnace refining and on-line refining, degassing and deslagging are carried out, and the impurity content is better controlled
S50: and carrying out bipolar filtration on the intermediate alloy liquid 4 to obtain an intermediate alloy liquid 5.
S60: and (3) casting the intermediate alloy liquid 5 into a bar blank with the diameter of phi 120-.
Preferably, in the step S10, the stirring time is not less than 15 min; in the step S20, the stirring time is not less than 15 min. To control the compositional uniformity of the alloy.
Preferably, in the step S20, standing and heat preservation are carried out for 15min, so as to ensure that the molten aluminum is completely melted and the components are uniform. And then sampling to detect the content of copper element, if the content of copper element meets the mass ratio of 0.4-0.6%, starting refining in the furnace, and if the content of copper element does not meet the mass ratio, secondarily adding the intermediate alloy to adjust to the required ratio.
Preferably, in S30, the flow rate of argon is 3-5m3The refining time is 25-40min, and the refining temperature is 730-.
Preferably, in S40, the flow rate of argon is 3-5m3H, refining time of 15-20min, and refining temperature of 730-.
Preferably, in S50, the bipolar filtration means an in-line filtration using a 40PPI and a 50PPI porosity filter plate.
Preferably, in S60, a semi-continuous casting machine is used to perform water cooling for the phi 120-.
The invention uses the raw material of 99.999-99.9995 wt% purity ultra-pure aluminum and 99.999 wt% purity high-purity copper to prepare the intermediate alloy, the mass percent of the intermediate alloy is controlled to be 0.4-0.6 wt% by adopting the multi-time adding process during smelting, and the bar with high surface quality and uniform structure is cast through furnace refining, on-line refining and bipolar filtration.
Example 1.
The specific operation steps are as follows:
preparing an S10 intermediate alloy: an ultra-pure aluminum raw material with the purity of 99.9995 wt% and high-purity copper with the purity of 99.999 wt% are used for preparing an intermediate alloy. Melting high-purity aluminum and high-purity copper in a vacuum melting furnace, heating and melting the vacuum melting furnace after vacuumizing, controlling the melt temperature to be 830 ℃ after an aluminum ingot is completely melted, preserving the temperature for not less than 15min, and continuously stirring to obtain intermediate alloy liquid 1 (the content of copper element in the intermediate alloy liquid 1 is 25 wt%).
S20 smelting: adding a high-purity aluminum ingot with the purity of more than 99.9995 wt% and an intermediate alloy liquid with the purity of 25 wt% into an intermediate frequency smelting furnace according to a specific proportion. The melting temperature is 750 ℃, the temperature is kept for not less than 15min after the melting is completed, and the stirring is continued. And controlling the temperature of the alloy liquid to 730 +/-5 ℃, standing and preserving the temperature for 15min to obtain intermediate alloy liquid 2. Sampling to detect the content of copper element, and when the mass percent of copper is 0.5%, the other impurity elements are in the control standard and enter the refining procedure in the furnace.
S30 furnace refining: refining the intermediate alloy liquid 2 in a furnace by adopting high-purity argon, wherein the flow of the argon is 3-5m3And h, controlling the refining temperature at 730-. And fishing out the surface scum after the refining in the furnace to obtain the intermediate alloy liquid 3.
S40 on-line refining: controlling the temperature of the master alloy liquid 3 to be 730 ℃ for online aluminum pouring. Refining with high-purity argon on-line with argon flow of 3-5m3And h, controlling the refining temperature at 730-.
S50 on-line filtration: and filtering the intermediate alloy liquid 4 by using a bipolar plate, wherein the porosity of the two filter plates is 40PPI and 50PPI respectively to obtain an intermediate alloy liquid 5.
S60: casting: adopting a semi-continuous casting machine to carry out water cooling to cast a bar blank with the diameter of 120mm, injecting the intermediate alloy liquid 5 into the crystallizer along a chute and a diverter plate, measuring the temperature by using a thermocouple in the casting process, and controlling the temperature of the aluminum liquid in the crystallizer of the casting machine to be 670-The temperature of molten aluminum in the furnace is 730 ℃, the casting speed is 120mm/min, and the flow rate of cooling water is 1200L/m3And obtaining the high-purity aluminum-copper alloy target blank for sputtering.
The high-purity aluminum-copper alloy target blank is subjected to sawing, turning, soaking, forging, rolling and annealing to refine and homogenize the grain structure, and then is subjected to sawing, turning and binding of a back plate to obtain the sputtering target.
FIG. 2 shows the microstructure of a cast AL-25% Cu high purity aluminum copper master alloy (polished non-corroded 100X).
FIG. 3 shows the macroscopically eroded microstructure of a cast AL-0.5% Cu target blank.
FIG. 4 shows the cast AL-0.5% Cu target blank microstructure (electropolishing and coating 50X).
As can be seen from the graphs in FIGS. 2-4, the prepared high-purity aluminum-copper alloy target blank has high surface quality, uniform structure, no defect with the size of more than 0.8mm, and fine and uniform crystal grains.
Example 2.
The specific operation steps are as follows:
preparing an S10 intermediate alloy: an ultra-pure aluminum raw material with the purity of 99.999 wt% and high-purity copper with the purity of 99.999 wt% are used for preparing an intermediate alloy. Melting high-purity aluminum and high-purity copper in a vacuum melting furnace, heating and melting the vacuum melting furnace after vacuumizing, controlling the melt temperature to be 830 ℃ after aluminum ingots are completely melted, preserving the temperature for 20min, and continuously stirring to obtain intermediate alloy liquid 1 (the content of copper element in the intermediate alloy liquid 1 is 20 wt%).
S20 smelting: adding a high-purity aluminum ingot with the purity of more than 99.9995 wt% and an intermediate alloy liquid with the purity of 25 wt% into an intermediate frequency smelting furnace according to a specific proportion. The smelting temperature is 720 ℃, after the materials are completely melted, the temperature is kept for 20min, and the materials are continuously stirred; and controlling the temperature of the alloy liquid to 730 +/-5 ℃, standing and preserving the temperature for 15min to obtain intermediate alloy liquid 2. Sampling to detect the content of copper element, and when the mass percent of copper is 0.4%, the other impurity elements are in the control standard and enter the refining procedure in the furnace.
S30 furnace refining: refining the intermediate alloy liquid 2 in a furnace by adopting high-purity argon, wherein the flow of the argon is 3-5m3The refining temperature is controlled at 730-Standing for 20min at a time of 40 min. And fishing out the surface scum after the refining in the furnace to obtain the intermediate alloy liquid 3.
S40 on-line refining: controlling the temperature of the master alloy liquid 3 to be 730 ℃ for online aluminum pouring. Refining with high-purity argon on-line with argon flow of 3-5m3And h, controlling the refining temperature at 730-.
S50 on-line filtration: and filtering the intermediate alloy liquid 4 by using a bipolar plate, wherein the porosity of the two filter plates is 40PPI and 50PPI respectively to obtain an intermediate alloy liquid 5.
S60: casting: casting a phi 164mm bar blank by adopting a semi-continuous casting machine for water cooling, injecting an intermediate alloy liquid 5 into a crystallizer along a chute and a diverter plate, measuring the temperature by using a thermocouple in the casting process, controlling the temperature of aluminum liquid in the casting machine crystallizer to be 680-690 ℃, the temperature of the aluminum liquid in the furnace to be 731 ℃, the casting speed to be 100mm/min and the cooling water flow to be 1000L/m3And obtaining the high-purity aluminum-copper alloy target blank for sputtering.
Example 3.
The specific operation steps are as follows:
preparing an S10 intermediate alloy: an ultra-pure aluminum raw material with the purity of 99.9995 wt% and high-purity copper with the purity of 99.999 wt% are used for preparing an intermediate alloy. Melting high-purity aluminum and high-purity copper in a vacuum melting furnace, heating and melting the vacuum melting furnace after vacuumizing, controlling the melt temperature to 850 ℃ after an aluminum ingot is completely melted, preserving the temperature for 25min, and continuously stirring to obtain intermediate alloy liquid 1 (the content of copper element in the intermediate alloy liquid 1 is 22 wt%).
S20 smelting: adding a high-purity aluminum ingot with the purity of more than 99.9995 wt% and an intermediate alloy liquid with the purity of 25 wt% into an intermediate frequency smelting furnace according to a specific proportion. The smelting temperature is 800 ℃, and after complete melting, the temperature is kept for 25min and stirring is carried out; and controlling the temperature of the alloy liquid to 730 +/-5 ℃, standing and preserving the temperature for 15min to obtain intermediate alloy liquid 2. Sampling to detect the content of copper element, and when the mass percent of copper is 0.6%, the other impurity elements are in the control standard and enter the refining procedure in the furnace.
S30 furnace refining: refining the intermediate alloy liquid 2 in a furnace by adopting high-purity argon, wherein the flow of the argon is 3-5m3H, refining temperatureControlling the temperature at 730-. And fishing out the surface scum after the refining in the furnace to obtain the intermediate alloy liquid 3.
S40 on-line refining: controlling the temperature of the master alloy liquid 3 to be 730 ℃ for online aluminum pouring. Refining with high-purity argon on-line with argon flow of 3-5m3And h, controlling the refining temperature at 730-.
S50 on-line filtration: and filtering the intermediate alloy liquid 4 by using a bipolar plate, wherein the porosity of the two filter plates is 40PPI and 50PPI respectively to obtain an intermediate alloy liquid 5.
S60: casting: adopting a semi-continuous casting machine to carry out water cooling to cast a bar blank with the diameter of 140mm, injecting the intermediate alloy liquid 5 into the crystallizer along a chute and a splitter plate, measuring the temperature by using a thermocouple in the casting process, controlling the temperature of 675-685 DEG of aluminum liquid in the crystallizer of the casting machine, the temperature of 730 DEG of the aluminum liquid in the furnace, the casting speed of 110mm/min and the cooling water flow of 1100L/m3And obtaining the high-purity aluminum-copper alloy target blank for sputtering.
The master alloy liquids 5 of examples 1 to 3 were examined to determine that the trace impurity elements were at an extremely low level: the content of alkali metal elements such as Na, K and the like is less than or equal to 0.2 ppm; fe. The content of heavy metal elements such as Si, Ni and the like is less than or equal to 1 ppm; u, Th and other radioactive elements are less than or equal to 0.001 ppm; C. o, N, etc. with the impurity content less than or equal to 10 ppm.
Unreasonable casting parameters will seriously affect the surface quality and microstructure of the cast ingot. When the casting temperature is higher than 690 ℃, feather grain structures are easy to appear, such as the cast AL-0.5% Cu target blank macro corrosion feather grain structures in figure 5, and the cast AL-0.5% Cu target blank feather grain microstructures in figure 6 (electrolytic polishing and film coating 100X). When the melting temperature is lower than 670 ℃, an abnormal structure with coarse grains is easy to appear, such as an abnormal microstructure (electropolishing and film coating 50X) of the cast AL-0.5% Cu target blank grains shown in figure 7. And once the two defects are formed in the casting process, the defects cannot be eliminated in the subsequent processing process, and the mechanical property and the processing property of the cast ingot are seriously influenced.
The invention adopts the self-prepared intermediate alloy and the ultra-pure aluminum raw material to prepare 0.4-0.6 wt% of Cu high-purity aluminum-copper alloy melt. The intermediate alloy adopts a fractional addition process, namely, the once-added alloy is completely melted and then is kept warm and kept stand for 20-30min, the components are controlled to be uniform through the electromagnetic stirring effect, and the secondary intermediate alloy addition is carried out after the sampling component detection. Controlling the trace impurity elements in the melt at an extremely low level: the content of alkali metal elements such as Na, K and the like is less than or equal to 0.2 ppm; fe. The content of heavy metal elements such as Si, Ni and the like is less than or equal to 1 ppm; u, Th and other radioactive elements are less than or equal to 0.001 ppm; C. o, N, etc. with the impurity content less than or equal to 10 ppm.
The invention uses a semi-continuous casting method to prepare the high-purity aluminum-copper alloy target blank for sputtering. The purity and uniformity of the alloy components are controlled by a casting process. The semi-continuous casting process has excellent degassing and deslagging effects, so that the process is suitable for industrial batch production and has practicability.
The invention self-prepares high-purity aluminum-copper intermediate alloy and casts the intermediate alloy into bar blank, can realize the purity control of the intermediate alloy components and ensure the uniformity of the alloy components. The technological processes of vacuum melting, on-line refining and bipolar filtration are adopted, so that the cast bar blank has uniform components, low content of trace elements and smooth surface, and has no defects of impurities, air holes, shrinkage cavities and the like.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the high-purity aluminum-copper alloy target blank for sputtering is characterized by comprising the following steps of:
s10: melting high-purity aluminum with the purity of 99.999-99.9995% and high-purity copper with the purity of more than 99.999% in a vacuum melting furnace, controlling the melting temperature at 800-: the content of copper element in the intermediate alloy liquid 1 is 20-25 wt%;
s20: adding a high-purity aluminum ingot with the purity of more than 99.9995 wt% and the intermediate alloy liquid into an intermediate frequency smelting furnace for smelting, wherein the smelting temperature is 720-800 ℃, stirring uniformly after complete melting, controlling the temperature of the alloy liquid to 730 +/-5 ℃, standing and preserving heat for 15min to obtain intermediate alloy liquid 2;
s30: refining the intermediate alloy liquid 2 in a furnace by adopting high-purity argon, and standing for 20min after refining to obtain intermediate alloy liquid 3;
s40: carrying out on-line refining on the intermediate alloy liquid 3 by adopting high-purity argon to obtain an intermediate alloy liquid 4;
s50: carrying out bipolar filtration on the intermediate alloy liquid 4 to obtain an intermediate alloy liquid 5;
s60: and (3) casting the intermediate alloy liquid 5 into a bar blank with the diameter of phi 120-.
2. The production method according to claim 1,
in the step S10, the stirring time is not less than 15 min;
in the step S20, the stirring time is not less than 15 min.
3. The production method according to claim 1,
and in S20, standing and preserving heat for 15min, sampling and detecting the content of copper element, starting refining in the furnace if the content of copper element meets the mass ratio of 0.4-0.6%, and adding the intermediate alloy for the second time if the content of copper element does not meet the mass ratio to adjust to the required ratio.
4. The production method according to claim 1,
in S30, the flow rate of argon gas is 3-5m3The refining time is 25-40min, and the refining temperature is 730-.
5. The production method according to claim 1,
in S40, the flow rate of argon gas is 3-5m3H, refining time of 15-20min, and refining temperature of 730-.
6. The production method according to claim 1,
in S50, bipolar filtration refers to in-line filtration using a 40PPI and a 50PPI porosity filter plate.
7. The production method according to claim 1,
in S60, a semi-continuous casting machine is used for water cooling to perform phi 120-.
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