Preparation method of sputtering target material of AgPdCu alloy

Abstract

The invention relates to the technical field of target materials, and provides a preparation method of an AgPdCu alloy sputtering target material, which comprises the following steps: firstly melting silver and preserving heat, then adding palladium and copper, heating to 1550 DEG C and preserving heat for 1 hour; the alloy liquid is subjected to heat preservation for 1 hour, the cast ingot is poured into a mold to be cooled after being subjected to homogenizing annealing, the cast ingot is obtained, casting stress can be eliminated, the non-uniformity of an as-cast structure is improved, and a more stable material basis is provided for follow-up machining; then the cast ingot is subjected to hot rolling at high temperature and at the machining rate of 85%, coarse as-cast grains can be crushed, the structure can be refined, the material compactness can be improved, and the mechanical property of the target material can be enhanced; 5 passes are conducted, cold rolling is conducted at the machining rate of 15% in each pass, the work hardening degree is controlled through step-by-step deformation, material cracking is avoided, and meanwhile the thickness precision is guaranteed; annealing treatment is performed, so that cold rolling internal stress can be eliminated, material plasticity is recovered, and the strength and processing performance of the target material are balanced; and finally, straightening and linear cutting are carried out.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and in particular to a method for preparing a sputtering target material of an AgPdCu alloy. Background Art

[0002] In the external parts of existing electronic components, their surface protection films or functional films are usually formed into pure silver films or silver alloy films on their surfaces by sputtering, ion plating, vapor deposition, etc., or are formed of pure silver or silver alloys. In addition to increasing the decorative value, they can also provide protection and functionality, such as conductivity and light transmittance.

[0003] However, when pure silver or the like is used as a material for external components, since pure silver is less corrosion-resistant than precious metals such as gold, platinum, and palladium, it will oxidize and turn black silver or corrode and turn yellow during use, affecting its conductivity and optical properties. Furthermore, it may be corroded by sulfur and other substances in the atmosphere during storage. Meanwhile, in recent years, the miniaturization of electrode and wiring patterns has been gradually promoted in displays, LEDs, touch panels, organic EL elements, and the like. Among these, since Ag is prone to the so-called ion migration phenomenon, short circuits may occur in miniaturized electrode and wiring patterns when current flows, requiring an Ag alloy film with excellent resistance to electron or ion migration. Therefore, a sputtering target of an Ag alloy is required. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to provide a method for preparing a sputtering target of AgPdCu alloy, which solves the problems in the background technology.

[0005] Based on the above purpose, the present invention provides a method for preparing a sputtering target of an AgPdCu alloy, wherein the target comprises 1.0wt%-2.0wt% of high-purity palladium, 0.5wt%-1.5wt% of high-purity copper, and the balance of high-purity silver;

[0006] The preparation method comprises the following steps:

[0007] Step 1: First, high-purity silver is placed at the bottom of a vacuum medium-frequency electric furnace. When the furnace temperature reaches 1000°C, this temperature is maintained for 20 minutes. Then, high-purity palladium and high-purity copper are added. The temperature is then raised to 1550°C and maintained for 1 hour to obtain a molten alloy.

[0008] Step 2: pouring the alloy liquid into a mold and cooling it to obtain an ingot;

[0009] Step 3: milling the ingot, heating it to 850-950°C in a heating furnace, and then hot rolling it to obtain a hot-rolled billet;

[0010] Step 4: After hot rolling, the billet is cold rolled for 5 passes;

[0011] Step 5: The cold-rolled sheet is placed in an annealing furnace and annealed at 650-750°C for 1-2 hours, followed by air cooling.

[0012] Step 6: The cold-rolled plate is straightened and wire-cut to a size of 12 inches in diameter to obtain the finished product.

[0013] Preferably, electromagnetic stirring is used throughout the entire process of step 1 to fully mix the high-purity silver, high-purity palladium and high-purity copper.

[0014] Preferably, in step 2, the ingot is subjected to homogenization annealing at a temperature of 900-950° C. for 8-10 hours.

[0015] Preferably, the processing rate of the hot rolling in step 3 is 85%.

[0016] Preferably, the cold rolling processing rate of each pass in step 4 is 15%.

[0017] Preferably, the purity of the high-purity silver, high-purity palladium and high-purity copper is greater than 99.999%.

[0018] Preferably, the alloy liquid in step 2 is kept warm for 1 hour and then poured into a mold to cool.

[0019] Preferably, after the cold rolling in step 4, the plate is subjected to hot isostatic pressing post-treatment at a temperature of 700° C., a pressure of 100 MPa, and a heat preservation period of 2 hours.

[0020] The beneficial effects of the present invention are as follows: the present invention adopts silver, palladium and copper raw materials with a purity of more than 99.999%, which reduces the interference of impurities on the performance of the target material from the source; by first melting silver and keeping it warm, then adding palladium and copper and heating it to 1550℃ and keeping it warm for 1 hour, combined with electromagnetic stirring, the alloy elements are fully mixed, the risk of component segregation is effectively reduced, and the uniformity of the alloy composition is ensured; the alloy liquid is then kept warm for 1 hour and the ingot is homogenized and annealed before being poured into a mold and cooled to obtain an ingot, which can eliminate casting stress, improve the unevenness of the cast structure, and provide a more stable material basis for subsequent processing; the ingot is then hot rolled at a high temperature and a processing rate of 85%, which can crush the coarse cast grains and refine the grains. The target material is organized and its density is improved, and its mechanical properties are enhanced; then cold rolling is carried out for 5 times with a processing rate of 15% per pass, and the degree of work hardening is controlled by step-by-step deformation to avoid material cracking while ensuring thickness accuracy; annealing treatment is then carried out to eliminate cold rolling internal stress, restore material plasticity, and balance the strength and processing performance of the target material; finally, straightening and wire cutting are carried out to meet the installation requirements of the sputtering equipment and improve the yield rate; the overall process improves the sputtering stability and thin film deposition quality of the target material through composition homogenization, organizational refinement and performance regulation. The alloy target material produced has small grains, high purity, and no ion migration phenomenon, which is suitable for high-precision thin film preparation scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the technical solutions in the present invention or the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only for ordinary technicians in this field of the present invention, and other drawings can be obtained based on these drawings without paying any creative work.

[0022] Figure 1 It is a production process flow chart of the present invention;

[0023] Figure 2 is a grain size diagram of Example 1 of the present invention;

[0024] Figure 3 This is a grain size diagram of Example 2 of the present invention. DETAILED DESCRIPTION

[0025] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to specific embodiments.

[0026] It should be noted that, unless otherwise defined, the technical or scientific terms used in the present invention should have the usual meanings understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly.

[0027] Example 1

[0028] like Figure 1 As shown, a method for preparing a sputtering target of an AgPdCu alloy, wherein the target comprises high-purity palladium, high-purity copper, and high-purity silver with a purity greater than 99.999%. The weight percentage of each component in the alloy is 1.0% palladium, 0.5% copper, and the balance is silver, thereby reducing the interference of impurities on the target performance from the source;

[0029] The preparation method is as follows:

[0030] S1: First, high-purity silver is placed at the bottom of a vacuum medium-frequency electric furnace. When the furnace temperature reaches 1000°C, this temperature is maintained for 20 minutes. Then, high-purity palladium and high-purity copper are added. The temperature is then raised to 1550°C and maintained for 1 hour. Electromagnetic stirring is used throughout the process to fully mix the alloy liquid. This promotes full mixing of alloy elements, effectively reduces the risk of component segregation, and ensures the uniformity of alloy composition.

[0031] S2, after the alloy liquid is kept warm for 1 hour, it is poured into a mold and cooled to obtain an ingot;

[0032] S3, homogenization annealing of the ingot at 900℃ for 8 hours can eliminate casting stress, improve the unevenness of the cast structure, and provide a more stable material foundation for subsequent processing;

[0033] S4, milling the ingot, then heating it to 900°C in a heating furnace and hot rolling it, with a hot rolling processing rate of 85%, to obtain a hot-rolled billet, which can crush coarse cast grains, refine the structure and improve the material density, thereby enhancing the mechanical properties of the target material;

[0034] S5, after hot rolling, the billet is cold rolled for 5 passes, with a processing rate of 15% for each pass. The degree of work hardening is controlled by step-by-step deformation to avoid material cracking while ensuring thickness accuracy;

[0035] S6, after cold rolling, the plate is subjected to hot isostatic pressing (HIP) treatment at a temperature of 700°C, a pressure of 100 MPa, and a holding time of 2 h to further improve the density of the target material and reduce internal porosity;

[0036] S7, the cold-rolled plate is placed in an annealing furnace and annealed at 750°C for 2 hours, followed by air cooling to eliminate cold-rolled internal stress, restore material plasticity, and balance the strength and processing performance of the target material;

[0037] S8, the cold-rolled plate is straightened and wire-cut to a size of 12 inches in diameter to obtain the finished product. The grain size is as follows: Figure 2 The obtained alloy target material has fine grains, high purity, and no ion migration occurs.

[0038] Example 2

[0039] like Figure 1 As shown, a method for preparing a sputtering target material of an AgPdCu alloy, wherein the target material includes high-purity palladium, high-purity copper and high-purity silver with a purity of >99.999%. The weight percentage of each component in the alloy is 2.0% palladium, 1.5% copper and the balance is silver, thereby reducing the interference of impurities on the target material performance from the source.

[0040] The preparation method is as follows:

[0041] S1: First, high-purity silver is placed at the bottom of a vacuum medium-frequency electric furnace. When the furnace temperature reaches 1000°C, this temperature is maintained for 20 minutes. Then, high-purity palladium and high-purity copper are added. The temperature is then raised to 1550°C and maintained for 1 hour. Electromagnetic stirring is used throughout the process to fully mix the alloy liquid. This promotes full mixing of alloy elements, effectively reduces the risk of component segregation, and ensures the uniformity of alloy composition.

[0042] S2, after the alloy liquid is kept warm for 1 hour, it is poured into a mold and cooled to obtain an ingot;

[0043] S3, homogenization annealing of the ingot at 900℃ for 8 hours can eliminate casting stress, improve the unevenness of the cast structure, and provide a more stable material foundation for subsequent processing;

[0044] S4, milling the ingot, then heating it to 950°C in a heating furnace and hot rolling it, with a hot rolling processing rate of 85%, to obtain a hot-rolled billet, which can crush coarse cast grains, refine the structure and improve the material density, thereby enhancing the mechanical properties of the target material;

[0045] S5, after hot rolling, the billet is cold rolled for 5 passes, with a processing rate of 15% for each pass. The degree of work hardening is controlled by step-by-step deformation to avoid material cracking while ensuring thickness accuracy;

[0046] S6, after cold rolling, the plate is subjected to hot isostatic pressing (HIP) treatment at a temperature of 700°C, a pressure of 100 MPa, and a holding time of 2 h to further improve the density of the target material and reduce internal porosity;

[0047] S7, the cold-rolled plate is placed in an annealing furnace and annealed at 800°C for 1.5 hours, followed by air cooling to eliminate cold-rolled internal stress, restore material plasticity, and balance the strength and processing performance of the target material;

[0048] S8, the cold-rolled plate is straightened and wire-cut to a size of 12 inches in diameter to obtain the finished product. The grain size is as follows: Figure 3 The obtained alloy target has fine grains and high purity.

[0049] Those skilled in the art will understand that the discussion of any of the above embodiments is merely illustrative and is not intended to limit the scope of the present invention to these examples. Within the spirit and principles of the present invention, the technical features of the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and many other variations exist in the various aspects of the present invention described above, which are not provided in detail for the sake of clarity. Any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A method for preparing a sputtering target of an AgPdCu alloy, characterized in that: The target material comprises 1.0wt%-2.0wt% of high-purity palladium, 0.5wt%-1.5wt% of high-purity copper and the balance of high-purity silver; The preparation method comprises the following steps: Step 1: First, high-purity silver is placed at the bottom of a vacuum medium-frequency electric furnace. When the furnace temperature reaches 1000°C, this temperature is maintained for 20 minutes. Then, high-purity palladium and high-purity copper are added. The temperature is then raised to 1550°C and maintained for 1 hour to obtain a molten alloy. Step 2: pouring the alloy liquid into a mold and cooling it to obtain an ingot; Step 3: milling the ingot, heating it to 850-950°C in a heating furnace, and then hot rolling it to obtain a hot-rolled billet; Step 4: After hot rolling, the billet is cold rolled for 5 passes; Step 5: The cold-rolled sheet is placed in an annealing furnace and annealed at 650-750°C for 1-2 hours, followed by air cooling. Step 6: The cold-rolled plate is straightened and wire-cut to a size of 12 inches in diameter to obtain the finished product.

2. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, characterized in that: The entire process of step 1 is carried out by using electromagnetic stirring to fully mix the high-purity silver, high-purity palladium and high-purity copper.

3. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, characterized in that: In the second step, the ingot is subjected to homogenization annealing at a temperature of 900-950° C. for 8-10 hours.

4. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, characterized in that: The processing rate of the hot rolling in step 3 is 85%.

5. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, wherein: The cold rolling processing rate of each pass in step 4 is 15%.

6. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, characterized in that: The purity of the high-purity silver, high-purity palladium and high-purity copper is greater than 99.999%.

7. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, characterized in that: In the second step, the alloy liquid is kept warm for 1 hour and then poured into a mold to cool.

8. The method for preparing a sputtering target of an AgPdCu alloy according to claim 1, characterized in that: In the fourth step, after cold rolling, the plate is subjected to hot isostatic pressing treatment at a temperature of 700° C., a pressure of 100 MPa, and a heat preservation time of 2 hours.

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